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1. SOP Alkalinity LFUCG Laboratory Page 7 of 219 Revision Number 2 Last Revised 9 09 ORION Total Alkalinity Test Kit HIGH RANGE 0 to 225 mg L as CaCO3 Add 10 mL of ORION Total Alkalinity Reagent to 100 mL and mix well Measure pH of mixture and read total alkalinity from this table Observed Total Observed Total Observed Total Observed Total Observed Total pH Alkalinity pH Alkalinity pH Alkalinity pH Alkalinity pH Alkalinity 3 66 0 0 4 01 47 4 36 93 4 71 140 5 06 187 3 67 1 2 4 02 48 4 37 95 4 72 141 5 07 188 3 68 2 5 4 03 49 4 38 96 4 73 143 5 08 190 3 69 3 8 4 04 51 4 39 97 4 74 144 5 09 191 3 70 5 2 4 05 52 4 40 99 4 75 145 5 10 192 3 71 6 5 4 06 53 4 41 100 4 76 147 5 11 194 3 72 7 8 4 07 55 4 42 101 4 77 148 5 12 195 3 73 9 2 4 08 56 4 43 103 4 78 149 5 13 196 3 74 1 4 09 57 4 44 104 4 79 151 5 14 198 3 75 2 4 10 59 4 45 105 4 80 152 5 15 199 3 76 3 4 11 60 4 46 107 4 81 153 5 16 200 3 77 5 4 12 61 4 47 108 4 82 155 5 17 202 3 78 6 4 13 63 4 48 109 4 83 156 5 18 203 3 79 7 4 14 64 4 49 111 4 84 157 5 19 204 3 80 9 4 15 65 4 50 112 4 85 159 5 20 206 3 81 20 4 16 67 4 51 113 4 86 160 5 21 207 3 82 21 4 17 68 4 52 115 4 87 161 5 22 208 3 83 23 4 18 69 4 53 116 4 88 163 5 23 210 3 84 24 4 19 71 4 54 117 4 89 164 5 24 211 3 85 25 4 20 72 4 55 119 4 90 165 5 25 212 3 86 27 4 21 73 4 56 120 4 91 167 5 26 214 3 87 28 4 22 75 4 57 121 4 92 168 5 27 215 3 88 29 4 23 76 4 58 123 4 93 169 5 28 216 3 89 31 4 24 77 4 59
2. sE el l e JE m S gt 5 e ale Nn g 5 Re ul Ps 23185 10 17 09 WH Raw Influent Sat 23186 0 17 09 Plant Effluent Sat 2321 0 19 09 Above Leak 2321 0 19 09 Below Leak 2321 0 19 09 In Spring al la s a s a s a s Quality Control Manager Is To Receive A Copy Of All Q C Results Presevation Cool 4 C H2SO to pH lt 2 Maximum Holding Time 28 days EPA Limit EPA Limit Averages Monthly TB PTE In Winter 10 5 mg L WH PTE In Winter 10 mg L TB PTE In Summer WH PTE In Summer 4 mg L Weekly 15 mg L 6 mg L v ad TOWN BRANCH WASTEWATER TREATMENT PLANT Town Branch Laboratory Carbonaceous Biochemical Oxygen Demand amp Biochemical Oxygen Demand Method EPA Method 405 1 5 Days 20 C BOD amp CBOD SEED CORRECTION DATA Bottle Number Date Sample Collected Volume of Seed Used in Seed Control S Initial D O of Seed Control Bottle B Date Sample Collected if Different from the above date Date Incubation Date Incubation Started Stopped Unseeded Blank Initial D O 5 Day D O Sodium Sulfite Added Plant Effluent Winkler Method Initial D O BIOCHEMICAL OXYGEN DEMAND CALCULATIONS Bottle Number Log Number Date Sample Collected ime Analysis Started _ ample Volume nitial D O of Sample Day D O of Sample Actual Value 198 mg L D O Dissolved Oxygen Analyst Setting Up Analysis B O D Biochemical Oxygen Demand B
3. 03298300 ee 117 Salt River at Shepherds ville Do ORIBE oo 138 Long Lick near Clermont d o BAZISI o 119 Rolling Fark Beech Fork at Maud De O3300400 0 20 Rolling Fork near Boston d aaa aae OIIDIS0O ii es 121 Wilson Creek at Harrison Fork Road near Deatsville e a a o o o 0 2 03201575 122 Pond Creek Southern Ditch Seuthern Ditch at Minors Lane near Okalona cy o es OMBGTBRO o 123 Slop Ditch near Okolosa a OB3OI8BS 2 124 Northem Ditch Fern Creek at Old Bardstown Road at Louisville co 0 ee es A ee 127 Northern Ditch at Coloma Ed ee OBRAR coo 128 Spring Ditch at Private Drive near Okolona dE ooo ee DIF ee 129 Pond Creek near Lovisville dd o ee eee O3302000 o 130 Pond Creek at Pendleros Road near Louisville 0 o 03302080 o 132 OTTER CREEK BASIN Otter Creek at Outer Creek Park near Rock Haven Ky fe 00 ee BRZIH o ee 133 Ohio River at Cannelton Dam BI 03303286 0 ee 134 GREEN RIVER BASIN Groen River Russel Creek near Columbia td oaa aaa Es aaa ee 142 Green River al Munfordville do 03308500 o 343 Nolin River at White Mills dh o ee P330 o 124 Nolin River at Kyrk aaa a e OB aaa aaa 145 Beaver Creek at Hwy 31 E near Glasgow iD o ooo OFFS oo 146 Barren River West Fork Drakes Creek near Franklin d 0 ee ee BIO o 147 Green River at Paradise Do 03330 we 348 So ty SURFACE WATER STATIONS IN DOWNSTREAM GRDER FOR WHICH RECORDS A
4. QUO SB jey uey LOW salenbs juno 9997 arenbs u gare mo 198 0 og Ag Adina pue sosenbs 1moA Juno st op 01 savy nod y paj osenbs o vare ue ogy pps aunseaurt nod dap Iaea jo orenbs yeg wonog 0 doy WO 1993 GZ AIOAG 10 S RAJOJUE UDUT UT PNS JULNSRIM MOA YEW ESTEAN 100 OM Je qidop Joye ANSE AGUAS MOLE weas OY JO RALLY BUOIAS SSOID I4 193 OL udag Jayem uy WN eT TRE i ER ce IEA eee See IAN LACAN INEA oe eae zo OZ Ek Gi Fi Gs Q B G 3 o Grp 220814 E umoys se oded ydeiS uo WGYSIS S80I5 WEINS 10 MRAP ay ABAP SIUBUISIMISBIL POPIODHA INOA WOLA p tl TDSTestr wm E __ Full readout pocket size TDS and conductivity testers l BEFORE FIRST USE Remove plastic strips berween batteries and contacts if present see box side panels Soak electrodes for a few minutes in alcoho to remove ails carros To AVOID CROSS CONTAMINATION BETWEEN SAMPLES NEVER IMMERSE THE TOSTESTR ABOVE THE COLOR RAND f CALIBRATION Using the guide on the side box panel select A ONT Te ene ee AR o E BA LIFT FLAP TO OPEN A EN a a calibration standard appropriate for your TDS Testr model When sefecting a TDS standard for ppt or ppm TDS readings it is best t select a standard having a similar chemical make up as the test solution Best accuracy is obtained when the calibration solution value is close to the test solution value Pour the calibration standard into two separate containers and some tap or d
5. SCORE 4 Sediment Deposition Parameters to be evaluated in sampling reach 20 19 18 17 16 Little or no enlargement of islands or point bars and less than 5 of the bottom affected by sediment deposition 15 14 13 12 11 Some new increase in bar formation mostly from gravel sand or fine sediment 5 30 of the bottom affected slight deposition in pools 10 9 8 7 6 Moderate deposition o new gravel sand or fine sediment on old and new bars 30 50 of the bottom affected sediment deposits at obstructions constrictions and bends moderate deposition of pools prevalent 514 3 2 1 0 Heavy deposits of fine material increased bar development more than 50 of the bottom changing frequently pools almost absent due to substantial sediment deposition SCORE 5 Channel Flow Status 20 19 18 17 16 Water reaches base of both lower banks and minimal amount of channel substrate is exposed 15 14 13 12 11 Water fills gt 75 of the available channel or lt 25 of channel substrate is exposed 10 9 8 7 6 Water fills 25 75 of the available channel and or riffle substrates are mostly exposed 5014132170 Very little water in channel and mostly present as standing pools SCORE 20 19 18 17 16 15 14 13 12 11 J Forms and Templates Technical Data Sheets and Checklists Streams Habita
6. 12 SOP NH LFUCG Laboratory Page 14 of 219 Revision Number 1 Last Revised 09 09 Bibliography 12 1 12 2 12 3 12 4 U S EPA Method 350 1 Nitrogen Ammonia Colorimetric Automated Phenate Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 HACH DOC316 53 01081 Method 10205 Nitrogen Ammonia Salicylate method TNTplus 830 HACH Company Loveland CO 2008 HACH DOC316 53 01082 Method 10205 Nitrogen Ammonia Salicylate method TNTplus 831 HACH Company Loveland CO 2008 HACH DOC316 53 01083 Method 10205 Nitrogen Ammonia Salicylate method TNTplus 832 HACH Company Loveland CO 2008 14 SOP CBOD LFUCG Laboratory Page 15 of 219 Revision Number 5 Last Revised 09 09 Biochemical Oxygen Demand BODs and Carbonaceous Biochemical Oxygen Demand CBODs Analysis EPA Method 405 1 Editorial Revision 1974 Standard Methods 5210 A and 5210 B Scope Significance to Process and Application The Biochemical Oxygen Demand BODs and Carbonaceous Biochemical Oxygen Demand CBODs analysis assesses the concentration and general composition of organic matter in raw water supplies wastewaters treated effluents and receiving waters This test is used to determine the efficiency of the treatment process at Town Branch West Hickman and Blue Sky Wastewater Treatment Plants Summary of Method
7. 12 13 14 Turn on the DRB200 Reactor Heat to 100 C For DRB200 Reactors with 16 mm wells make sure the 16 to 13 mm adapter sleeve are in each well before turning on the reactor Carefully remove the protective foil lid from the DosiCap Zip Unscrew the cap from the vial Carefully pipet 0 5 mL 500 uL of sample into the vial Flip the DosiCap Zip over so the reagent side faces the vial Screw the cap tightly onto the vial Shake the capped vial 2 3 times to dissolve the reagent in the cap Verify that the reagent has dissolved by looking down through the open end of the DosiCap Zip Insert the vial in the DRB200 Reactor Close the protective cover Heat for 1 hour at 100 C After the timer expires carefully remove the hot vial from the reactor Insert it in a test tube rack and allow to cool to room temperature 15 25 C Pipet 0 2 mL 200 uL of Reagent B into the cooled vial Immediately close the Reagent B container Screw a grey DosiCap C onto the vial Invert the capped vial 2 3 times to dissolve the reagent in the DosiCap Wait 10 minutes When the timer expires invert the vial again 2 3 times Clean the outside of the vial with a Kim Wipe and insert it into the DR5000 cell holder The instrument reads the barcode then selects and performs the correct test Results are in mg L PO4 No instrument Zero is required Note and record the indicated values on the bench sheet TNTplus 844 Reactive Phosphoro
8. 24 TB Laboratory QAP September 16 2009 Revision 1 12 3 12 4 12 2 9 12 2 10 12 2 11 12 2 12 12 2 13 12 3 1 12 32 12 3 3 12 3 4 12 4 1 Sample preservation must comply with the requirements of the approved test method Sample volume must be sufficient to perform the necessary analyses Samples must be received within the time specified by the test method Upon receiving a sample the laboratory will determine if the analysis can be performed within the allotted holding time Bypass samples and Town Branch 24 hour composite samples are collected the night before analysis and are delivered to Town Branch Laboratory and kept in a secure location until analysis The chain of custody COC form is stored with the samples Town Branch grab samples West Hickman 24 hour composite samples Blue Sky 24 hour composite samples and Industrial Waste 24 hour composite samples are brought to the Laboratory Analyst during operating hours Verification of Preservation Samples are examined for method preservation and proper documentation During 24 hour composition samples are examined daily for thermal preservation Thermal preservation will be acceptable if e Temperature is either within 2 C or at the method s specified range For samples with a specified temperature of 4 C a temperature of 2 0 to 6 0 C is acceptable e Samples have been hand delivered to the laboratory within 6 hours of collec
9. TB Laboratory QAP September 16 2009 Revision 1 as mg L elemental nitrogen Also present in some groundwater as nitrate and in some polluted groundwater in other forms Nitrogen ammonia Quantity of elemental nitrogen present in the form of ammonia NH3 Ammonia is a chemical combination of Hydrogen H and Nitrogen N occurring extensively in nature The combination used in water and wastewater engineering is expressed as NH3 The protonated form NH coexists with NH water and predominates under conditions of low pH Nitrogen Cycle A graphical presentation of the conservation of matter in nature form living animal matter through dead organic matter various stages of decomposition plant life and the return of living animal matter showing changes which occur in course of the cycle It is used to illustrate biological action and also aerobic and anaerobic acceleration of the transformation of this element by wastewater and sludge treatment Nitrogen Kjeldahl A standard analytical method used to determine the concentration of the organically bound ammonia nitrogen state The method covers the determination of total Kjeldahl nitrogen in surface waters domestic and industrial wastes and saline waters The procedure converts nitrogen components of biological origin such as amino acids proteins and peptides to ammonia but may not convert the nitrogenous compounds of some industrial wastes such as amines nitro compounds hydrazon
10. 0 1 ft for horizontal readings Locations of permanent cross sections and pebble count monitoring will be indicated within the recorded profile Each stream profile will be surveyed twice once at the initial site visit following monument installation and approximately nine months subsequent to first measurement Differences Wolf Run Watershed Page 49 of 67 Revision No 0 Based Plan Date April 11 2011 between these two measurements will allow estimation of changes to channel bed elevation facet slope and facet length B2 2 5 3 Pebble Counts Reach wide pebble counts will be collected within the stream where the longitudinal profiles are taken at the nine hydrogeomorphic monitoring sites If substrate does not appear similar in all riffles riffles with considerably coarser substrate that could be indicative of a large rock fall will be avoided Each reach pebble count will sample within the riffles and pools proportional to the length of the reach comprised of riffles and pools Riffle and pool data will be kept separate but can be combined later to produce a reach average particle distribution For the reach wide pebble counts particle sampling will be completed along evenly spaced transects over the entire bankfull width and consist of at least 100 particles refer to Rosgen 2008 and Bunte and Steven 2001 for pebble count procedures Since much of the bed material in these streams is predominantly sand silt and clay or bedrock a h
11. 1 1 1 1 1 1 1 1 1 1 1 9 Zz O Zz Original COC To Laboratory Accompany Samples amp Report COC Copy TRC Project File COC Copy TRC Laboratory Services Coordinator sje 04 11 11 COC CHAIN OF CUSTODY Page 1 of 1 Client Third Rock Consultants LLC q E WDupy Analytical Report to N SUR Project Name Wolf Run Watershed Based Plan KENTUCKY GEOLOGICAL SURVEY mwooton thirdrockconsultants com Project KY10 030 S Laboratory Services Marcia L Wooton Project Contact sampling Marcia L Wooton la y Third Rock Consultants LLC Phone 859 977 2000 COAL WATER MINERALS 2526 Regency Road Collected By 228 Mining amp Mineral Resources Building University of Kentucky Suite 180 Lexington Kentucky 40506 0107 Lexington KY 40503 859 323 0555 859 977 2000 Matrix Code Preservation Type Turnaround Time Required 30 Working Days pW Suracowater Tiscali usa Preservative Code FF Field Filter Comments eres Ortho Phosphorus to RL of 0 05 mg L NA HNO3 Phosphorus to RL of 0 02 mg L SA H2S04 Nitrate to RL of 0 03 mg L te es TKN to RL of 0 5 mg L a Ice A e Grab q Collection Collection Comp Sample Location Matrix Date Time Wolf Run Old Frankfort Pike Methodology Required 40CFR Part 136 Filtd of Containers Per XN Analysis wot 11_ wo02 11__ WO03 11 __ WO04 11_ _ WO5 11_ WO6 11_ WO7 11_ WO08 11_ WO09 11_ W10 11_ W11 11 W12 11 _ WDD 11 __ Relinquished
12. 2 Filters stuck to the aluminum pan will produce incorrect results re filter sample and reweigh with a new filter if possible QA QC Requirements 9 1 Balance must be calibrated using ASTM Class 1 weight set before analysis 9 2 EPA requires filters with samples be placed back in the oven an reweighed three times Expected Results 10 1 KPDES Plant Effluent Permit Requirements 1 30 mg L for Monthly Average 45 mg L for Weekly Average In the event that analysis results indicate values greater then KPDES permit requirements retest If the value indicated by the retest is greater than KPDES permit requirements Immediately notify the Plant Superintendent and the Laboratory Supervisor 10 2 Process Ranges Typical values mg L for each plant are Town Branch Influent 89 485 30 mL sample Town Branch Effluent 9 31 500 800 mL sample West Hickman Influent 137 513 West Hickman Effluent 2 7 Blue Sky Influent 134 880 Blue Sky Effluent 2 14 Data Analysis and Calculations 11 1 Non filterable residue mg L W2 W1 V 1 000 000 83 12 SOP TSS LFUCG Laboratory Page 84 of 219 Revision Number 3 Last Revised 09 09 Bibliography 12 1 12 2 12 3 12 4 12 5 U S EPA Method 160 2 Residue Non Filterable amp Total Suspended Solids Issued 1971 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washingt
13. 6 PE sample results and raw data Records of Standards and Analytical Reagents 14 3 1 14 3 2 14 3 3 14 3 4 14 3 5 14 3 6 14 3 7 14 3 8 Traceability of standards The laboratory verifies that standards are traceable to National Standards If traceability is not possible the laboratory demonstrates by appropriate means i e analyses of PE samples that the instrumentation and equipment is properly calibrated Receipt and use of reagents and standards The laboratory retains records of the origin purity and traceability of all reagents and standards These records also include the date of receipt storage conditions the date of opening and an expiration date Traceability of working and intermediate standards The laboratory maintains records of traceability from working and intermediate standards to purchased stock standards or neat compounds which include the date or preparation and preparer s initials Identification of prepared reagents and standards All prepared reagents and standards are labeled with the identity the reagent or standard concentration preparation date and preparer s initials Records of Instrument or Equipment Calibrations The laboratory documents and maintains calibration procedures that establish calibration frequency and calibration acceptance criteria All graphs of calibration curves have descriptive titles labeled axes and date of calibration time of calibration tes
14. APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 HACH AutoCat 9000 Chlorine Amperometric Titrator Instruction Manual HACH Company Loveland CO 26 SOP Free Cyanide LFUCG Laboratory Page 27 of 219 Revision Number 3 Last Revised 09 09 Free Cyanide CN F HACH Method 8027 Pyridine Pyrazalone Method Scope Significance to Process and Application 1 1 Measurement of the concentration of free cyanide in industrial wastewater samples Summary of Method 2 1 Discussion The Pyridine Pyrazalone method used for measuring cyanide gives an intense blue color with free cyanide Health amp Safety Precautions 3 1 All municipal and industrial wastewaters are potentially hazardous Gloves and safety glasses should be worn when dispensing these samples 3 2 Cyanides their solutions and Hydrogen cyanide liberated by acids are very poisonous Both gas and solutions can be absorbed through the skin Latex gloves and safety glasses should be used 33 CyaniVer3 CyaniVer 4 and CyaniVer 5 reagent powder pillows are used May be respiratory hazard Sample Handling and Preservation 4 1 Collect samples in glass or plastic bottles and analyze as quickly as possible The presence of oxidizing agents sulfides and fatty acids can cause the loss of cyanide during sample storage
15. Condition Category Habrat Optimal Suboptimal Marginal P Parameter ptima uboptima argina oor 6 Channel Channelization or dredging Some channelization Channelization may be Banks shored with gabion Alteration absent or minimal stream present usually in areas of extensive embankments or cement over 80 of the stream reach channelized and disrupted Instream habitat greatly altered or removed entirely Generally all flat water or shallow riffles poor habitat distance between riffles divided by the width of the stream is a ration of gt 25 20 19 18 17 16 Banks stable evidence of erosion or bank failure absent or minimal little potential for future problems lt 5 of bank affected 15 14 13 12 11 Moderately stable infrequent small areas of erosion mostly healed over 5 30 of bank in reach has areas of erosion 10 9 8 7 6 Moderately unstable 30 60 of bank in reach has areas of erosion high erosion potential during floods 514 3 2 1 _0 Unstable many eroded areas raw areas frequent along straight sections and bends obvious bank sloughing 60 100 of bank has erosional scars Left Bank 10 9 8 7 6 5 4 3 2 1 0 Right Bank 10 9 8 7 6 5 4 3 2 1 0 More than 90 of the 70 90 of the streambank 50 70 of the streambank Less than 50 of the streambank surfaces and Surfaces covered by native surfaces covered by streambank surfaces im
16. Dissolved solids 500 mg L dissolved solids umho cm or mg L OR gt 5 0 mg L WAH gt 4 0 mg L instantaneous Dissolved oxygen mg L 9 1 mg L Total Organic Carbon mg L 3 5 mg L Total Suspended Solids 42 4 mg L mg L Ammonia Nitrogen lt 0 05 mg L unionized NH 0 15 mg L mg L WAH l lt 6 4 mg L Total NH NH N at pH 7 4 and 15 C Nitrate Nitrite lt 10 mg L WS 0 85 mg L Nitrogen mg L Phosphorus total NC 0 15 mg L mg L Sulfate mg L lt 250 mg L DWS 3 Criteria KY Average Values Limits lt 250 mg L DWS lt 600 mg L WAH Fluoride mg L lt 1 0 mg L DWS Not available Parameters Chloride mg L oul scn Calciom mL Magnesium ng L Iron mg L lt 1 0 mg L WAH Aluminum mg L Barium mg L lt 1 0 mg L DWS Cadmium mg L 10 6 mg L 1 34 mg L 6 7 mg L lt 0 001 mg L WAH calculated at hardness 100 lt 0 01 mg L DWS 0 0014 mg L Chromium mg L lt 0 011 mg L WAR 0 0026 mg L calculated at hardness 100 lt 0 05 mg L DWS Lead mg L 0 003 mg L WAH 0 0127 mg L calculated at hardness 100 lt 0 05 mg L DWS Manganese mg L lt 0 05 mg L DWS 0 211 mg L Sodium mg L NC 14 8 mg L Biological Chlorophyll A NC Algal Assays NC CRITERIA WAH Warm Water Aquatic Habitat DWS Domestic Water Supply PCR Primary Contact R
17. Evaluation For each DQI indicate whether the field personnel met the project objectives Document in the comments columns the actual specification for that DQ and explain any non conformances Data Quality Indicator DQ ENE Comments Precision Agreement among repeated measurements of the same property under identical or substantially similar conditions random error i e duplicates Bias Systematic error or persistent distortion of a measurement in one direction Accuracy Overall agreement of a measurement to a known value includes a combination of precision and bias i e difference from known Representativeness Qualitative term expressing the degree to which a portion accurately and precisely represents the whole i e where sampled conditions Completeness Amount of valid data needed to be obtained Ensure all data is recorded and all datasheets are filled out in their entirety Sensitivity Capability to discriminate between measurement responses representing different levels of variable interest i e reporting limit lowest unit of measure Interference Elimination of distorting or inhibiting effects on the measurement Training Documented evidence of meeting all necessary training requirements Yes No Indicates that the task performed in conformance out of conformance with the project s DQI If the DQI is not relevant to the task write N A in t
18. H gt SO to pH lt 2 Alkalinity SM 2320 B TSS TDS Total Hardness Nitrite Ortho phosphorus SM 2540 D EPA 160 1 SM 2340 C SM 4500 NO B EPA 365 1 Plastic 32 oz Plastic 8 oz Ice to lt 6 C Field Filter Cool lt 6 C H SO to pH lt 2 Total phosphorus TKN EPA 365 3 SM 4500 Norg C Plastic 32 oz Cool lt 6 C H SO to pH lt 2 Nitrate EPA 300 0 Plastic 8 oz Ice to lt 6 C TABLE 10 SAMPLE PRESERVATION AND HOLD TIME Deliver To LFUCG Town Branch Laboratory Kentucky Geological Survey Laboratory Macroinvertebrate samples KDOW 2009c B2 2 Sampling Methods 1 Liter wide mouth plastic 95 ethanol B2 2 1 Karst Hydrograph Characterization Because the karst drainage collected by the Prestons Spring Basin emerges as a spring and surface water only surface water discharge methods will be used to characterize the hydrograph of the karst system Surface water discharge Q will be calculated using two variables flow area A and water velocity V according to the equation Q AV However because the velocity is variable across a stream cross section the flow area and velocity must be measured in intervals across the stream and summed as shown in Figure 2 The flow area of each interval is the product of the width w and depth d for that interval The velocity will be measured for each of these areas Third Rock Macroinvertebra
19. Revision History This page documents the revisions over time to this document The most recent iteration should be listed in the first space with consecutive versions following Signatures may be required for revised documents Date of Revision Page s Section s Revision Explanation Revised 04 12 11 All Original preparation date of document Wolf Run Watershed Page 5 of 67 Revision No 0 Based Plan Date April 12 2011 A2 Table Of Contents SECTION A PROJECT MANAGEMENT 000 0 ccccccccccesecsseeseeeeeeseeeeceseeeeeseeeeees 3 A1 Title and Approval Sheet c cccsssccssssecssscecsscecssececssscecsscceesseceessecesssecessneeees 3 A2 Table Of Contents scortare oae o 6 A3 Distrib tion Eist A 9 A4 Project Task Organization oooooononoccnnonccconoccconnnccononccononccononccnno nono no nono nnncnn nano 10 A5 Project Definition Background ooooooonnncconocccnoocccconnocononcconononononocno nono nnnccnnnno 11 A6 Project Task Descripti0N ooooooonnnoccnonncncoonncconnnccononocononccononcnono nono no cnn nn nccnnnnos 13 A6 1 General Overview of Prol diia ieii 13 A6 1 1 Karst Hydrograph Characterization oooncnncnnnnnncnnoncncnconanononononnnonncnnccnncnnnos 17 A6 1 2 C ductivity A 17 A6 1 3 Benthic Macroinvertebrate Collection ooooonnconincninncconncconcconoconnconnncnnncnnn 17 A6 1 4 Watershed Habitat Assessments ccccccscccsseces
20. 2009 Revision 1 Table A4 Data Provided to the Laboratory by Operations Staff Town Branch WWTP Total Influent Flow Peak Flow Rainfall West Hickman WWTP Total Influent Flow Peak Flow Rainfall Nitrification Return Flow Nitrification Waste Flow Total Pounds Chlorine Total Pounds SO Number of Tanks in Service Raw Influent pH Raw Influent DO Combined Influent pH Combined Influent DO Zone 1 Effluent 30 min Settleable Zone 2 Effluent pH Zone 2 Effluent 30 min Settleable Zone 2 Effluent Rise Time Plant Effluent pH Plant Effluent DO Plant Effluent TP Plant Effluent Fecal Coliforms Chlorine Contact Residual Chlorine Plant Effluent Residual Chlorine Creek Above Plant pH Creek Above Plant DO Creek Below Plant pH Creek Below Plant DO Blue Sky WWTP Total Influent Flow Rainfall Raw Influent pH Raw Influent DO Plant Effluent pH Plant Effluent DO Plant Effluent Residual Chlorine TB Laboratory QAP Appendix C September 16 2009 Revision 1 APPENDIX B STAFF RESPONSIBILITIES TB Laboratory QAP Appendix C September 16 2009 Revision 1 Appendix B Staff Responsibilities Class Title LABORATORY SUPERVISOR Reports To Division of Water Quality Director Supervision Exercised Laboratory Technicians General Function Manage the operation and maintenance of the government s wastewater laboratory Performs work of moderate to considerable difficulty in conduc
21. 9 10 11 12 13 14 15 SOP Fecal Coliform LFUCG Laboratory Page 46 of 219 Revision Number 3 Last Revised 09 09 Clean work area with Lysol disinfectant 20 solution Light Bunsen burner with striker Open sterile filter holder Use sterile blue sheet as a sterile field Indicator trip and tape should indicate that the filter has been sterilized Flame forceps and use it to remove the Indicator Strip without touching anything else except the strip Use Petri dishes with sterile pad already in dish Break open ampule of media and pour onto media pad Decant excess media and cover dish to protect sterile pad Place the bottom of the sterile filter holder onto the vacuum flask Flame forceps remove sterilized filter from packaging and place onto sterilized filter holder grid side up Do not touch the filter with anything except the forceps Place or clamp the top unit onto filter holder Gently mix sample In advance determine sample volume that will yield 20 60 fecal coliform units FCU If the volume of sample to be used is 0 1 to 5 mL pour approximately 10 mL of peptone into filter unit before dispensing sample Turn on vacuum after the sample is introduced For sample volumes 5 to 50 mL use sterile pipettes for dispensing into filter unit Do not touch the inside of the filter holder unit Do not allow the pipette tip to touch the filter 46 16 17 18 19 20 21 22
22. Analytical results for Plant operation samples Analytical results for samples obtained from industrial dischargers Results obtained for the PE Sample results that may be integral to on going or possible litigation 18 3 Procedure for Open Records Requests Requests for open records must be made in writing to the Laboratory Supervisor The requests will be reviewed by the Laboratory Supervisor and require final authorization by the Division Director before release of records The request and released records will be filed by the Laboratory Supervisor 37 TB Laboratory QAP September 16 2009 Revision 1 19 1 19 2 19 3 Section 19 Procedures for Internal Audits Annual Internal Audit The Quality Assurance Officer and or Laboratory Supervisor conducts an annual internal audit of the laboratory 19 1 1 This auditor conducts a systematic audit of technical activities from previously prepared checklists 19 1 2 The auditor determines whether the quality assurance practices and other laboratory procedures described or referenced in the QAP have been implemented 19 1 3 The auditor then prepares a written report which includes copies of the check lists and a list of all noted deficiencies Corrective Actions Regarding the Annual Internal Audit Laboratory management takes appropriate corrective actions in response to the internal audit including a written response plan which covers e Completed corrective actions e P
23. DC 1982 U S EPA Method 160 3 Residue Total Gravimetric Dried at 103 105 C Issued 1971 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 160 4 Residue Volatile Gravimetric Ignition at 550 C Issued 1971 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 310 1 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 330 1 Chlorine Total Residual Titrimetric Amperometric Issued 1978 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 335 4 Revision 1 0 August 1993 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 350 2 Distillation procedure Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 365 2 Phosphorous All Forms Colorimetric Ascorbic Acid
24. Environmental Resource Associates Ready To Use Wastewater QC Standards Cat 743 Arvada CO 1 800 ERA 0122 Glutamic Acid Stock Standard C3HsNH gt COOH 2 100 ppm Dry Glutamic Acid in oven at 105 C for 24 hours Cover and place in dissector until cool Dissolve 1 051g in DI water and dilute to 1 L preserve with 2 mL chloroform CHClz Store in refrigerator for no longer than 6 months Nitrate Stock Standard NO3 N 1000 ppm Dry Potassium Nitrate KNO3 in oven at 105 C for 24 hours Cover and place in dissector until cool Dissolve 0 7218g in DI water and bring to 1 L preserve with 2 mL chloroform CHCl Store in refrigerator for no longer than 6 months Nitrate Working Standard 10 ppm Dilute 100 mL of Nitrate Stock Standard to 1000 mL in 1 L flask Preserve with 2 mL chloroform CHCI3 Store in refrigerator for no longer that 6 months 5 Procedure A Turn on the CEM MSP 1000 Microwave Digestion Unit and allow it to warm up for at least 15 minutes B Standards Prep 1 Using the 100 ppm Glutamic Acid Stock Standard prepare the following a 0 4 ppm 1 mL of 100 ppm diluted to 250 mL b 0 8 ppm 2 mL of 100 ppm diluted to 250 mL c 1 6ppm 4 mL of 100 ppm diluted to 250 mL 2 Using the 10 ppm Nitric Stock Standard prepare the following 0 1 ppm mL of 10 ppm diluted to 100 mL 0 2 ppm 2 mL of 10 ppm diluted to 100 mL 0 4 ppm 4 mL of 10 ppm diluted to 100 mL 0 8 ppm 8 mL of 10 ppm diluted to 1
25. Federation Washington DC 2005 12 3 U S EPA Method 365 2 Phosphorous All Forms Colorimetric Ascorbic Acid Single Reagent Revised March 1983 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 28 APPENDIX D LABORATORY BENCHSHEETS cd pH Meter Calibration irst Buffer 7 00 pH econd Buffer 4 00 pH TOWN BRANCH amp WESTHICKMAN WASTEWATER TREATMENT PLANT Town Branch Laboratory Grab Samples pH Method EPA Method 150 1 pH Electrometric Issued 1971 Editorial revision 1978 and 1982 Second Calibration Enter Date Jo First Buffer Second Buffer 4 00 pH SS Third Buffer 10 00 pH Slope Calibrated By 7 00 pH hird Buffer 10 00 pH pH _ Sample Name Date Samples Collected ime Analysis Started E H Standard Units Analyst Date Analysis Completed KPDES Permit Limits on Plant Effluent 6 0 mg L is the Lowest pH we can have on any given sample 9 0 mg L is the Highest pH we can have on any given sample Total Alkalinity Orion Research Incorporated Laboratory Products Group po Sample Name Date Samples Collected ime Analysis Started Volume of Sample mL D Total Alkalinity A D mg L as CaCO Blank Date Analysis Completed Presevation None required Analyze Immediately S Ma O NTE PTE ph Time sampled Time receiv
26. Fill Titrator with Sodium Thiosulfate 0 025N 4169 Titrate until sample color is pale yellow DO NOT DISTURB TITRATOR Add 8 drops of Starch Indicator 4170WT Continue titration until blue color just disappears and solution is colorless Read result in ppm Dissolved Oxygen LaMOTTE COMPANY Helping People Solve Analytical Challenges PO Box 329 e Chestertown Maryland 21620 USA 800 344 3100 410 778 3100 Outside U S A Fax 410 778 6394 Visit us on the web at www lamotte com 67414 MN 4 07 19 Watershed Watch Project Procedures Collecting Samples for Laboratory Analysis Version 3 0 2005 10 11 Watershed Watch Sample Collection Methods Table of Contents Introduction a Background Watershed Watch in Kentucky b Overview Watershed Watch s Synoptic Sampling Program Data Rigor Training Planning a Synoptic Sampling Event a Sampling Event Coordinator b Selection of Laboratory Sampling Site Selection a Objectives b Maps c Rationale d Accessibility and Appropriateness e Health and Safety Location and Description of Sampling Sites a Diagram Depicting Physical Setting b Coordinates c Photographs Sample Materials a Containers and Preservatives b Preprinted Forms and Instructions Sampling Procedures a Completing the Chain of Custody form b In stream sampling Location and Approach d Sampling for Parameters other than Bacteria d Sampling for b
27. Four 1 5V alkaline batteries Eveready A76BP supplied 150 hrs continuous use Alternate replacement Model Eveready 303 silver oxide 70 hrs continuous use Dimensions 6 5 L x 1 5 dia 165 x 38mm Weight 3 25 oz 90 gms Electrode replacement You can replace the electrode module at the fraction of the cost of a new Testr When the Testr fails to calibrate gives fluctuating readings in buffers shows error messages E2 or OR in a buffer and the procedures in the Maintenance section do not help you need to change the electrode 1 With dry hands grip the ribbed Testr collar with electrode facing you Twist the collar counter clockwise see diagram A Save the ribbed Testr collar and O ring for later use Rotate collar away from you A SS SS gt A 2 Pull the old electrode module away from the Testr 3 Align the four tabs on the new module so they match the four slots on the testr see diagram B Y Small O Ring hidden Large O Ring o J WATERPROOF Small Tab Large Tab Electrode module Insert Electrode 4 Gently push the module onto the slots to seat it in position Push the smaller O ring fully onto the new electrode module Push the col lar over the module and thread it into place by firmly twisting clockwise Warranty Each TDSTestr and ECTestr meter body is war ranted against defects in materials and work manship for a period of
28. Lite Goose Creek near Hurmads Creek e o o o re 03292480 o 90 BEARGRASS CREEK BASIN South Fork Beargrass Creek at Louisville dc ee 03292500 IS South Fork Beargrass Creek at Winter Avenue at Louisville o ooo 03292550 02 0 aaa 393 Middle Fork Beargrass Cecek at Louisville dc 00 ooo o A ee 94 Middle Fork Beargrass Creek at Scenic Loop at Lowisyile c oo OS293200 co o 96 Muddy Fork at Mockingbird Valley Road at Louisville 0 ooo oo 03293530 ooo 4 7 Ohio River at Louisvidle ee 89294500 2 0 ee 98 MILL CREEK BASIN MIR Creek Cutoff near Louisville O 03294550 2 90 Mill Creek at Orell Road ness Louisville Eh 03294570 0 aaa aa 100 SALT RIVER BASIN Salt River at Gleasborn td o 03295400 2 aaa IH Brashears Creek at Taylorsville d aaa aaee 03295890 aaa 102 Floyds Fork Floyds Fork near Pewee Valley Q 0 es O3297900 cc ee 103 Long Run near Fisherville 0 oaaao OSZ9T9RO o 104 Floyds Fork at Fisherville 8 0 O3298000 2 ee 105 Pope Lick at Pope Lick Road near Middletown 0c 2 ooo OR29R 100 a sed age Gc e hes 107 Chenoweth Run at Gelhaus Lane near Fora Creek ce 0 o ORIBE oe 108 Floyds Fork neas Mount Washington da ooo 03298200 aa 109 Cedar Creek at Fairmount Road near Mt Washington Ky 0 oo 2 OIEA o 10 Cedar Creek at Thixion Road near Louisville c o ee M3298250 00 0000 02004 RG Pennsylvania Run at Mt Washington Road near Louisville fc o
29. Loveland CO 2008 Standard Methods Part 4500 P Phosphorous APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 U S EPA Method 365 1 Phosphorous All Forms Colorimetric Automated Ascorbic Acid Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 365 3 Phosphorous All Forms Colorimetric Ascorbic Acid Two Reagent Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 77 SOP Settleable Solids LFUCG Laboratory Page 78 of 219 Revision Number 3 Last Revised 09 09 Settleable Solids EPA Method 160 5 Residue Settleable Matter Standard Methods Part 2540 F Scope Significance to Process and Application 1 1 This method is applicable to surface and saline waters domestic and industrial wastes 1 2 The practical lower limit of the determination is about 1 mL L hour Summary of Method 2 1 Executive Summary Settleable solids is the term used for material settling out of suspension within a defined period of time It may include floating material depending on the technique Solids analyses are important in the control of bio
30. Macroinvertebrates and Fish Second Edition EPA 841 B 99 002 USEPA Office of Water Washington D C Bunte Kristin Abt Steven R 2001 Sampling surface and subsurface particle size distributions in wadable gravel and cobble bed streams for analyses in sediment transport hydraulics and streambed monitoring Gen Tech Rep RMRS GTR 74 Fort Collins CO U S Department of Agriculture Forest Service Rocky Mountain Research Station 428 p Compton M C G J Pond and J F Brumley 2003 Development and application of the Kentucky Index of Biotic Integrity KIBI Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky Harrelson C C C L Rawlins and J P Potyondy 1994 Stream channel reference sites An illustrated guide to field technique General Technical Report RM 245 Fort Collins CO U S Department of Agriculture Forest Service Rocky Mountain Forest and Range Experiment Station 61p In Situ Inc 2006 Level TROLL Operator s Manual www in situ com Kentucky Division of Water KDOW 2004 Project Final Report Guidelines for Clean Water Act 319 h Funded Projects Kentucky Energy and Environment Cabinet Department for Environmental Protection Division of Water Watershed Management Branch Nonpoint Source Section KDOW 2008 Methods for Assessing Biological Integrity of Surface Waters in Kentucky Kentucky Department of Environmental Protection KDOW 2009a In situ Water Quality
31. On the field data sheet record the nearest bank REW LEW as 0 Record the farthest bank as the total width of the stream Wolf Run Watershed Page 38 of 67 Revision No 0 Based Plan Date April 11 2011 6 Have one person stand at the starting point on the tagline and a second person stand at the point designated as the end of the run The person at the end of the run should use a stopwatch that can measure to tenths of a second 7 The person at the starting point will throw a floating object large stick orange hedge apple etc just upstream of the top cross section within the first longitudinal profile area When the object crosses the upstream cross section the person will say start and the person at the end of the run will start the timer 8 When the object crosses the downstream cross section the person with the timer will stop the timer 9 Record the distance the object traveled and the number of seconds to the tenths of a second the object took to travel that distance 10 Repeat Steps 6 9 for the remaining profiles Velocity and flow area measurements must manually be recorded in a bound field book or on other appropriate field data sheets using indelible waterproof ink and waterproof paper Discharge values are to be calculated in the office according to the equations specified in KDOW 2010b In addition to the discharge measurements collected temporary water level gages pressure transducers with data logg
32. Ortho phosphate Table A1 Town Branch Laboratory Analysis List Analysis Requirements Required Required Required Required Required Required Required Required Required Required Required Required Required Required Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation September 16 2009 TB Laboratory QAP Appendix A Revision 1 Sample Name Creek Above Plant Tap Water Mixed Liquor Return Activated Sludge R A S Raw Sludge to Thickener Raw Sludge Thicken Sludge Raw Sludge Thickener Overflow Combined Sludge Density Meter Analysis pH Dissolved Oxygen CBOD TSS Ammonia Settleable Total Phosphorus Ortho phosphate Hardness Fecal Coliforms Metals Total Total Phosphorus pH Total Alkalinity Inf Total Alkalinity Eff Settleable MLTSS MLVSS SVI SDI Rise Time Micro Exam pH TSS VSS Total Solids pH Total Solids Volatile Solids Total Solids TSS Total Phosphorus Total Solids Volatile Solids Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Oper
33. Physical Demands and Working Conditions e Physical demands include standing lifting carrying and walking e Must have the strength and agility to allow the employee to perform job duties which would be found at the level of medium work i e exerting 20 to 50 pounds of force as defined in the PAQ e Working conditions include performing a majority of job duties indoors with wet and humid surroundings fumes odors and chemicals Knowledge Skills and Abilities Considerable knowledge of e the occupational hazards and safety precautions necessary relative to the area of assignment e the elementary principles practices and techniques of bacteriology and chemistry e the operation maintenance and calibration of standard and complex chemical laboratory equipment Good knowledge of e the elementary principles practices and techniques of bacteriology and chemistry e personal computers and related software used in the field e the operation and care of standard chemical laboratory equipment Ability to perform standard chemical and bacteriological tests accurately follow oral and written instructions exactly prepare reports on the results of laboratory tests performed establish and maintain effective working relationships with fellow employees and other involved parties e understand set up and run standard laboratory tests on wastewater and sludge per standard methods Special Requirements e May be required
34. Reach mixing sites near major tributaries or point sources should be avoided to minimize backwater effects or poorly mixed flows Proximity to major man made disturbances like bridges or dams and Known health risks in the stream e g proximity to a treatment plant or straight pipes e Health and Safety The following health and safety factors are addressed in the training Notifying others of itinerary and whereabouts Never visiting an isolated site alone Never sampling in high water Bewaring of hunters poisonous reptiles and sudden high water Carrying identification Taking a cellular phone when available and Wearing disposable powderless gloves when handling sample preservatives such as acid 5 Location and Description of Sampling Sites a Diagram depicting physical setting The Volunteer Monitor documents the physical setting of the site using a standard form Physical Characterization Water Quality Field Data Sheet which may be found in Appendix D b Coordinates Latitude and longitude are determined for the site in one of two ways e The Volunteer Monitor determines them using a handheld GPS unit and submits the coordinates with the Physical Characterization form In this instance the GPS unit must be tuned to the coordinate specifications called for in http kywater org dow gps or e Acopy of the 1 24 000 topographic map for the stream reach is mailed to the Volunteer Monitor with the
35. Run 4 blanks with each batch 3 seeded one unseeded Run 1 random duplicate per 20 samples Data acceptance criteria Analysis values for GGA Standards should be 198 mg L 30 5 mg L Duplicate values must agree within 5 Blank depletion values must be no greater than 0 2 mg L If these criteria are not met corrective action is indicated See Quality Assurance Program QAP Sec 15 Corrective Action Policies and Procedures 19 10 11 SOP CBOD LFUCG Laboratory Page 20 of 219 Revision Number 5 Last Revised 09 09 Expected Results 10 1 KPDES Permit Requirements PTE 10 mg L maximum for monthly average and 15 mg L maximum for weekly average In the event that analysis results indicate values greater then KPDES permit requirements notify the Plant Superintendent and Laboratory Supervisor 10 2 Process Ranges Influent BOD values vary with season rainfall amounts and influent flow rate Typical influent values for Town Branch Plant range 200 mg L to 50 mg L with an average of approximately 130 mg L West Hickman Plant influent values range from 250 mg L to 50 mg L with an average of approximately 180 mg L Typical effluent BOD values at both Town Branch and West Hickman are lt 10 mg L Data Analysis and Calculations Initial and final dissolved oxygen values are entered into the BOD CBOD worksheet which calculates the BOD or CBOD values in accordance with the following Given B initial DO reading o
36. See Section 8 4 3 of the Users Manual 7 2 Reactive gas chlorine and hydrogen sulfide 7 3 Air bubbles in sample or on surface of probe tip SOP WH FIELD D O West Hickman WWTP Laboratory Page 4 of 219 Revision Number 3 Last Revised 09 09 Procedures 8 1 Calibration and Start Up It is suggested that at the Users Manual be initially consulted when following these procedures 1 2 3 4 5 6 7 Press the power button on the HQ40d and allow the unit to perform its startup self check routine Clean by rinsing with Nanopure lab water then blot dry the probes tip with a Kim Wipe Inspect the probe tip for indications contamination or damage Take a 300 mL BOD bottle containing approximately one inch of lab water cap and shake remove cap and replace it with the probe Press Calibrate blue button the meter will prompt you to Dry the probe and place in water saturated air amp press Read Press Read the screen will scroll from 0 to 100 then indicate Calibration Complete Record from display screen both the temperature and the dissolved oxygen value indicated under the temperature Log the values on the dissolved oxygen calibration section of the Dissolved Oxygen bench sheet under D Temperature and E Dissolved Oxygen from HQ40d Note the barometric pressure value from the laboratory barometer located adjacent to the D O meter and record on the dissolved oxygen calibration sect
37. Single Reagent Revised March 1983 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 405 1 Biochemical Oxygen Demand 5 Days 20 C Issued 1971 Editorial revision 1974 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S 53 TB Laboratory QAP September 16 2009 Revision 1 Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Microbiological Methods for Monitoring the Environment Water and Wastes EPA 600 8 78 017 U S Environmental Protection Agency Environmental Monitoring and Support Laboratory Office of Research and Development Washington DC 1978 page 124 Water Pollution Control Federation Simplified Laboratory Procedures for Wastewater Examination Third Edition 1985 54 APPENDIX A LABORATORY ANALYSIS LIST TB Laboratory QAP Appendix A Revision 1 Sample Name Raw Influent Plant Effluent Raw Influent Primary Influent Primary Effluent Plant Effluent Analysis CBOD TSS Ammonia pH Dissolved Oxygen CBOD TSS Ammonia Total Phosphorus Hardness Fecal Coliforms Residual Chlorine Metals Dissolved Metals Total pH Dissolved Oxygen Settleable Total Phosphorus Ortho phosphate Metals Dissolved Metals Total CBOD Settleable TSS CBOD Settleable TSS Settleable
38. The QAPP completion and approval is expected to occur in April 2011 prior to the initial volunteer training If the QAPP approval is delayed beyond April the monitoring schedule will be delayed a similar period The first volunteer training event is scheduled for April 16 2011 with four total training sessions planned FOWR and its Science Advisors are to conduct these training sessions in accordance with this QAPP Wolf Run Watershed Page 19 of 67 Revision No 0 Based Plan Date April 11 2011 The Wolf Run Watershed Council will meet on a quarterly basis at minimum Progress reports on the monitoring activities will be presented at these meetings For the karst hydrograph characterization data loggers will be installed in May 2011 Subsequent to their installation the base flow event and wet weather event will be monitored during the respective weather conditions A rainfall event of 1 inch will qualify as a wet weather event Both events are expected to occur by the end of August 2011 if weather conditions allow Data analysis will follow the events with the expected completion data of the report in May 2012 Trained volunteer samplers will conduct the conductivity survey during medium to low flow conditions 0 5 to 5 cfs at the USGS gage Unless interrupted by a precipitation event the survey will be completed over a one week period such that the results reflect a snapshot of watershed conditions Ifa precipitation event occur
39. Town Branch Laboratory Grab Samples Total Solids Method Residue Total EPA Method 160 3 Gravimetric Dried at 103 105 C Issued 1971 Total Volatile Solids Method Residue Volatile EPA Method 160 4 Gravimetric Ignition at 550 C Issued 1971 Enter Date Date Sample Collected Time Analysis Started Wt Tare amp Wet Sample W gm Wt Tare W gm Wt Tare amp Dried Solids W gm Wt Tare amp Ashed Solids W gm Date Analyses Performed Analyst Setting Up Analysis Analyst Reading amp Calculating Analysis QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS Log book Monday Tbmonsht xls TB Total Solids Grab cI d TOWN BRANCH WASTEWATER TREATMENT PLANT Town Branch Laboratory 24 Hour Composite Samples Settleable Matter Method EPA Method 160 5 Settleable Matter Volumetric Imhoff Cone Issued 1974 Settleable Matter Enter Date 12 1 2 1 03 4 a TD 5 u 19 Log Number Sample Name PT Date Samples Collected Alia gt aia A MiS a gt lie e RBA Vessel Used Imhoff Cone Imhoff Cone Imhoff Cone Time Analysis Started NAAA ee Settleable Matter 60 minutes mL L Hr Analyst Date Analysis Completed QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS Presevation None required Maximum Holding Time 48 hours Settleable Matter Settlometer TOWN BRANCH WASTEWATER TREATMENT PLANT Town Branch Laboratory Grab
40. Unless interrupted by a precipitation event the survey should be completed over a one week period If a precipitation event occurs during this period the survey will resume when water levels are consistent with the initial survey conditions A6 1 3 Benthic Macroinvertebrate Collection Macroinvertebrate samples will be collected at six sites within the Wolf Run watershed in addition to the site at the mouth of Wolf Run which is monitored for macroinvertebrates under the MS4 permit The six sites are located on Vaughn s Branch Big Elm Tributary Cardinal Run McConnell Branch and two sites on Wolf Run one upstream of Harrodsburg Road one upstream of Versailles Road These sites are identified on Exhibit 1 The macroinvertebrate community at each site will be sampled using the recommended methods developed by KDOW 2009b 2009c which involve the collection of two separate samples riffle and multihabitat The riffle sample consists of four 0 25 meters m samples collected from two separate riffles at each station using a 0 25 m grid and a kicknet 600um mesh Riffle collections at each station will be composited to form one semi quantitative sample The qualitative multihabitat sample includes where habitat is available samples from leaf packs sticks wood bedrock slabrock undercut banks submerged roots aquatic macrophyte beds soft sediment using a U S 10 sieve Wolf Run Watershed Page 17 of 67 Revision No 0 Based P
41. changes in stability of standard incomplete protein precipitation etc Zinc Zn Zinc is ubiquitous in the environment so that it is present in most foodstuffs water and air 50 TB Laboratory QAP September 16 2009 Revision 1 Section 23 Bibliography Code of Federal Regulations CFR 2003 Guidelines Establishing Test Procedures for the Analysis of Pollutants 40 CFR 136 3 Title 40 Chapter 1 U S Environmental Protection Agency pg 5 337 Fisher Scientific AR50 Fisher Scientific User Manual Fisher Scientific Inc HACH AutoCat 9000 Chlorine Amperometric Titrator Instruction Manual HACH Company Loveland CO HACH DR 4000 Handbook Method 8083 Procedure Code N 3 Nessler Method following distillation HACH Company Loveland CO HACH DR 4000 procedure method 8027 HACH Company Loveland CO HACH DR 4000 Procedure Manual EPA approved Method 8190 Phosphorus Total HACH Company Loveland CO HACH HQ Series Portable Meter Users Manual September 2006 Edition 5 HACH Company Loveland CO HACH Water Analysis Handbook Method 8023 Chromium Hexavalent 1 5 Diphenylcarbohydrazide Method 2 Edition 1992 HACH Company Loveland CO HACH Water Analysis Handbook Method 8213 Hardness Total with a Digital Titrator 2 Edition 1992 HACH Company Loveland CO HACH Water Analysis Handbook Method 8291 Volatile Acids Buret Titration Method gnd Edition 1992 HACH Company Loveland CO Memorandum EPA R
42. e Prepares reagents and mixtures as required for laboratory testing Sample Testing Analysis e Conducts a variety of laboratory analyses in accordance with government regulations to include pH biochemical oxygen demand suspended and total solids volatile solids chemical concentrations alkalinity and other e Conducts routine bacteriological examination on wastewater samples Conducts microorganism counts of activated sludge e Makes dissolved oxygen and pH readings in the field when requested Recording Reporting Results e Records all data on worksheets and monthly sheets e Prepares monthly reports e Maintains inventory of supplies by informing Laboratory Supervisor when inventories get low Miscellaneous e Travels to West Hickman WWTP Laboratory to calibrate equipment and or run analyses on request e Maintains special laboratory programs such as safety quality control or quality assurance e Answers telephone inquiries and relays messages and information e May be assigned to perform duties of higher or lower level classifications in this or related class series and or perform duties on a temporary or acting basis in accordance B 4 TB Laboratory QAP Appendix C September 16 2009 Revision 1 with Ordinances 21 15 and 21 16 and or act as a lead worker e Responsible for knowing and complying with all UCG and division safety rules and for attending safety meetings Performs other related duties as required
43. edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Standard Methods Part 2540 E Fixed and Volatile Solids Ignited at 550 C APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Standard Methods Part 2540 F Settleable Solids APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Standard Methods Part 3500 B Chromium Colorimetric Method APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Standard Methods 4500 Cl D Chlorine Residual Amperometric Titration Method APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Standard Methods Part 4500 P Phosphorous APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Wash
44. onnorn mol Neer OPS M5 00N1L 0n MmMO tTwWOD OON tT 0010 Do0m0 m 010010 0 aAtTNOD tTwWood T0MO7 onane NOOO O MMOD aoonn aoarwno amome ne HK ON 0MNr O 050000 Omoto Oooo Oman Oo Onomod OmMwWoan anonor or ma toot m oe SNM MA on storm SNR wM WOAON oeer te O t OO an oaoct anno 0M O FNO 010 o0mn NO 0 NI NAEROSSON 0 010 m0 11 12 13 14 15 NOR OM 0 0010 5 nm NANOS wowotwe aanmot OLOO 1 00 nortom NOYO ooonn ONYO MmYOO anonnm onore NO OM tnwWOo Neye MID NONT N 010 OM NWOAN owoww enpo NOYO em O em em em onnnw noststn 1 0N 0 ONDOY Korov nTOnRN Somo Oteo oronw NONN e wo wood vooo nnen oatan QOo od oOnmnwnoe Nenen o omogo myoom TONON OMMOYAN NNOO TOMN 0 Povon ONMYO mpe NOOO MMN POON ooog 0010 0 novtoo tTocN lt DOMON ot OPM 21 22 23 24 25 H N TOM ONY Oonwee otOr O 00 10 00 0 00 00500 00m won A MKONGO ouen ostnono NOMW OD 7300M0 NOe OO wanes 00m NNN WO aovrtsto NEO WON Nowonm Nenog TM O00 Y M0 ANADO 0 N 00 Or O OMOo 1 ONONO Qet oE e e 2 EE a OONO ONNO Y 26 27 28 29 30 Field Sampling Audit Checklist General Information Project No Description Field Personnel Methods Reviewed Associated SOP manual or quality standard
45. so that its concentration falls between 0 010 ppm and 1 000 ppm The sample must be diluted using volumetric flasks and pipettes 8 Method Performance The method detection limit MDL should be established by determining seven replicates that are 2 to 5 times the instrument detection limit The MDL is defined as the minimum concentration that can be measured and reported with 99 confidence that the analyte concentration is greater than zero and is determined from analysis of a sample in a given matrix containing the analyte MDL E 1 10 99 S where t the t statistic for n number of replicates used n number of replicates S standard deviation of replicates 9 References U S EPA Method 365 3 1978 Standard Methods for the Examination of Water and Wastewater 20 edition 1998 Method 4500 P E pg 4 146 01 2009 KGS 9056 TKN amp Total Nitrogen by Ion Chromatography of Water 1 Discussion Principle This method addresses the sequential determination of the following inorganic anions bromide chloride fluoride nitrate Kjeldahl nitrogen total nitrogen and sulfate A small volume of water sample is injected into an ion chromatograph to flush and fill a constant volume sample loop The sample is then injected into a stream of carbonate bicarbonate eluent The sample is pumped through three different ion exchange columns and into a conductivity detector The first two columns a precolumn or guard column and a sep
46. streams and rivers ground water and treatment facilities requires the analyst to utilize a number of tests and test methods The sampling selected for study are intended to profile water quality in the water bodies in the project area The Kentucky Department for Environmental Protection uses methods for analysis as approved by the United States Environmental Protection Agency USEPA The parameters and test methods are shown below Criteria and Kentucky average values for these parameters are presented in Table L PARAMETER Field Data Temperature pH Conductivity Dissolved Oxygen Laboratory Analysis pH Total Organic Carbon Total Suspended Solids Ammonia Nitrogen Nitrate Nitrite Nitrogen Phosphorus total Bromide Fluoride Sulfate Chloride Metal Scan Aluminum Barium Cadmium Calcium Chromium Iron Lead Magnesium Manganese Sodium Zinc Biological Analysis Chlorophyll A Algael assays USEPA ANALYTICAL METHOD Thermometer Colorometric Specific Conductance Modified Winkler Electrometric UV Promoted Gravimetric lon Chromatography lon Chromatography Spectrometric lon Chromatography lon Chromatography Spectrometric lon Chromatography ICP Es TABLE 1 Parameters Criteria KY Average Values Temperature C lt 22 2 C 72 F Avg Oct 16 31 WAH lt 25 C 77 F instantaneous maximum WAH Conductivity lt 800 micromhos cm or 335 umhos cm
47. 0 C 0 5 C for 24 2 hours Log initials time and date in the Microbiology bench sheet After 24 2 hours count the colonies Use a 10 to 15X stereoscopic microscope if necessary If no red or blue colonies appear the sample can be considered negative If red or blue colonies appear at 24 hours incubation the result is positive for total coliforms or E coli respectively No confirmation step is required Log results initials time and date in the Microbiology bench sheet 57 SOP Total Coliforms and E coli LFUCG Laboratory Page 58 of 219 Revision Number 1 Last Revised 09 09 8 2 Before and After Blanks 1 2 3 4 5 6 7 8 9 10 11 Blanks must be analyzed before and after filtration of a set of samples Before any sample is filtered place a sterile filter in the filter holder unit Add 50 mL peptone buffer to filter unit Turn on vacuum and filter the buffer this will be the Before Blank Remove and plate filter as indicated in Section 8 1 Proceed with sample filtration and plating Place a sterile filter in the filter holder unit Add 50 mL peptone buffer to filter unit Turn on vacuum and filter the buffer this will be the After Blank Remove and plate filter as indicated in Section 8 1 Log results initials time and date in the Microbiology bench sheet 8 3 Peptone Buffer Preparation See SOP Fecal Coliform Section 8 4 for peptone buffer preparation 8 4 Helpful Hints
48. 09 2 West Hickman WWTP Raw Effluent 214 27 1 Zone 1 Effluent 177 10 7 Zone 2 Effluent 170 15 8 Return Activated Sludge 284 26 2 Data Analysis and Calculations 11 1 Calculations determined by dilution 11 2 See following pages for alkalinity concentration tables Bibliography 12 1 U S EPA Method 310 1 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 12 2 Standard Methods 2320 B APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21th edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 12 3 Total Alkalinity Measurement in Natural Waters Application Information Procedure 517 Thermo Fisher Scientific Inc http www thermo com com cda products product_application_details 1 11636 0 0 html SOP Alkalinity LFUCG Laboratory Page 6 of 219 Revision Number 2 Last Revised 9 09 ORION Total Alkalinity Test Kit LOW RANGE 0 to 25 mg L as CaCO3 Add 1 mL of ORION Total Alkalinity Reagent to 100 mL and mix well Measure pH of mixture and read total alkalinity from this table Observed Total Observed Total Observed Total Observed Total Observed Total pH Alkalinity pH Alkalinity pH Alkalinity pH Alkalinity pH Alkalinity 4 00 0 0 4 35 5 4 4 70 10 9 5 05 16 4 5 40 21 9 4 01 0 1 4 36 5 6 4 71 11 1 5
49. 1 000 000 11 2 Total Solids mg L W3 W1 W2 W 100 87 12 SOP Total Solids LFUCG Laboratory Page 88 of 219 Revision Number 3 Last Revised 09 09 Bibliography 12 1 12 2 12 3 12 4 U S EPA Method 160 3 Residue Total Gravimetric Dried at 103 105 C Issued 1971 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 Standard Methods Part 2540 B Total Solids dried at 103 C to 105 C APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Code of Federal Regulations CFR Guidelines Establishing Test Procedures for the Analysis of Pollutants 40 CFR 136 3 Title 40 Chapter 1 U S Environmental Protection Agency U S Environmental Protection Agency pg 5 337 2003 Simplified Laboratory Procedures for Wastewater Examination Water Pollution Control Federation Third Edition pg 25 27 1985 88 SOP Volatile Acids LFUCG Laboratory Page 89 of 219 Revision Number 3 Last Revised 09 09 Volatile Acids Standard Methods Part 5560 C Distillation Method HACH Method 8291 Buret Titration Method Scope Significance to Process and Application 1 1 This technique recovers acids containing up to six carbon atoms 1 2 Fracti
50. 2 The practical range of the determination is 10 mg L to 20 000 mg L Summary of Method 2 1 Executive Summary Total solids are the material residue left in a vessel after evaporation of a sample and subsequent oven drying at a defined temperature Total suspended solids TSS is the portion of total solids that is retained by filter Solids analyses are important in the control of biological and physical wastewater treatment processes and for assessing compliance with regulatory agency effluent limitations 2 2 Discussion A well mixed sample is filtered through a standard filter and the residue retained on the filter is dried to constant weight at 103 C to 105 C The filtrate from this method may be used for Residue Total filterable Health amp Safety Precautions 3 1 Watch out for broken glass from crucibles cylinders and beakers 32 Wastewater samples should be considered potentially hazardous Use proper personal protective equipment 3 3 Crucibles can be hot 103 C to 105 C use proper gloves when handling Sample Handling and Preservation 4 1 Collect samples in plastic or glass containers 4 2 No preservative required 4 3 Maximum holding time 7 days Reagents 5 1 Drierite 8 mesh 5 2 Nanopure Grade water 81 SOP TSS LFUCG Laboratory Page 82 of 219 Revision Number 3 Last Revised 09 09 Equipment amp Lab Ware 6 1 Analytical Balance 6 2 ASTM Class 1 weight set 6 3 Environmental Express
51. 2 mL of Hydrochloric Acid Store at 4 C 39 F or less Preserved samples may be stored up to 28 days Before analysis warm stored samples to 20 23 C 68 73 4 F and neutralize to pH 7 0 with 5 0 N Sodium Hydroxide Correct the test result for volume additions Reagents and Lab Equipment 5 1 Ammonia TNTplus ULR Reagent Set HACH TNT830 5 2 Ammonia TNTplus LR Reagent Set HACH TNT831 5 3 Ammonia TNTplus HR Reagent Set HACH TNT832 5 4 Pipetors 100 1000 uL 1 5 mL 5 5 Pipet Tips 5 6 Nitrogen Ammonia Standard Solution 1 0 mg L NH3 N HACH 189149 5 7 Nanopure Water 5 8 Hydrochloric Acid Standard Solution 1N 5 9 Hydrochloric Acid concentrated ACS 5 10 Sodium Hydroxide Standard Solution IN HACH 104532 5 11 Test Tube Rack for 13 mm vial 5 12 DRB200 Reactor 115 V 9x13mm Interferences 6 1 The ions listed in the Interfering substances table have been individually tested up to the given concentrations and do not cause interference The cumulative effects of these ions or the influence of other ions have not been determined 6 2 Primary amines are determined and cause high bias results A 10 000 fold excess of urea does not interfere All reducing agents interfere and cause low bias results 6 3 Important Note An analyte concentration greatly in excess of the stated range will adversely affect color formation resulting in a false reading within the method range 6 4 Measurement resu
52. 2010 at http lexingtonky gov modules ShowDocument aspx documentid 3572 United States Environmental Protection Agency US EPA March 2008 Handbook for Developing Watershed Plans to Restore and Protect Our Waters Office of Water Nonpoint Source Control Branch EPA 841 B 08 002 Wolf Run Watershed Page 65 of 67 Revision No 0 Based Plan Date April 11 2011 APPENDIX A DATASHEETS Wolf Run Watershed Page 66 of 67 Revision No 0 Based Plan Date April 11 2011 Volunteer Monitoring Participant Agreement Please fill this out keep one and turn one in Please Print Name Best Phone Organization Shipping Address City State Zip E mail I to the best of my ability will Check those that apply 1 _ Conduct Field Chemistry D O pH Conductivity Temp 2 ___Collect Grab Samples 3 Take Photographs 4 __ Read and follow the Project Quality Assurance Project Plan 5 __ Return equipment when retire from the project 6 Equipment checked out to me KIT 10 Lab Analysis Sample Sights Requested ID Stream Name Sampling Site Map Reference 11 ____ understand and agree that the stream can be a dangerous place the project organizers cannot protect me from slick banks high water snakes falling timber and other hazards will ask permission before crossing private property will be on my guard and exercise due caution when handling chemicals The information above is c
53. 23 24 25 26 27 28 29 30 31 32 33 SOP Fecal Coliform LFUCG Laboratory Page 47 of 219 Revision Number 3 Last Revised 09 09 For sample volumes 50 to 100 mL pour sample into cylinder and use the scale on the side of the cylinder for measurement Turn on vacuum Once sample has filtered through turn off vacuum Rinse top of the filter unit with peptone two times using autoclaved peptone in a Nalgene squeeze bottle Turn on vacuum to drain peptone Turn off vacuum Flame forceps Remove top of the filter unit and place on the sterile blue field Open Petri dish Use sterile flamed forceps to grab the edge of the filter and remove it from the filter holder unit Place filter grid side up onto edge of the Petri dish and gently slide it onto the surface of the media saturated pad Replace Petri dish cover Place Petri dishes into a 4 5 X 9 inch sterile sampling bag Make sure not contaminate the inside of the bag Seal bag Place bag with Petri dishes face down into water bath at 44 5 C 0 2 C for 24 2 hours Log initials time and date in the Microbiology bench sheet After 24 2 hours count blue colonies See Section 10 Log results initials time and date in the Microbiology bench sheet 47 8 2 8 3 SOP Fecal Coliform LFUCG Laboratory Page 48 of 219 Revision Number 3 Last Revised 09 09 Before and After Blanks 1 Blanks must be analyzed b
54. 57 Adm nistr tv a o e a ones 30 14 6 Laboratory Record Entries and Change of Entries ooooonccncnoconocononcncnnnncnnnconanononnnonos 30 J amp T Record O iD is 31 14 8 Raw Data Associated with Sample Analysis oooconnccnonnnnccnoncnconncconocconoconn cono cconncnn 31 TB Laboratory QAP September 16 2008 Revision 1 149 dest ata RE ES 31 14 10 Blecttonie Data liam ster is 32 14 11 Sample Disposal Records ii riii EA E ia 32 WAND A n a ANE a a N E E nR 32 Section y O 33 Corrective Action Policies and Procedures csscsssseecessceseesseseeecescescesceeeceesencessceseenseenees 33 ISA SeoPedia A AN 33 15 2 Identification of DISC o das leo E 33 15 3 Staff Responsible for Investigation and Corrective Action oonconocnnccnoccnonconanoncnnnonos 33 15 4 Documentation and Review of Corrective ACtiOM ooooonoccnnononoccnononconncconacnnnconncionncnn 34 SECO lui a 35 Procedures for Permitting Departures from Documented Policies and Procedures 35 LOA II E a a Basses e he oe A 35 16 2 Requests for and Approval of Departures ooooocnnncnnnnccnoncconaconcnonnnconnccnocanc nono ccnn conos 35 16 3 Use of Analytical Methods Not Approved by KYDEP or U S EPA eee 35 16 4 Reporting of Non compliant Data ti netancets igen inetaavens 35 Secon a alten ch wide e e cet E A aon a E A EET 36 Procedures for Dealing with Complaints ii ita 36 A A NS NN 36 17 2 Complaint Receipt Pr dad tare aaa 36 17 3 Complaint I
55. 67 Revision No 0 Based Plan Date April 11 2011 from the top of bank indicating the extent of the measured cross section and can serve as surveying benchmarks If installation of such monuments is not feasible other permanent monuments will be established To facilitate profile relocation during the second surveying period the following actions shall be taken in the field 1 monuments shall be marked with a piece of flagging or paint 2 GPS points shall be recorded at monuments and any other locations that would aid in site relocation 3 photographs will be taken for both relocation and to document the current site conditions and 4 notes will be recorded on site identification characteristics e g bank condition distinguishing landmarks features and other pertinent data The methods for each of these sampling efforts are described below B2 2 5 1 Cross Sections Cross sections to be surveyed will be located within riffle features and identified by permanent monuments Points will be taken frequently at horizontal stations within each cross section such that the surveying indicates all significant breaks in slope and provides a thorough characterization of each cross section refer to USFS 1994 for surveying procedures Equipment used will include a 50 or 100 ft surveying tape laser level leveling accuracy lt 3mm 30m on a tripod and surveying rod Data may be recorded in RiverMorph software using a Rugged Reader
56. 83 Countable plate is a plate that has a number of well formed Blue colonies that can be easily counted 0 to about 150 The EPA states that a count of 20 to 60 colonies is the desired range for Fecal Coliform plates Enter these signs as follows The Font is Symbol The size is 11 Nomenclature Symbols Keystrokes Approximately equal to Hold down the Alt Key and type 0187 Greater Than Hold down the Shift Key and type gt Less Than Hold down the Shift Key and type lt Greater Than or equal to Hold down the Alt Key and type 0179 Less Than or equal to Hold down the Alt Key and type 0163 IA IV A V Note Per KDEP letter dated March 17 2006 When entering data in the DMR form if there is a greater than sign gt in the results enter the number without the sign A note must be made that the number had a greater than sign and as to why there was a greater than sign No changes are needed when other signs are used This is for the monthly and weekly average data 53 SOP Total Coliforms and E coli LFUCG Laboratory Page 54 of 219 Revision Number 1 Last Revised 09 09 m ColiBlue24 Method for the Determination of Total Coliforms and E coli HACH Method 10029 Federal Register Dec 1 1999 FR Vol 64 No 230 67449 67467 40 CFR 141 Scope Significance to Process and Application 1 1 The coliform analysis is applicable to investigations of stream pollution raw water sources and wastewater treatment systems 1 2 m Co
57. A Upon receipt of the results a review of the laboratory data shall be performed by the QA Manager or his designee to ensure that the project DQOs have been satisfied The Laboratory Data Quality Checklist see Appendix A shall be utilized to document this review The final reports for each of the monitoring activities will include an evaluation of the quality assurance and will compare the data produced under the water quality monitoring to the data quality indicators listed herein Quarterly Section 319 h Nonpoint Source Project Progress Report will be submitted to the KDOW by the Grantee Project Manager to document the progress on the project milestones SECTION D DATA VALIDATION AND USABILITY D1 Data Review Validation and Verification Data review is the internal examination to check if data has been recorded transmitted and processed correctly Data verification is the process of evaluating whether the data meets method procedural or contractual specifications Data validation is the review of the quality of the data based on the specific DQIs indicated in this QAPP The sampler will perform data review for all field data initially before submitting to the laboratory Upon submission to the laboratory the laboratory will review the COC for completeness and document any non conformances on the COC For the chemical laboratory data the laboratory analyst will initially conduct the review and the data will be peer reviewed by
58. Charlie Begley 234 4886 Mark Stager 368 7296 81 d Sunday s Sheets Total Chlorine Residual 04 26 63 EPA Method 330 1 Chlorine Analysis Method Total Residual Titrimetric Amperometric Issued 1978 Microbiology Log Number 23129 14969 Sample Name Blank Before PTE PTE Blank After Analysis Fecal Coliform Sample Volume V mL 10 100 Colonies Counted A 0000 PTE 04 26 63 Colonies 100 mL A V x 100 Averages Date Sample Collected Saturday January 00 1900 Total Chlorine Residual mg L Date Analysis Completed 04 26 63 Time Analysis Completed Time Sample Collected Time Analysis Started Set up Analyst B D L Below Detection Limit lt 0 01 mg L Date Analysis Completed Sunday January 01 1900 KPDES Permit Limits on Plant Effluent Res Ch Time Analysis Completed _ lt A A 0 010 mg L for Monthly Average Reading Analyst es 0 019 mg L for Daily Maximum Preservation Cool 4 C Maximum Holding Time 6 hours Presevation None required Analyze Immediately Note Plates should be read within 24hrs 2Hrs of set up time KPDES Permit Limits on Plant Effluent Fecal Coliform 200 100mL for Monthly GED 400 100mL for Maximum Weekly GED OAK ON Waterproof TDSTestr and ECTestr Series Instructions Before you Begin Remove electrode cap Soak electrodes for a few minutes in alcohol to remove oils Calibration Tester is factory calib
59. DR5000 Spectrophotometer 6 4 Adjustable volume pipettes 100 1000 uL with tips 6 5 Adjustable volume pipettes 1000 5000 uL with tips 6 6 Test Tube Rack 6 7 _ Vials with 9 and 19 mL of Nanopure water for dilutions 70 SOP TP LFUCG Laboratory Page 71 of 219 Revision Number 1 Last Revised 09 09 Interferences TA Do not use commercial detergents containing phosphate for cleaning any lab ware utilized in this method 7 2 Excess Turbidity Procedures 8 1 TNTplus 843 Total Phosphorous LR 0 05 1 50 mg L PO P 1 2 3 4 5 6 7 8 9 10 11 12 13 Turn on the DRB200 Reactor Heat to 100 C For DRB200 Reactors with 16 mm wells make sure the 16 to 13 mm adapter sleeves are in each well before turning on the reactor Carefully remove the protective foil lid from the DosiCap Zip Unscrew the cap from the vial Carefully pipet 2 0 mL of sample into the vial Flip the DosiCap Zip over so the reagent side faces the vial Screw the cap tightly onto the vial Shake the capped vial with 2 3 times to dissolve the reagent in the cap Verify that the reagent has dissolved by looking down through the open end of the DosiCap Zip Insert the vial in the DRB200 Reactor Close the protective cover Heat for 1 hour at 100 C After the timer expires carefully remove the hot vial from the reactor Insert it in a test tube rack and allow to cool to room temperature 15 25 C Pipet 0 2 mL 200 uL o
60. Development Washington DC 1978 Page 124 12 3 Federal Register Dec 1 1999 FR Vol 64 No 230 67449 67467 12 4 Code of Federal Regulations CFR 40 CFR 141 National primary drinking water regulations U S Environmental Protection Agency 59 SOP Hardness LFUCG Laboratory Page 60 of 219 Revision Number 2 Last Revised 09 09 Hardness Total mg L as CaCO Titrimetric EDTA HACH Method 8213 Hardness Total with a Digital Titrator Standard Methods 2340 C U S EPA Method 130 2 Scope Significance to Process and Application 1 1 Hardness is defined as a characteristic of water which represents the total concentration of calcium and magnesium expressed as their calcium carbonate equivalent Summary of Method 2 1 Executive Summary The EDTA titration method measures the calctum and magnesium ions and may be applied with appropriate modification to any kind of water The procedure affords a means of rapid analysis 2 2 Discussion Sample is titrated with 0 800 M EDTA titrant until the color changes from red to pure blue The EDTA complexes calcium and magnesium ions Color change occurs when all calcium and magnesium ions are complexed indicating the end point of titration Health amp Safety Precautions 3 1 Watch out for broken glass from cylinders and porcelain dishes 3 2 Wastewater samples have the potential to be hazardous use appropriate caution 3 3 Use of Nitric Acid use appropriate caution Sample Ha
61. Extended sample hold times volatilization from mechanical agitation and exposure to various light sources can affect results 7 7 At very low temperatures there is slow response of cell and longer time is required but precision is not compromised Procedures 8 1 Steps 1 Prior to testing pre rinse all glassware and stir bars with sample Do not rinse with Nanopure once pre rinsed 2 Using a 250 mL graduated cylinder measure 200 mL of sample 3 Pour sample into a 250 mL beaker with stirring bar raise the electrode assembly and place the beaker on unit 4 Turn on instrument The display will request user to press 1 for Total Cl Fwd press 1 display will then request user confirmation press 1 to confirm 5 The display will request confirmation of sample volume 200 mL press 1 6 The sample will begin to stir 7 Display will request the addition of 1 mL of Potassium Iodide 5 Reagent 1 pipette reagent into sample then press OK 8 Display will request the addition of 1 mL of Acetate buffer pH 4 Reagent 2 pipette reagent into sample then press OK 9 A mixing timer will countdown for 5 sec then the display will request that the electrodes be dipped into the sample lower electrode assembly into sample and press OK 10 The display will request user to confirm the Increment Setting should be 0 0010 press 1 to confirm 11 Unit will begin analysis total time r
62. Latitude Longitude By Date Preservative Per Sample Continue on Reverse for More Samples Headwater Stream Wadeable Stream Large River Lotic Other Bluegrass Mountain Pennyroyal Mississippi Valley Interior River Lowlands Other KN KickNet TK Traveling Kick MH Multihabitat S Surber HD Hester Dendy Multiplate HDD HD Deep HDS HD Shallow OT Other NA Not Available MacLIMS Client Setup Login By Date Reported By Date Invoiced By Date Sample Reference ID Qualitative or Quantitative Latitude Longitude Collected By Collection Date Field Preservative of Containers Per Sample Third Rock Consultants LLC Macroinvertebrate Sample Sorting Efficiency Form Client Name SamplelD Third Rock Project Original Sorter Resorted By Date Sorted Date Resorted of Grids Sorted of Grids Sorted of Organisms Originally Sorted Additional Organisms Recovered organisms additional organisms organisms recovered originally sorted Sorting Efficiency sorted d Additional Organisms Located Taxon Number Total Comments Reviewed By Date Updated 4 29 10 Third Rock Consultants LLC Macroinvertebrate Sample Taxonomic amp Enumeration Effi
63. Non representative particles such as leaves sticks and debris 7 3 Temperature differentials i e ambient temperature DO probe used to analyze a colder sample 74 Air entrapped in the BOD bottle bubbles 16 Procedures 8 1 Steps 8 1 1 8 1 4 SOP CBOD LFUCG Laboratory Page 17 of 219 Revision Number 5 Last Revised 09 09 Preparation of BOD stoppers 1 BOD stoppers are washed with detergent and tap water 2 Stoppers are then soaked in HCI 1 1 for at least 1 h 3 Stoppers are then soaked in Nanopure water 4 Allow to air dry 5 Wrap stoppers in blue sterile paper and indicator tape 6 Autoclave wrapped stoppers 7 Stoppers are maintained in sterile wrap until ready to use Preparation of BOD bottles 1 Obtain correct number of Env Express disposable 300 mL BOD bottles Use only once 2 Using a permanent marker label bottles in accordance with bench sheet 3 To each sample BOD bottle add 2 shots cycle the dispenser twice of HACH Nitrification Inhibitor Do not add Nitrification Inhibitor to the unseeded blank the blanks or to industrial samples Preparation of dilution water 1 Place 9 L of Nanopure water into a 10 L dilution bottle 2 Place filled dilution bottle on stir plate inside incubator 20 1 C 3 Adda 3 L pillow and a 6 L pillow of BOD nutrient buffer into the dilution water bottle 1 mL nutrient to 1 L of lab water 4 Mix thoroughly using a magnetic stirrer P
64. O value allowable in a Plant Effluent sample at any given time In the event of a indicated value less than 7 0 mg L assure correct calibration resample and retest If the value indicated by retest is less than 7 0 mg L Immediately notify the Plant Superintendent and Laboratory Supervisor 10 2 Process Ranges Raw influent dissolved oxygen values are typically less than 1 mg L Target values for mixed liquor dissolved oxygen concentration in the aeration basins is 2 0 mg L Data Analysis and Calculations 11 1 None required values are taken directly when measurement stability is indicated 42 12 SOP LAB D O LFUCG Laboratory Page 43 of 219 Revision Number 5 Last Revised 09 09 Bibliography 12 1 12 2 12 3 Report on the Validation of Proposed EPA Method 360 3 Luminescence for the Measurement of Dissolved Oxygen in Water and Wastewater August 2004 HACH Company Loveland CO Memorandum EPA Recommendation for the use of HACH method 10360 Revision 1 1 January 2006 ATP Case N04 0013 HACH HQ Series Portable Meter Users Manual September 2006 Edition 5 HACH Company Loveland CO 43 SOP Fecal Coliform LFUCG Laboratory Page 44 of 219 Revision Number 3 Last Revised 09 09 Fecal Coliform Membrane Filter Procedure U S EPA 600 8 78 017 Microbiological Methods for Monitoring the Environment Water and Wastes Scope Significance to Process and Application 1 1 The fecal coliform an
65. O D 5 Day Biochemical Oxygen Demand C B O D Carbonaceous Biochemical Oxygen Demand Analyst Reading amp Calculating Analysis KPDES Permit Limits on Plant Effluent 10 mg L for Monthly Average QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS 15 mg L for Maximum Weekly Average Presevation Cool 4 C Maximum Holding Time 48 hours S d TOWN BRANCH WASTEWATER TREATMENT PLANT Town Branch Laboratory Grab Samples Total Chlorine Residual Enter Date ES ER VET VE A EE HET VS VE EEC ES EE E VE E VE CI E E CT Analysis Method EPA Method 330 1 Chlorine Total Residual Titrimetric Amperometric Issued 1978 EPA Method 330 5 Chlorine Total Residual Spectrophotometric DPD Issued 1978 Log Number pp pp T pp pp pp T AH Total Chlorine Residual mg L Analyst Date Analysis Completed Time Analysis Completed PTE Chlorine Residual Time sampled Within 15 min limit Time received QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS Time started Presevation None required Analyze Immediately KPDES Permit Limits on Plant Effluent 0 01 mg L for Monthly Average 9 d TOWN BRANCH WASTEWATER TREATMENT PLANT Town Branch Laboratory Grab Samples Dissolved Oxygen Method EPA Method 360 3 Oxygen Dissolved Luminescent Probe Issued 2006 Dissolved Oxygen Meter Calibration Barometer Reading Dissolved Oxygen from HQ40D Temp
66. Oitas Accuracy ES AIFS RES EISES Operating Temperature 6 50 C 3210 12 F Temperature Automate ATC 32 to 22 F 0 40 JOC Compensation 2 per C 1 11 per F Battery Life apos LAV Eveready EPOTSBPI200 hours Dimensions SAL LW x 0 94 H Wetted 316 Stainless Steel and glass reinfore Materials thermoplastic polyester i Opiate POE e oe Weight _ 3 25 ounces 92 gm unit only 45 ounces 128 gm boxed Use the guide below for selecting 6 calibration solution appropriate _ for your TOSTestr asd TDS Testri Use a standard belween 200ppm and 1998ppm TOSTestr2 Use a standard between 3ppt and 10 00 ppt TOSTestr 3 Use a standard between 30048 and 1990u5 TOSTestr 4 Use a standard between ams and 19 9amS IODA ERE A A Sar peenar pee mere mee Id nae Pocket sized testers for the measurement of Total Dissolved Solids or Conductivity with DIRECT READOUT i p to 1990 ppm Lange LCD with direct recodo no multiplicofion needed Automatic Temperature Compensation ATC Cale Ae ij a Parmer 22 FS accuracy COLE PARMER INSTRUMENT COMPANY Solashproot membrane keypad 626 East Bunker Gourt 5 i gan Vomon Hiis IL 60061 Four models available leatwing 00 323 4340 the mos usetul ranges tor the wides voriety of applications Parameters Methodology and Environmental Impact The analysis of water samples from surface water lakes
67. Pocket PC or in a field notebook Surveying precision shall be 0 01 ft for vertical readings and 0 1 ft for horizontal readings Notes related to observed changes at various elevations within the cross section will be made Each stream permanent cross section will be surveyed twice once at the initial site visit following monument installation and approximately nine months subsequent to first measurement Differences between these two measurements will allow estimation of channel change and if degradation is occurring the erosion rate can be calculated B2 2 5 2 Profiles Representative stream longitudinal profiles will be taken over a distance that includes approximately three riffle features at each of the nine hydrogeomorphic monitoring stations Permanent monuments on a designated bank and at least 10 feet back from the top of bank will mark the upstream and downstream extents of the profiles and can serve as benchmarks for surveying Profile measurements will be taken within the stream thalweg and will be of adequate frequency to identify all grade changes and facet slopes within the profile refer to USFS 1994 for surveying procedures Equipment used will include a 100 ft surveying tape laser level leveling accuracy lt 3mm 30m on a tripod and surveying rod Data will be recorded in RiverMorph software using a Rugged Reader Pocket PC or in a field notebook Surveying precision shall be 0 01 ft for vertical readings and
68. Powder 6286 Immediately use the 1 0 g Add 8 drops of i Cap and gently invert the bottle At this point 6 to te de otic until the NOTE the sample has recipitate and the reagent been fixed and contact ne totally dissolved The between the sample and the solution will be clear yellow y atmosphere will not affect the to orange if the sample test result Samples may be contains dissolved oxygen e at this point and titrated ater TEST PROCEDURE PART 3 THE TITRATION Fill the titration tube 0608 to the 20 mL line with the fixed sample Cap the tube Insert the Titrator into the plug in the top of the Sodium Thiosulfate 0 025N 4169 titrating solution 74 Y Invert the bottle and slowly withdraw the cia until the arge ring on the plunger is opposite the zero 0 line on the scale Turn the bottle upright and remove the Titrator wae plunger of the Titrator 0377 NOTE If small air bubbles appear in the Titrator barrel expel them by partially filling the barrel and pumping the titration solution back into the reagent container Repeat until bubble disappears NOTE If the sample is a very pale yellow go to Step 9 continued TEST PROCEDURE Y m depress the i plunger to dispense the Insert the tip of the j titrating solution until Titrator into the the yellow brown opening of the color chang
69. QA QC is the responsibility of everyone in the chain of custody of a sample its analysis and the data that results A first level of QA QC is compliance with procedures and methods in the Standard Sampling Curriculum The second level of QA QC is an understanding of and compliance with these Standard Operating Procedures among everyone involved in the sampling event 11 The third level of QA QC is discrete procedures for analyzing quality using the data generated in the sampling program These procedures are the responsibility of the Laboratory s internal QA program and the Steering Committee s Data Manager and Quality Assurance Officer A fourth and final level of QA QC are activities at the statewide level by the Quality Assurance Committee that include e Review of QA QC reports submitted with data by Steering Committees e Audits of Steering Committee QA QC activities and e Comparison of data with statewide and nationwide databases The remainder of this section outlines QA QC procedures that apply to Tier IIT and IV data uses b Duplicate Samples and Field Blanks The Sampling Event Coordinator selects sites for duplicate samples and field blanks in consultation with the Steering Committee s Science Advisor and Quality Assurance Officer Sites selected for duplicate and blank samples should be chosen to be representative of the range of conditions encountered and to rotate through different sampling teams Sites expect
70. Results from this project will be compared with Bluegrass Bioregion Criteria reference reach scores and results from MS4 permit sampling at the mouth of Wolf Run These results and the results of the watershed habitat assessment monitoring will be combined into a final report entitled Assessment of Habitat and Macroinvertebrates in the Wolf Run Watershed due to the KDOW and LFUCG by December 31 2011 B2 2 4 Watershed Habitat Assessments Habitat assessments will include a visual assessment of ten habitat parameters that characterize the stream micro scale habitat the macro scale features and the riparian and bank structure features that are most often influential in affecting the other parameters The method follows the US EPA s Rapid Bioassessment Protocols for Use in Wadeable Streams and Rivers Barbour et al 1999 Each of the parameters will be evaluated on a Condition Category scale from 0 to 20 The categories within this scale include Optimal for scores from 20 to 16 Suboptimal for scores from 15 to 11 Marginal for scores from 10 to 6 and Poor for scores from 5 to 0 The score for each parameter will be summed to produce a final habitat score maximum 200 For parameters 1 to 5 the habitat assessment will evaluate a composite of the entire biological sampling reach For parameters 6 to 10 an area beginning approximately 100 m upstream of the sampling reach through the sampling reach will be e
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72. Samples containing these substances must be pretreated as described in the following procedures before preservation with sodium hydroxide If the sample contains sulfide and is not pretreated it must be analyzed within 24 hours Reagents 5 1 CyaniVer 3 CyaniVer 4 and CyaniVer 5 reagent powder pillows Equipment amp Lab Ware 6 1 Plastic beakers at least 50 mL 6 2 Funnel plastic or glass 6 3 Glass Microfibre Filter paper 125mm diameter 27 SOP Free Cyanide LFUCG Laboratory Page 28 of 219 Revision Number 3 Last Revised 09 09 6 4 Two 1 inch sample cells 10 mL with cap zeroing vial sample vial 6 5 Fixed 5 mL pipette with 5 mL pipette tip 6 6 Spec Color Standards kit 6 7 DR 4000 1 inch Cell Adapter 6 8 HACH DR 4000 Spectrophotometer Interferences 7 1 Chlorine 7 2 Metals 7 3 Oxidizing agents 74 Reducing agents 15 Turbidity Procedures 8 1 Steps 8 1 1 Filtration 1 Pour approximately 40 mL from the Cyanide sample container to the plastic beaker as soon as the sample arrives Preserve the remaining sample with 1 25 mL of 12 5 N NaOH for total cyanide analysis 2 Fold the glass microfibre filter paper to fit in the funnel 3 Slowly pour sample into filter so it does not overflow 4 Collect filtered sample 8 1 2 Reaction 1 Fill sample cell with 10 mL of filtered sample 2 Add CyaniVer 3 powder pillow to the 10 mL in sample cell cap and shake 30 seconds Wait an additional 30 seconds leaving the samp
73. Society Other grades may be used provided it is first ascertained that the reagent is sufficiently high in purity to permit its use without lessening the accuracy of the determinations Purity of water Unless otherwise indicated references to water shall be understood to mean Type 1 reagent grade water Milli Q Water System conforming to the requirements in ASTM Specification D1193 Ammonium molybdate antimony potassium tartrate solution This solution has a long shelf life and is stable for approximately six months It is stored in a one liter plastic bottle Dissolve 8 g of ammonium molybdate and 0 2 g antimony potassium tartrate in 800 mL water and dilute to liter Ascorbic acid solution This solution has a shelf life of two weeks and should be stored in a one liter amber bottle in the refrigerator Be sure to indicate on the label when the solution was made Dissolve 15 g of ascorbic acid in 125 mL water and dilute to 250 mL Add 0 5 mL of spec grade acetone Sulfuric acid 12 N This solution is stable for up to six months It is stored in a one liter plastic bottle Slowly add 333 3 ml concentrated H2SO0 to approximately 600 mLwater Allow solution to cool and dilute to 1000 mL Phosphate as P Stock 1000ppm Purchases stock from ERA Phosphate as P Standard Solution 10mg L Smls of 1000mg L stock in 500ml flask dilute with Milli Q water Quality control sample Dilute ortho p QC stock solution so that the QC value f
74. West Hickman WWTP Laboratory Page 17 of 219 Revision Number 4 Last Revised 09 09 WH Fecal Coliform Membrane Filter Procedure U S EPA 600 8 78 017 Microbiological Methods for Monitoring the Environment Water and Wastes Scope Significance to Process and Application 1 1 The fecal coliform analysis is applicable to investigations of stream pollution raw water sources and wastewater treatment systems 1 2 The fecal coliform analysis differentiates between coliforms of fecal origin Summary of Method 2 1 Executive Summary The sample is filtered through a Millipore membrane filter The filter is placed on a filter pad containing media in a sterile Petri dish The samples are then incubated at 44 5 C 0 2 C for 24 hours 2 hours Colonies are counted and fecal coliform calculations are performed 2 2 Discussion Fecal coliforms are defined as gram negative non spore forming rods The major species is Escherichia coli which indicates fecal pollution and the presence of enteric pathogens Colonies produced by fecal coliform bacteria are various shades of blue Non fecal coliform colonies are gray to cream colored Health amp Safety Precautions 3 1 3 2 3 3 3 4 All municipal and industrial wastewaters are potentially hazardous Gloves and safety glasses should be worn when dispensing these samples Possible exposure to enteric pathogens Care must be taken to avoid undue exposure A flame is used to sterilize for
75. When using the GP50 Gradient Pump all due care must be taken before one switches from local procedures to remote procedures The bottle from which the eluent is being pumped i e A B C or D must exactly match the bottle specified in the method If there is a difference then once the pump control is turned over to remote control irreversible damage and destruction of suppressors columns piston seals and check valves on the GP50 Gradient Pump will occur NEVER switch from bottle C to A B or D without flushing the system lines with water to remove all traces of eluent from bottle C from the lines B Sample Preparation 1 Ifthe sample was not filtered in the field it must be done so now Transfer 50 mL of a well mixed sample to the filtering apparatus Apply the suction and collect the filtrate pi 8 If the conductivity values for the sample are high dilution will be necessary to properly run the sample within the calibration standard range Dilutions are made in the Polyvials with the plastic Filter Caps If the dilutions are gt 20X then volumetric glassware is required All dilutions are performed with reagent grade DI water Be sure to mix the dilution well For Fluorides and Bromides pipette 5 0 mL of the filtered samples into the Polyvials For all other anions including TKN and Total Nitrogen first pipette 0 05 mL of 100X sample spiking eluent into the Polyvials then pipette 4 95 mL of the filtered samples on top of
76. a 250 mL graduated cylinder measure 200 mL of sample 3 Pour sample into a 250 mL beaker with stirring bar raise the electrode assembly and place the beaker on unit 4 Turn on instrument The display will request user to press 1 for Total Cl Fwd press 1 display will then request user confirmation press 1 to confirm 5 The display will request confirmation of sample volume 200 mL press 1 6 The sample will begin to stir 7 Display will request the addition of 1 mL of Potassium Iodide 5 Reagent 1 pipette reagent into sample then press OK 8 Display will request the addition of 1 mL of Acetate buffer pH 4 Reagent 2 pipette reagent into sample then press OK 9 A mixing timer will countdown for 5 sec then the display will request that the electrodes be dipped into the sample lower electrode assembly into sample and press OK 10 The display will request user to confirm the Increment Setting should be 0 0010 press 1 to confirm 11 Unit will begin analysis total time required for analysis will vary with sample strength and chosen increment value During analysis the display graphs the progress of the titration Upon completion the unit will display the resulting concentration value and calculated confidence limits press OK to accept results 12 Record the results on the Total Chlorine Residual bench sheet In the case of the PTE sample also log in the pro
77. ae estas es oko Dieses iaa 54 B34 Sample Designation nunne nre o sate igi E E E ata tates 55 B4 Analytical Methods Requirements oooooooooccnoccccconococononononononononononononono nono noncnn nono 55 B5 Quality Control Requirements oooooonooconoooccnonocccononcnonononononononononononcnnnnncnnnnnccn nono 56 BO l Field Quality Comos aco a ds es le los it as Bale 56 B5 2 Macroinvertebrate Taxonomic Quality Controls ooooooccnnnccioconoccnononcnanconncconacnnos 56 B5 3 Chemical Laboratory Quality ControlS oooonncnnnccnnncnnnccnoncconnoconoconn nono ccnnnccnocnnos 57 B6 Instrument Equipment Testing Inspection Calibration and Maintenance ReguirementS ooo ls pd 57 B7 Data Manantial 58 SECTION C ASSESSMENT AND OVERSIGHT cccccccccccceeeeeeeeteceeeeeees 59 SECTION D DATA VALIDATION AND USABILITY 0cccccccceseeteeneees 61 D1 Data Review Validation and Verification ooonooocccnnonocccononancnononanocononnonos 61 D2 Validation and Verification MethodS ooo ooonnicninncnnnciconcconccononconncconoconn cono cconnonns 62 D3 Reconciliation with User Requirements and Data Quality Objectives 63 SECTION E REFERENCES AND CITATIONS oooocccccnnonconnconccononononncnnnconccnnconncnos 63 List of Exhibits Exhibit 1 Project Sampling Sites espiar 14 Exhibit 2 Karst System Hydraulic Monitoring s sessesseeessseseesesseseesesseseesssseesresesseseese 15 Exhibit 3 W
78. analyses are performed samples are selected on a rotating basis from among various water samples wastewater samples monitoring locations and other applicable locations All procedures used to select samples for matrix spike duplicate or sample duplicate analyses are documented Each analytical SOP references quality control criteria to use in determining discrepancies and accepting data when duplicate samples do not meet acceptance criteria Section 15 Corrective Action Policies and Procedures references procedures for taking corrective actions when duplicate samples do not meet acceptance criteria Quality Control Charts and Tabulations 6 7 1 6 7 2 6 7 3 The laboratory maintains tabulations quality control charts or a combination of tabulations and quality control charts for the results from all quality control procedures All calculations for the tabulations and or control charts are performed according to Standard Methods 21 Edition Part 1020 B Separate tabulations and or control charts are maintained for each test method for each matrix and for each analytical range Each tabulation and or control chart includes the following information e Title Identification of standard operating procedure Name of quality control procedure being tabulated Analytical method Analyte Analyte units of measure Matrix Fortification concentration TB Laboratory QAP September 16 2009 Revision 1 e Mean Standard Dev
79. another analyst or capable reviewer Data will be reviewed according to the laboratory QA Manual and the method specific SOP for data entry calculations and transformations as well review of quality control criteria If deviations are noted corrective actions will be taken with verification of both the reviewer and the original data collector If consensus cannot be reached the data will be rejected During verification and validation of the data all data that does not meet the DQIs listed in this QAPP will be qualified or rejected A list of the type of qualifiers that may be applied to this data is listed in Table 14 All qualified data will be evaluated according to the actions listed Wolf Run Watershed Page 61 of 67 Revision No 0 Based Plan Date April 11 2011 TABLE 14 DATA QUALIFIERS AND RESPONSE Definition Action To Be Taken Analyte detected in associated Method Blank Reject results Indicates all or a portion of the amount found in a sample may be due to laboratory sources Diluted out Accept results Indicates a dilution to overcome matrix effects caused other analytes of interest to be diluted out of range Normal quantitation is not available Holding time exceeded Reject results Method required holding time is exceeded Estimated value Accept results when used to indicate result is below the project reporting limit but above the Method Detection Limit MDL Matrix Spike and or Matrix
80. colored manganic hydroxide For every molecule of oxygen in the water four molecules of manganous hydroxide are converted to manganic hydroxide Chemically this reaction can be written as 4Mn OH O 2H 0 gt 4Mn OH Manganous Oxygen Water Manganic Hydroxide Hydroxide After the brown precipitate is formed a strong acid such as Sulfamic Acid Powder 6286 or Sulfuric Acid 1 1 6141 is added to the sample The acid converts the manganic hydroxide to manganic sulfate At this point the sample is considered fixed and concern for additional oxygen being introduced into the sample is reduced Chemically this reaction can be written as 2Mn OH T 3H2SO 4 gt Mn2 SO4 3 6H0 Manganic Sulfuric gt Manganic Water Hydroxide Acid Sulfate Simultaneously iodine from the potassium iodide in the Alkaline Potassium Iodide Azide Solution is oxidized by manganic sulfate releasing free iodine into the water Since the manganic sulfate for this reaction comes from the reaction between the manganous hydroxide and oxygen the amount of iodine released is directly proportional to the amount of oxygen present in the original sample The release of free iodine is indicated by the sample turning a yellow brown color Chemically this reaction can be written as Mn2 SO4 3 2KI gt 2MnSO K2SO L Manganic Potassium gt Manganous Potassium Iodine Sulfate Iodide Sulfate Sulfate The
81. completion by December 31 2012 A7 Data Quality Objectives DQOs and Criteria for Measurement Data A7 1 Data Quality Objectives Data quality objectives DQOs are qualitative and quantitative statements that clarify the intended use of the data define the type of data needed to support the decision identify the conditions under which the data should be collected and specify tolerable limits on the probability of making a decision error due to uncertainty in the data The data quality objectives for the respective sampling activities are listed in Table 5 along with the Standard Operating Procedures associated with each of these activities The overall objective of this project is to collect data of sufficient quality and quantity to support the development of a watershed based plan for the Wolf Run watershed Wolf Run Watershed Page 22 of 67 Revision No 0 Based Plan Date April 11 2011 TABLE 5 SUMMARY OF DATA QUALITY OBJECTIVES AND STANDARD OPERATING PROCEDURES Sampling Activity Karst Hydrograph Characterization Objective Characterize the flow distribution between the surface water and ground water systems Standard Operating Procedures References KDOW 2010b Measuring Stream Discharge Standard Operating Procedure Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky DOWSOP03019 In Situ Inc 2006 Level TROLL Operator s Manual www in situ com Conductivity Survey I
82. designated area on the COC B3 2 Sample Handling and Transport The sampler will be responsible for sample handling in the field and transport of samples to the laboratory The sampler will collect the sample at the source following established protocols The sampler will be responsible for collecting the sample in appropriately identified collection containers with the correct preservative as applicable and ensuring that the container lid is secured tightly to prevent leakage or outside contamination Sample containers for chemical analysis shall be immediately placed in a cooler on ice to maintain a temperature of 4 2 C for transport to the laboratory Sample bottles shall be placed in the cooler with lid side up in an organized manner per COC entry Sample coolers will be of adequate size to allow ice to surround all sample bottles It is the responsibility of the sampler to ensure that coolers are properly packed in the field and that they have sufficient cooler space on their vehicle for their daily sample load Coolers shall be secured during transport such that significant disturbance of the samples is avoided Macroinvertebrate samples will be analyzed at Third Rock The LFUCG Town Branch laboratory and Kentucky Geological Survey laboratory will process the chemical sampling parameters Upon receipt at the laboratory the sample custodian shall review the COC for completeness and accuracy Anomalies shall be documented The laboratory shal
83. dilute to 1 liter Prepare daily Phosphorus standard solution 2 5 mg L Dilute 50 mL of the stock solution to exactly 1 liter of water Prepare daily Blank teagent grade water Total phosphorus stock QC solution Using a commercially available Quality Control solution dilute to desired range and record manufactures name lot and date Quality control sample Dilute total P stock solution so that QC value falls midway in analysis working range 0 05 1 00 ppm Using 6 11 ppm QC stock solution dilute 25 mL of Total Phosphorous stock solution to 500 mL resulting in a concentration of 0 306 ppm Acid for glassware Carefully add 250 mL of concentrated hydrochloric acid to approximately 600 5 Procedure ml of water Dilute to 1 liter A Prepare the spectrophotometer by turning on the lamp and allowing it to warm up for at least one hour See the Spectrophotometer GLP for a detailed listing of necessary computer commands B Standards Prep 1 Prepare a series of phosphorus standards from the 2 5 mg L phosphorus standard solution according to the following table Dilute each to 50 mL with water Volume of phosphorus standard mL Standard concentration ppm 1 0 05 2 0 10 4 0 20 7 0 35 10 0 50 15 0 75 20 1 00 2 Prepare all standards daily C Sample Prep 1 2 3 SI Pour 50 mL of each of the two blanks standards samples duplicates and Total P QC s into 100 mL glass beakers Add 3 6 gl
84. evaluated for data quality The purpose of the data compilation and assessment was to thoroughly describe the Wolf Run watershed and to determine what additional data would be necessary in order to identify the impairments in the watershed and their causes and sources to calculate the extent of the impairments and to determine solutions for improving water quality Based on this analysis six major sampling needs were identified which include e measurements to characterize of the discharge hydrograph for the Preston Springs karst basin watershed conductivity survey macroinvertebrate collections on tributaries and headwaters watershed wide habitat assessments hydrogeomorphic assessment of the watershed a water quality monitoring data set meeting the specifications of KDOW s Watershed Planning Guidebook for Kentucky Communities KWA and KDOW 2010 This QAPP will establish the quality criteria and collection process necessary to produce data which will fill the identified gaps and allow for the determination of the locations in the watershed in which BMPs will be most feasible efficient and effective Wolf Run Watershed Page 12 of 67 Revision No 0 Based Plan Date April 11 2011 A6 Project Task Description A6 1 General Overview of Project This project will involve six different monitoring activities as follows e karst hydrograph characterization e conductivity survey benthic macroinvertebrate collection watershed
85. final stage in the Winkler titration is the addition of sodium thiosulfate The sodium thiosulfate reacts with the free iodine to produce sodium iodide When all of the iodine has been converted the sample changes from yellow brown to colorless Often a starch indicator is added to enhance the final endpoint Chemically this reaction can be written as 2Na28 05 L Na28406 2Nal Sodium Iodine Sodium Sodium Thiosulfate Tetrathionate Iodide 13 GENERAL SAFETY PRECAUTIONS Read all instructions and note precautions before performing the test Store the test kit procedure in a cool dry area Keep all equipment Read the labels on A at all reagent bottles chemicals out Note warnings and of the reach of first aid information young Read all Material children Safety Data Sheets Avoid contact between 6 Wear safety glasses when o reagent chemicals and skin performing test procedures eyes nose and mouth CAUTION AVOID SKIN CONTACT In the event of an accident or suspected poisoning immediately call the Poison Center phone number in the front of your local telephone directory or call a physician Additional information for all LaMotte reagents is available in the United States Canada Puerto Rico and the US Virgin Islands from Chem Tel by calling 1 800 255 3924 For other areas call 813 248 0585 collect to contact Chem Tel s International access number Each reagent can be identified by th
86. first sampling container for the site with a request that the monitor identify the site on the map and return it to the Data Manager c Photographs The Volunteer Monitor is requested to submit two photographs of the stream reach with the Physical Characterization form e Upstream of the sample point looking downstream at the sample point marked downstream and e Downstream of the sample point looking upstream at the sample point marked upstream 6 Preparation for Sampling a Containers and Preservatives Containers and preservatives for samples are obtained by Steering Committees through the ICC purchasing cooperative or independently and meet the criteria found in Appendix E Environmental Sample Preservation and Holding Times The container is pre marked with the unique Site Number by the Sampling Event Coordinator designated by the Steering Committee before it is mailed to the Supervising Sampler for the site A Chain of Custody form see Appendix F for the template is prepared for each site and preprinted with the Site Number usually by the Data Manager It is enclosed by the Sampling Event Coordinator with a set of instructions Samplers should open and read their packet upon receipt 7 Sampling Procedures The purposes of the following streamside sampling procedures are to assure that the sample container correlates with the documented sampling activity and to prevent water samples from contami
87. if worn with stream water before sampling with the container Do not pre rinse the container and avoid contaminating the inside of the container especially with an ungloved finger Dip the pre marked sample container to a depth of about four inches with the open end facing upstream Push the mouth of the container upstream at this depth until the container is nearly full The mouth of the container should at all times be upstream of the sample collector and any disturbed sediments Leave enough airspace in the top of the sample container so the sample can be remixed just before filtration at the laboratory Immediately chill the sample in an ice slurry see following section e Sample preservation Sample preservation procedures prevent reduction or loss of water quality variables of interest Variable loss can occur between sample collection and laboratory analysis because of physical chemical and biological processes that result in chemical precipitation absorption oxidation reduction ion exchange degassing or degradation Preservation stabilizes variable concentrations for a limited period of time Some samples particularly of bacteria have a very short holding time before laboratory analysis may begin In all Watershed Watch sampling events sample containers are placed in a container with a slurry of chilled water and ice immediately following sample collection to maintain them at 4 degrees Centigrade plus or minus 2 degrees without
88. intensity proportional to the total phosphorus concentration which is then quantifiable by the spectrophotometer Health amp Safety Precautions 3 1 During sample digestion the digester block is HOT 150 C Burn Hazard Use digester block safety shields In addition the capped glass sample vials contain hot 150 C acidic solution under pressure 3 2 PhosVer3 powder pillow can be a respiratory hazard Wear a mask or place samples in hood when dispensing 33 Wastewater samples should be considered potentially hazardous Use proper personal protective equipment 24 SOP WH TP West Hickman WWTP Laboratory Page 25 of 219 Revision Number 5 Last Revised 09 09 Sample Handling and Preservation 4 1 Analyze samples immediately after collection for best results If prompt analysis is impossible preserve samples for up to 28 days by adjusting the pH to 2 or less with H2SO and storing at 4 C Prior to analysis allow samples to warm to room temperature and neutralize Document sample preservation Reagents 5 1 PhosVer 3 Phosphorus Reagent Powder 5 2 Potassium Persulfate Reagent Powder 5 3 Sodium Hydroxide Solution 1 56 N 5 4 Total and Acid Hydrolyzable Test Vials Test N Tubes 5 5 Nanopure Grade Water 5 6 Phosphate Standard Solution 1 mg L as PO Equipment amp Lab Ware 6 1 HACH DBR200 COD Reactor with Test N Tube block calibrated to 150 C with safety shields 6 2 HACH DR 4000 Spectrophotometer wi
89. is greater than zero and is determined from analysis of a sample in a given matrix containing the analyte MDL lia 99 S where t the t statistic for n number of replicates used for n 7 t 3 143 n number of replicates S standard deviation of replicates 8 Reference EPA SW 846 9056 Chapter 5 September 1994 U S EPA Method 300 0 March 1984 ASTM vol 11 01 1996 D 4327 Standard Test Method for Anions in Water by Chemically Suppressed lon Chromatography 04 2011 KGS 4500 N C Total Kjeldahl Nitrogen Preparation 1 Discussion Principle Total Kjeldahl Nitrogen is the sum of organic nitrogen and ammonia nitrogen compounds of a sample This method oxidizes all of the organic and inorganic nitrogenous compounds at 100 to 110 C to nitrate The digestion also helps dissolve solid material that could interfere with obtaining an accurate reading The total nitrogen is then determined by the analysis of nitrate in the digestate with an IC Total Kjeldahl Nitrogen is then determined by subtracting the pre determined nitrite plus nitrate nitrogen values from the total nitrogen values Sensitivity This method covers the range from 0 1 ppm to 2 9 ppm Interferences Since this method is designed to oxidize ammonia to nitrate for analysis the use of ammonia and or ammonia based substances should be avoided in the work area and on the glassware as this could produce increased positive results that are inaccurate S
90. is uniquely identified and provided with a uniquely identified thermometer graduated in increments no larger than 10 C for muffle furnaces and 1 C increments for oven and warm air incubators Temperatures are recorded daily The monitoring logs include oven and thermometer identification date time temperature initials of the responsible person and the acceptable temperature range 17 TB Laboratory QAP Revision 1 8 9 September 16 2009 8 8 2 The following table lists the ovens that are used in the Town Branch Laboratory Description Unique Identifier Comments Drying Oven Drying Oven 1 103 105 C Iso temperature Oven Iso Temp Oven Adjustable Muffle Furnace Muffle Furnace Adjustable Other Laboratory Equipment 8 9 1 The laboratory monitors and controls method specific temperature requirements for heating blocks and water baths etc The laboratory also maintains documentation of the results 8 9 2 Autopipetors and dilutors of sufficient accuracy are used for some applications The autopipetors repipettors are serviced and calibrated annually by a qualified service representative The service representative issues the laboratory a certificate of calibration for each unit and labels each unit to indicate service calibration Logs of these checks are maintained for each device 18 TB Laboratory QAP September 16 2009 Revision 1 Section 9 Test Methods and SOPs 9 1 Scope Th
91. laboratory that allows for accuracy precision and reliability of laboratory analyses and that data produced in the laboratory meets or exceeds user requirements Good Laboratory Practices are employed to maximize data reliability Specific Objectives The laboratory will employ methods capable of meeting user s needs for accuracy precision sensitivity and specificity Whenever possible analytical methods used will be those approved by regulatory or accrediting authorities Under the supervision of the Laboratory Management laboratory staff members will receive training in quality technology of sufficient depth to perform their assigned duties The laboratory will establish a level of quality for routine performance to use as a baseline from which to measure quality improvement efforts Laboratory staff will monitor routine operational performance through analysis of appropriate quality control solutions and through participation in inter laboratory testing programs The laboratory will provide for corrective actions as necessary The laboratory will operate in conformance with requirements established by the State of Kentucky and or the USEPA QAP Availability Copies of the laboratory s QAP are available from Dr David J Price Ph D Laboratory Supervisor Mrs La Vada M Green QA QC Manager TB Laboratory QAP September 16 2009 Revision 1 Section 2 Laboratory Organization and Staff Responsibilities 2 1 Laboratory Organiza
92. may need to be remade and rerun 2 Once the spectrophotometer is standardized properly the samples may be analyzed 3 Once the analysis is completed print out a copy of the standard values plotted curve and the sample values Copy the relevant data onto the Total Phosphorous Data Sheet E Clean Up 1 Turn off the spectrophotometer lamp 2 The waste must be placed in the acid waste container 3 For glassware clean up refer to the Total P section of the Glassware GLP 6 Quality Control A quality control sample should be run at the beginning and end of each sample delivery group SDG or at the frequency of one per every ten samples The QC s value should fall between 10 of its theoretical concentration A duplicate analysis should be run for each SDG or at the frequency of one per every twenty samples whichever is greater The RPD Relative Percent Difference should be less than 10 If this difference is exceeded the duplicate must be reanalyzed From each pair of duplicate analytes X and X3 calculate their RPD value X 2 X 2 where X X2 means the absolute difference between X and X3 7 Method Performance The method detection limit MDL should be established by determining seven replicates that are 2 to 5 times the instrument detection limit The MDL is defined as the minimum concentration that can be measured and reported with 99 confidence that the analyte concentration is greater than
93. mean divided by n 1 Standard Deviation Interval Measure of difference between our lab mean and the average of all lab means in a comparison group The difference is expressed in terms of the SD of all the means in the group Tare A clean dry container used in a gravimetric analysis T test Used to ascertain whether the means of two sample groups differ significantly Calculated using the mean and SD of two matched groups Refer to Tietz TI Therapeutic Index is the ratio of the dose required to produce a toxic effect Total Oxygen Demand TOD a quantitative measure of all oxidizable material in a sample of water or wastewater as determined instrumentally by measuring the depletion of oxygen after high temperature combustion as TOC COD Total Carbon TC a quantitative measure mg L of both total inorganic TIC and total organic carbon TOC in water or wastewater Determined instrumentally by chemical oxidation to CO and subsequent infrared detection in a carbon analyzer Total Organic Carbon The amount of carbon bound in organic compounds in a sample Because all organic compounds have carbon as the common element total organic carbon measurements provide a fundamental means of accessing the degree of organic pollution The carbonaceous analyzer measures all of the carbon in a sample after injection into the combustion tube Because of various properties of carbon containing compounds in liquid samples preliminary t
94. necessary Time sample taken Name of Supervising Sampler on site when sample collected Lab Notes If name not correct please Sampler ID t in Comment Box Telephone Flow Rate 48 Hr Rainfall Turbidity Water Chemistry 0 Dry 0 0 Clear Oxvgenppm pHSU 1 Ponded 0 1 1 2 Low 0 5 2 3 Normal 1 0 3 Turbid Conductivity 4 Bank Full 1 5 5 Flood 2 0 General comments questions corrections concerns or suggestions When transporting samples to the lab it is necessary to have each person that controls the sample to sign when they receive it AND when they relinquish it Relinquished by Time Date Received by Time Date This form must accompany your sample to the lab The first signature in the relinquished by column must match the supervising Sampler s name Make a copy for yourself then send the original on its way with your sample runner Please correct errors on the pre printed part of this record If you have questions or difficulties please contact us at 1 800 928 0045 Ext 473 04 2011 KGS D515 Total Phosphorus in Water 1 Discussion MDL 0 02 as of 5 2002 Principle Separation into total dissolved and total recoverable forms of phosphorus depends on filtration of the water sample through a 0 45 um membrane filter Total recoverable phosphorus includes all phosp
95. net flush on the substrate and disturbing approximately 0 1m of area to dislodge attached organisms Material will be emptied into a wash bucket rinsed inspected for organisms and discarded Three replicates will be conducted This sub habitat must be sampled for wadeable sites and may be sampled for headwater if present Wolf Run Watershed Page 42 of 67 Revision No 0 Based Plan Date April 11 2011 Justicia americana water willow Beds These will be sampled by working the net through a Im section in a jabbing motion The material will then be emptied into a wash bucket and any J americana stems will be thoroughly washed inspected and discarded Three replicates will be conducted This sub habitat must be sampled for wadeable sites and may be sampled for headwater if present Leaf Packs Leaf packs will preferably be collected from conditioned i e not new fall material material when possible Samples will be taken from a diversity of habitats i e riffles runs and pools and placed into the wash bucket The material will be thoroughly rinsed to dislodge organisms inspected and discarded Three replicates will be conducted for both headwater and wadeable sites Silt Sand and Fine Gravel A U S No 10 sieve will be used to sort larger invertebrates e g mussels burrowing mayflies dragonfly larvae from silt sand and fine gravel by scooping the substrate to an approximate depth of 5cm A variety of collection sit
96. new addition includes additional bench space and cabinets A schematic layout of the laboratory showing current space utilization is shown in Appendix 5 Access and Security Measures 10 2 1 Entrances to the Town Brach WWTP are located at the north east and south ends of the plant Automatic gates are open during normal operating hours Magnetic access cards are required for entry during off hours 10 2 2 Any visitors to the Town Branch WWTP and Laboratory are required to sign in with Reception in the Administrative Building 10 2 3 Normal operating hours for the laboratory are 7 30 AM to 4 00 PM Monday through Friday A Laboratory Technician is present 7 30 AM to 4 00 PM on Saturdays Building Services 10 3 1 Air Temperature and Quality The laboratory s heating and air conditioning are generally to control laboratory temperatures between 68 and 75 F and temperature fluctuations rarely exceed more than 4 degrees per hour 10 3 2 Electricity 110 and 220 volt electrical service is provided throughout the laboratory 10 3 3 Illumination Lighting in most areas and all work areas is provided by fluorescent lighting Emergency lighting is located throughout the lab 20 TB Laboratory QAP September 16 2009 Revision 1 10 4 10 5 10 6 Safety 10 4 1 Fire Safety Fire alarms are located throughout the building Fire extinguishers are prominently displayed throughout the lab and all laboratory personnel are tra
97. of 219 Revision Number 3 Last Revised 09 09 Expected Results 10 1 KPDES Permit Requirements None required If value is inconsistent DNS Data Not Supportable is typed into computer 10 2 Process Ranges The practical determination range is 10 mg L to 20 000 mg L Data Analysis and Calculations 11 1 Volatile Solids mg L W3 W4 W2 W1 1 000 000 112 Volatile Solids W3 Wa W3 W1 100 Bibliography 12 1 U S EPA Method 160 4 Residue Volatile Gravimetric Ignition at 550 C Issued 1971 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 12 2 Standard Methods Part 2540 E Fixed and Volatile Solids Ignited at 550 C APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 96 WEST HICKMAN CREEK SOPs SOP WH FIELD D O West Hickman WWTP Laboratory Page 2 of 219 Revision Number 3 Last Revised 09 09 WH Dissolved Oxygen Field Analysis D O HACH Method 10360 Luminescent Dissolved Oxygen Probe Method Proposed EPA Method 360 3 Luminescence for the Measurement of Dissolved Oxygen in Water and Wastewater Scope Significance to Process and Application 1 1 Dissolved Oxygen D O analysis measures the concentration o
98. of 219 Revision Number 5 Last Revised 09 09 Dissolved Oxygen Analysis D O HACH Method 10360 Luminescent Dissolved Oxygen Probe Method Proposed EPA Method 360 3 Luminescence for the Measurement of Dissolved Oxygen in Water and Wastewater 1 Scope Significance to Process and Application 1 1 The Dissolved Oxygen D O analysis is the measurement of the concentration of oxygen dissolved in a water sample 1 2 This method is recommended for samples containing intense color or turbidity 1 3 This method is recommended for work in the field as the equipment is portable allowing hold times to be minimized 1 4 KPDES Permit Limits on Plant Effluent is a minimum of 7 0 mg L 1 5 Dissolved Oxygen concentration levels are very important in both process plant effluent In process dissolved oxygen is required by various organisms and the plant effluent dissolved oxygen levels must be conducive to the receiving environment and within permit limits See Section 10 1 2 Summary of Method 2 1 Executive Summary Dissolved Oxygen is measured directly by a HACH model HQ40d portable meter and HACH model LBOD101 probe located on the BOD bench After the meter indicates a stable reading the analyst records the value 2 2 Discussion The HACH LDO system uses a sensor coated with a luminescent material Blue light from an LED is transmitted onto the sensor surface exciting the luminescent material which then emits red light as
99. one ManVer 2 Hardness Indicator Powder Pillow and stir 7 Titrate the sample with 0 800 M EDTA titrant until the color changes from red to pure blue 8 Read the concentration of total hardness as mg L CaCOs directly from the digital counter window 61 10 11 12 SOP Hardness LFUCG Laboratory Page 62 of 219 Revision Number 2 Last Revised 09 09 QA QC Requirements 9 1 None required Expected Results 10 1 KPDES Permit Requirements None required Monitored quarterly by 24 hour composite sample concurrent with whole effluent testing 10 2 Process Ranges i Average Annual Hardness 247 mg L Minimum monthly average 177 mg L Maximum monthly average 321 mg L Based on DMR data January 1 2001 through June 30 2006 Data Analysis and Calculations 11 1 None required Bibliography 12 1 HACH Water Analysis Handbook Method 8213 Hardness Total with a Digital Titrator 2 Edition 1992 HACH Company Loveland CO 12 2 Standard Methods 2340 C APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 12 3 U S EPA Method 130 2 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 62 SOP pH LFUCG Laboratory Page 63 of 219 R
100. ore IM U Sae uasAxo Poajossi uoyyurjdoyAud pue av8ye syuejd ogenbe jo sisayyu sozoyd jo pnpoid asem e se pue juatusaow pider uogezoe Aq ire Supunoiins DYP Way UOTSAJTP Aq apem ogui 5108 ua3Axg uopnjos snoanbe ue uy paajosstp 10 uag Axo snoosel jo JUNOULE SY soINseaw SIS JRUR OQ ua sxo paasjossta spaepurys 351 Syenbe sprepueyg 1038 EMNE AAR uo poseg yeqgepy onenby IJCMAUNE Ma a1qeidadoy ayqeidadoeury A S SuIOz 1 3u pp HVM Loe 9045 A IJE MUE M SOISEM ame 310 WOI UOUE JUO peust ts ABUT sposo UaSAXO MO spewurue pue syueyd ogenbe jo yuouruoraus Auyyeey e yroddns O JoyeM SOPJIMS Y JO JIIQE I aye IpuT SPAJ USB XO SIQJRA VANJOU UT 10398 Loy WO V st US SAXO paajossig uasAXO P3AJOSSIC Y A a AVIYLS YILVAN NEVA UAE NAL _ LLL JONVY NOOd O NIDAXO OINTOSSIO O CRIO Moe a PURA UD LER e AS ROG Od Audio SIMP US puso SHOPPE enamine e sae meee Pin AA an Ay BARE yo MERTEN PPO O OAE SILENT POO TAINO AACE AOne qudd Gy poseadsip muodras O UNGWL PBUTRYO M JO anu aya apoy 61 aang 97 asad 350 361 HPO UUAA TUORE IYI 2nunuos pue sora yop qye simodo ugya 10103 jujodpuo aya 21039q ida 3 peas JONAH ays UO AUT vio moq ayi Soy3e0 du aunda yy S sa BAYO pporjossq wdd up osas 359 Py pea aros 101241 O NANY dp aakungd ayi ayp sacacdesip asof 1002 ang ap pun dupenp arupuos pue 1014 pur den aya aoejday y any wm poys ajdutns ayj 10 Ep ep
101. partially filled with water then fill to volume 4 Calibration Standard 4 Pipette 5 0 mL of 1000 mg L I stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume 5 Calibration Standard 5 Pipette 10 0 mL of 1000 mg L I stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume 6 Quality Control Sample Pipette 5 0 mL of 1000 mg L I stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume 08 2010 KGS 365 3 Orthophosphate as Phosphate in Water 1 Discussion MDL 0 003 as of 5 2002 Principle Ammonium molybdate and antimony potassium tartrate react in an acid medium with dilute solutions of orthophosphate to form an antimony phospho molybdate complex This complex is reduced to an intensely blue colored complex by ascorbic acid The color is proportional to the orthophosphate concentration Sensitivity The range of determination for this method is 0 010 mg L to 1 000 mg L in the PO P form when analyzed at 880 0 nm Method states using 650nm wavelength or 880 0nm if instrument is capable and the Cary 50 UV Vis is capable Interferences Arsenate iron and silica cause interferences Reducing the arsenic acid to arsenious acid with sodium bisulfite may eliminate arsenate interference When high concentrations of iron are present recovery of phosphorus will be lowered because the iron will use some of th
102. precipitation In the event of a precipitation event the Sampling Coordinator will reschedule the remaining sampling a minimum of 72 hours after the precipitation has ceased Wolf Run Watershed Page 39 of 67 Revision No 0 Based Plan Date April 11 2011 Each volunteer will be equipped with a GPS unit digital camera conductivity meter thermometer and Conductivity Survey Field Datasheets Appendix A Volunteers will each be assigned stream segments as shown in Table 9 and Exhibit 3 Before and after monitoring activities the volunteer shall calibrate the conductivity meters using a standard of known value The standard value initial calibration reading prior to monitoring and final calibration reading after monitoring is completed shall be recorded on the datasheets along with the meter identification number serial number Calibration and measurements with the conductivity meter shall be performed according to the specifications in the instruction manual see Appendix B Volunteers will begin the survey in the upstream portion of these reaches and work downstream recording the time of measurement latitude and longitude NAD83 decimal degrees conductivity temperature and additional observations including anomalous conditions if applicable at each site Photographs will be taken to document unusual conditions with the photograph numbers indicated on the datasheet Datasheets will be used to document only one stream reach and m
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104. reporting limit method blank contamination Completeness Amount of valid data required Ensure all data is reported with a useable result Preservation Handing Analyzed within hold time and properly preserved Interference Elimination of distorting or inhibiting effects on the measurement Other Describe non conformance Yes No Indicates that the is in conformance out of conformance with the projects DQI If the DQI is not relevant to the data write N A in the comments column Page 1 of 1 APPENDIX B STANDARD OPERATING PROCEDURES Wolf Run Watershed Page 67 of 67 Revision No 0 Based Plan Date April 11 2011 Lexington Fayette Urban County Government Division of Water Quality Town Branch Laboratory Quality Assurance Plan QAP and Standard Operating Procedures SOPs July 8 2008 Revised September 16 2009 David J Price Ph D Laboratory Supervisor TB Laboratory QAP September 16 2008 Revision 1 Table of Contents FORWARD a aoe Hae 1 O 2 Quality Policy Statement annist ascot dd i Betis e OO 2 1 1 Quality Policy atentan i E E R a a a 2 1 2 Specific ODISEA ad 2 3 QAP Availability ss ado ls e eo ele O 2 SECON 2 ee E bee i See 3 Laboratory Organization and Staff Responsibilities 0 0 0 ee esceseesceereeeeeeeecesecneeeeeeaeeeeeeereaees 3 2 1 Laboratory Oreani Za ton sassszaccgess sissy chi ii 3 2 2 AA a a e a r a 3 2 3 Current Personnel ts Cueva ces to la
105. request Electronic data will be presented in Adobe Acrobat Microsoft Word and or Microsoft Excel depending on the data type These final reports are as follows Karst Hydrograph Characterization in the Wolf Run Watershed Assessment of Habitat and Macroinvertebrates in the Wolf Run Watershed Conductivity Survey of the Wolf Run Watershed Hydrogeomorphic Assessment of the Wolf Run Watershed Wolf Run Watershed Monitoring Report Wolf Run Watershed Based Plan Final Project Report The Wolf Run Watershed Monitoring Report will include an evaluation of the quality assurance and will compare the data produced under the water quality monitoring to the data quality indicators listed herein The Wolf Run Watershed Based Plan will be developed in accordance with the KDOW s Watershed Planning Guidebook for Kentucky Communities 2010 and meeting the USEPA s nine key elements for watershed based plan The Final Project Report will meet the requirements of the KDOW Project Final Report Guidelines for Clean Water Act 319 h Funded Projects 2004 In addition to these reports quarterly Section 319 h Nonpoint Source Project Progress Report will be submitted to the KDOW to document the progress on the project milestones SECTION B DATA GENERATION AND ACQUISITION B1 Sampling Process Design As previously mentioned this QAPP addresses six different monitoring types A summary of the sampling locations and rationale behind the monitoring type
106. reviewed 15 3 2 Once a discrepancy is established staff should proceed with one or more of the following 1 re run samples if available and holding time permits 2 document results as invalid and note on any reports 3 investigate discrepancy document cause and corrective action taken and include with data 15 3 3 Staff responsible for investigating the discrepancy shall review sample and quality control results integrity of quality control samples and technique If a quality control result does not meet method or laboratory criteria it shall be documented on the analysis bench sheet and quality control chart Staff should also review sampling procedures and preservation washing of glassware and any sources of contamination to samples or quality control standards 33 TB Laboratory QAP September 16 2009 Revision 1 15 4 15 3 4 The Laboratory staff performs corrective actions to eliminate any of the above mentioned possible causes for data discrepancies Examples of corrective actions are review of proper procedures quality control standard preparation changes to procedures or sampling protocol and improving analyst technique If the investigation cannot determine a known cause for invalid results retraining and procedure review are the appropriate corrective actions 15 3 4 For each data discrepancy event the investigation and corrective action shall be documented Documentation and Review of Corrective Action Labor
107. separated anions in their acid form are measured using an electrical conductivity cell Anions are identified based on their retention times compared to known standards Quantitation is accomplished by measuring the peak area and comparing it to a calibration curve generated from known standards Sensitivity Ion Chromatography values for anions ranging from 0 to approximately 40 mg L can be measured and greater concentrations of anions can be determined with the appropriate dilution of sample with deionized water to place the sample concentration within the working range of the calibration curve Interferences Any species with retention time similar to that of the desired ion will interfere Large quantities of ions eluting close to the ion of interest will also result in interference Separation can be improved by adjusting the eluent concentration and or flow rate Sample dilution and or the use of the method of Standard Additions can also be used For example high levels of organic acids may be present in industrial wastes which may interfere with inorganic anion analysis Two common species formate and acetate elute between fluoride and chloride The water dip or negative peak that elutes near and can interfere with the fluoride peak can usually be eliminated by the addition of the equivalent of 1 mL of concentrated eluent 100X to 100 mL of each standard and sample Alternatively 0 05 mL of 100X eluent can be added to 5 mL of each stan
108. specified forms of phosphorus in surface waters domestic and industrial wastes and saline waters They may be applicable to sediment type samples sludges algal blooms etc but sufficient data is not available at this time to warrant such usage when measurements for phosphorus content are required The methods are based on reactions that are specific for the orthophosphate ion Thus depending on the prescribed pretreatment of the sample the various forms of phosphorus shown above may be determined Except for in depth and detailed studies the most commonly measured forms are phosphorus and dissolved phosphorus and orthophosphate and dissolved orthophosphate Hydrolysable phosphorus is normally found only in sewage type samples and insoluble forms of phosphorus as noted are determined by calculation The methods are usable in the 0 01 to 0 5 mg L P range Precision Ability of self duplication amount of spread between replicates Range Measure of dispersion of values and is merely the difference between the largest and the smallest of a group of measurements 47 TB Laboratory QAP September 16 2009 Revision 1 Reagent Substance used in a chemical reaction to produce another substance or to detect its composition Reliability Measure of a method s ability to achieve both accuracy and precision Risk The probability that a substance will produce harm Risk Assessment Takes into account possible harmful effects on individua
109. streams embayments or pools which can get very warm in mid summer 5 ii SAMPLE COLLECTION METHODS FOR IMMUNOASSAY TESTING CHECKLIST _Chain of Custody Record Field Data Sheet __Pre cleaned amber glass bottle with Teflon lined screw cap ae Water proaf pen Scripis Ice Cooler or bucket Waders and gloves as desired COLLECTION METHOD Avoid disturbing sediment layer If you are wading into the stream allow the water to clear before you take the sample Face upstream water js running toward you to sample so that contaminants from your hands will not be collected Collect the sample only in the pre cleaned amber glass bottle provided DO NOT use any plastic container Rinse the collection bottle three times in the water to be sampled before the final fill Fill with mouth of bottle facing upstream away from your bady or hands Fill the bottle no air space if at all possible Cap with the Teflon lined screw cap provided Complete information on the chain of custody record Be sure the sample number on the chain of custody Record matches the sample number on the lid of the bottle Chill on ice immediately keep refrigerated or on ice until the sample reaches the lab CHAIN OF CUSTODY Complete chain of custody record for each sample taken Be sure your sample cade is indicated in the upper right hand comer of the Chain of Custody Record Please include a complete site description with reference points you wou
110. support fish Levels of 5 to 6 ppm are usually required for growth and activity This test kit uses the azide modification of the Winkler method for determining dissolved oxygen TABLE OF CONTENTS Page Kit Contents siiessiccadicecsicwiesensesckeeetesescadscsecsessecesseessesccseanoseee 2 Test Procedure Part 1 Collecting a Water Sample cicstssanccsasecicbicseondavies 3 Part2 Adding the Reagents sesriscsrisesisessiisiesiiisseisiss 4 Part 3s A eee er enS 5 EPA C oti plintic indvcuscsmiaenaummaunhnumaioknusn TO Dissolved Oxygen Fact She tsssissassesssicnssissancssossanassctessinasas LO General Safety Precios ninas 13 Use Proper Analytical Technrriques ccrcscorsssssscessssees 14 Material Safety Data Sheets siii 15 Kit Diagrams sccccsccscssssssssscssscsscsssesesscssscsscssseseeescces Z Short Form Instructions cccccsscessssceessceeeseeeeeee Back Cover WARNING This set contains chemicals that may be harmtul if misused Read cautions on individual containers carefully Not to be used by children except under adult supervision KIT CONTENTS QUANTITY CONTENTS CODE 30 mL Manganous Sulfate Solution 4167 G 30 mL Alkaline Potassium Iodide Azide 7166 G 50 g Sulfamic Acid Powder 7414 Kit 6286 H 30 mL Sulfuric Acid 1 1 5860 Kit 6141WT G 60 mL Sodium Thiosulfate 0 025N 4169 H 30 mL Starch Indicator Solution 4170WT G 1 Spoon 1 0 g plastic 7414 Kit 06
111. technicians must meet either of the following requirements for analyses performed utilizing specialized laboratory instrumentation 1 e Atomic Absorption e The technician shall have satisfactorily completed a minimum of four hours training that is offered by the equipment manufacturer a professional organization a university or qualified training facility e The technician shall have served a two week period of apprenticeship under an experienced staff member Training Records Laboratory management maintains employee training records The records are updated periodically for each employee receiving training 41 TB Laboratory QAP September 16 2009 Revision 1 Section 22 Glossary Acid An inorganic or organic compound that a reacts with metals to yield hydrogen b reacts with a base to form a salt c dissociates in water to yield hydrogen or hydroniumions d has a pH of less than 7 0 and e neutralizes bases or alkaline media Accuracy Degree of conformity of a measure or test to a standard or true value Aliquot A portion of a sample Alkali Any compound having highly basic properties ATM Atmosphere pressure measurement Arsenic As The major source of occupational exposure to arsenic is in the manufacture of pesticides herbicides and other agricultural products Barium Ba Barium is used in various alloys in paints soap paper and rubber Base A substance that usually liberates OH anions
112. the preparation and analysis of a minimum of one matrix spike sample spiked at the current MDL Results are verified by the laboratory supervisor e An MDL is considered verified and acceptable for continued use if results of the analysis of the matrix spike sample are within the 95 confidence interval as set forth in Appendix B of 40 CFR Part 136 e Ifan MDL cannot be verified a new MDL is determined MDL replicate percent a recovery acceptance criterion is defined by the range of the percent mean recovery 2 times the percent relative standard deviation RSD found for the seven replicates If any of the seven replicates fails this acceptance criterion then the analyst discards all results and performs another set of seven replicates The spiking concentrations used to determine an MDL are between 1 and 10 times the calculated MDL Internal Audits 6 10 1 The laboratory conducts annual internal audits of its operations QA QC practices and record keeping 6 10 2 The internal audit is performed by the designated quality assurance officer 11 TB Laboratory QAP September 16 2009 Revision 1 6 11 6 12 6 13 6 14 6 10 3 The results of the internal audit should specify procedures or practices that are not in compliance with the QAP and corrective action shall be taken and documented 6 10 4 Where the results of an internal audit indicate that the laboratory s test results are invalid the laboratory takes imme
113. the spiking eluent The Filter Caps are pressed into the Polyvials using the insertion tool Place the Polyvials into the Sample Cassette which is placed into the Autosampler The white black dot on the Sample Cassette should be located on right hand side when loaded in the left hand side of the Automated Sampler for System 2 For every ten samples the following should be included a 1 DI water blank b 1 Duplicate of any one sample c 1 Quality Control sample calibration check C Calibration and Sample Analysis 1 2 MAA E Set up the instrument with proper operating parameters established in the operation condition procedure The instrument must be allowed to become thermally stable before proceeding This usually takes 1 hour from the point on initial degassing to the stabilization of the baseline conductivity To run samples on the Dionex Ion Chromatography System a Make a run schedule on the Chromeleon 6 8 Software Section labeled SEQUENCE b Double click the mouse on the SYSTEM 1 SEQUENCES or SYSYTEM 2 SEQUENCES to display the Scheduler Area The name of the calibration standards must be entered under the sample name section as Standard 1 Standard 2 and Standard 3 Note Level must be changed to the corresponding standard level or the calibration will be in error Example Standard 1 Level 1 Standard 5 Level 5 c Next enter QC blanks QC samples duplicates QC and blanks in that order d
114. this Comprehensive Quality Assurance Plan Laboratory Management is responsible for ensuring the required training is made available Training Required for Laboratory Supervisor 21 2 1 The Laboratory Supervisor shall hold a bachelor s degree in natural or physical sciences or have completed enough course work in chemistry to equal a major in chemistry 21 2 2 The Laboratory Supervisor shall have a minimum of one year s experience in analyses pertaining to the applicable fields of testing Training Required for Quality Assurance Officer 21 3 1 The QA Officer shall hold a bachelor s degree in natural or physical sciences or have completed enough course work in chemistry to equal a major in chemistry 21 3 2 The QA Officer shall have a minimum of one year s experience as an analyst in a laboratory 21 3 3 The QA Officer shall have documented training in quality assurance and quality control Training Required for Technicians 21 4 1 Technicians shall hold a bachelor s degree in natural or physical sciences or have completed enough course work to equal a major in chemistry 21 4 2 Technicians shall have a minimum of one year s experience in the analyses pertaining to the applicable fields of testing 21 4 3 Technicians shall meet the instrument training requirements specified in Section 21 9 21 4 4 After completing training technicians shall perform an Initial Demonstration of Method Performance IDMP study for each analysi
115. to increased turbidity siltation and other effects Ortho phosphorus total phosphorus nitrate nitrite and TKN will be assessed to identify imbalances which may cause eutrophication and impacts to stream biota Ammonia will be assessed to evaluate levels for toxicity to plants animals and humans Alkalinity and hardness will be assessed to measure the buffering capacity of the water against rapid pH changes Because E coli levels will be evaluated against the geomean criteria it is necessary to collect five samples in 30 days for this project For other parameters at least two dry weather and two wet weather events will be sampled at all sites in order to adequately characterize the loadings geographically It is expected that no flow conditions will be observed in the watershed during the sampling period Wolf Run Watershed Page 35 of 67 Revision No 0 Based Plan Date April 11 2011 B2 Sampling Methods B2 1 Sampling Equipment Equipment to be utilized in sampling is listed in Table 3 Sampling Equipment Summary Samples are to be collected and preserved according to the specifications in Table 10 Parameter E coli Analysis Method SM 9221 E Maximum Holding Time Sample Container Sterilized Plastic 4 oz Fecal Coliform SM 9221 F Sterilized Plastic 4 oz Sample Preservation Cool lt 6 C Na S 03 No Cl Ammonia EPA 350 1 Plastic 8 oz Cool lt 6 C NaoS 03 No CL
116. to possess a valid driver s license e Physical strength and agility to allow considerable walking lifting climbing and working with samples that are odorous and hazardous e Must be able to work weekends and holidays and perform on call duty e Must be able to operate Urban County Government equipment and vehicles in a safe prudent and responsible manner e All positions require drug testing before employment and will require a pre TB Laboratory QAP Appendix C September 16 2009 Revision 1 employment physical as stated in Ordinances 2114 b and 23 16 e Pursuant to the Drug Free Workplace Act of 1988 and to sections 21 52 22 34 and 23 50 of the Code of Ordinances all employees must remain drug and alcohol free when reporting to work while at work and while engaged in any work related activities e Based on Federal Regulation 19 10 some positions in this classification are eligible for and will be offered the hepatitis vaccinations In addition employees will be required to sign a statement stating they have accepted or declined the hepatitis vaccination TB Laboratory QAP Appendix C September 16 2009 Revision 1 APPENDIX C CURRENT PERSONNEL AND LAB APPROVED SIGNATURES TB Laboratory QAP Appendix C September 16 2009 Revision 1 Appendix C Current Personnel and Laboratory s Approved Signatures Job Title Laboratory Supervisor Name Dr David J Price Employee 46274 Education Ph D Biology University of Kent
117. transducers with data loggers will be installed at each of the five gaging stations Flow measurements will be conducted according to KDOW s Measuring Stream Discharge Standard Operating Procedure KDOW 2010b A minimum of 5 percent replicate measurements will be made during this gaging effort The base flow event will consist of a single flow measurement at each of six gaging stations as shown on the attached Exhibit 2 It is anticipated that the base flow period will begin in mid summer and extend to early fall The wet weather event will target a storm event that is expected to have uniform rainfall across the watershed with expected accumulation of over inch The gaging will be performed by two teams of surveyors circulating to each of the five gaging points a minimum of every thirty minutes during the storm event Monitoring will continue until well past the hydrograph peak A6 1 2 Conductivity Survey During medium to low flow conditions 0 5 to 5 cfs at the USGS gage the Wolf Run watershed will be surveyed by in situ field temperature and specific conductance measurements to identify locations of jumps in the specific conductance levels as possible locations of pollution Using GPS data loggers field meters data sheets and photographs all streams and tributaries approximately 13 5 miles will be measured at approximately 100 foot intervals approximately 700 locations Volunteer samplers will be trained to perform this study
118. undergo extreme amounts of oxidation leaving no oxygen for the living organisms which eventually leave or suffocate OTHER FACTORS The oxygen level of a water system is not only dependent on production and consumption Many other factors work together to determine the potential oxygen level including e Salt vs fresh water Fresh water can hold more oxygen than salt water e Temperature Cold water can hold more oxygen than warm water e Atmospheric pressure Altitude The greater the atmospheric pressure the more oxygen the water will hold TESTING DISSOLVED OXYGEN Dissolved oxygen is often tested using the Azide modification of the Winkler method When testing dissolved oxygen it is critical not to introduce additional oxygen into the sample Many people avoid this problem by filling the sample bottle all the way and allowing the water to overflow for one minute before capping The first step in a DO titration is the addition of Manganous Sulfate Solution 4167 and Alkaline Potassium Iodide Azide Solution 7166 These reagents react to form a white precipitate or floc of manganous hydroxide Mn OH Chemically this reaction can be written as MnSO 2KOH gt Mn OH K2SO Manganous Potassium gt Manganous Potassium Sulfate Hydroxide Hydroxide Sulfate 12 Immediately upon formation of the precipitate the oxygen in the water oxidizes an equivalent amount of the manganous hydroxide to brown
119. upper right side of the screen Meter is now calibrated and ready for sample measurements 22 Record the slope temperature buffer values time calibrated and initials in the bench sheet and calibration folder Sample Measurements 1 Touch the meas button on the upper right side of the screen 2 When testing samples for pH place probe into sample container and record the reading once the measurement has become stable STABLE will appear once the meter recognizes that the measurement is stable 3 Turn off stirrer and rinse probes with Nanopure water between samples 4 When all analytes have been tested for that day touch the mode button to put meter into power save mode 5 Replace plastic sleeve or cap to cover hole in pH probe for safe storage 6 Store pH probe in pH 7 0 buffer solution Weekend Check Standard 1 For Sunday operators calibrate meter as described in Section 8 1 2 Measure pH of Buffer Solution pH 6 86 to ensure meter is working correctly Record value of Check Standard in bench sheet 3 Proceed to measure samples as described in Section 8 2 Helpful Hints 1 Avoid strong acids and greasy samples 2 Make sure that probe is thoroughly rinsed between samples to avoid cross contamination 66 10 11 12 SOP pH LFUCG Laboratory Page 67 of 219 Revision Number 3 Last Revised 09 09 QA QC Requirements 9 1 If sample is not collected properly or analyzed within 15
120. 00 mL 1 6 ppm 16 mL of 10 ppm diluted to 100 mL 2 9 ppm 29 mL of 10 ppm diluted to 100 mL 3 The QC is diluted from the ordered solution perform an appropriate dilution creating a QC with a value midway on calibration curve 1 5 ppm using the ordered standard 4 If it is deemed necessary ICV s Initial Calibration Verification and CCV s Continued Calibration Verification can be run using a 0 8 ppm and or 1 6 ppm glutamic acid solution Pao C Sample Prep 1 The Prep Blank is 10 mL of reagent grade DI water poured into the first liner 2 For all samples and QC a 10 mL aliquot should be poured into one of the advanced composite vessels or ACV liners 3 Add 5 mL of Digestion Reagent to each liner 4 Assemble the ACV system as described in Microwave Digestion GLP D Digestion Set Up From the options on the main menu of the microwave press F3 Recall Method Data Press Fi Recall Stored Method Use arrow keys to scroll down to TKN SM press Enter Press Fl Load Program Press F4 Start Press FI Yes Once a digestion is started watch the temperature probe and pressure tube carefully to make sure they do not become tangled up If they do become tangled press F1 to abort the run and remedy the problem 7 Once the run is complete disassemble the ACV s add 1 mL of Borate Buffer Solution to each liner all QC samples dups etc and pour the digested samp
121. 06 16 6 5 41 22 1 4 02 0 3 4 37 5 8 4 72 11 3 5 07 16 7 5 42 22 2 4 03 0 4 4 38 5 9 4 73 11 4 5 08 16 9 5 43 22 4 4 04 0 6 4 39 6 1 4 74 11 6 5 09 17 1 5 44 22 6 4 05 0 7 4 40 6 2 4 75 11 7 5 10 17 2 5 45 22 7 4 06 0 9 4 41 6 4 4 76 11 9 5 11 17 4 5 46 22 9 4 07 1 1 4 42 6 5 4 77 12 0 5 12 17 5 5 47 23 0 4 08 1 2 4 43 6 7 4 78 12 2 5 13 177 5 48 23 2 4 09 1 4 4 44 6 9 4 79 12 4 5 14 17 8 5 49 23 3 4 10 1 5 4 45 7 0 4 80 12 5 5 15 18 0 5 50 23 5 4 11 1 7 4 46 7 2 4 81 12 7 5 16 18 2 5 51 23 7 4 12 1 8 4 47 7 3 4 82 12 8 5 17 18 3 5 52 23 8 4 13 2 0 4 48 TS 4 83 13 0 5 18 18 5 5 53 24 0 4 14 2 1 4 49 7 6 4 84 13 1 5 19 18 6 5 54 24 1 4 15 2 3 4 50 7 8 4 85 13 3 5 20 18 8 5 55 24 3 4 16 2 5 4 51 8 0 4 86 13 4 5 21 18 9 5 56 24 4 4 17 2 6 4 52 8 1 4 87 13 6 5 22 19 1 5 57 24 6 4 18 2 8 4 53 8 3 4 88 13 8 5 23 19 3 5 58 24 7 4 19 2 9 4 54 8 4 4 89 13 9 5 24 19 4 5 59 24 9 4 20 3 1 4 55 8 6 4 90 14 1 3 29 19 6 5 60 25 1 4 21 3 2 4 56 8 7 4 91 14 2 5 26 19 7 4 22 3 4 4 57 8 9 4 92 14 4 5 27 19 9 4 23 3 6 4 58 9 1 4 93 14 5 5 28 20 0 4 24 3 7 4 59 9 2 4 94 14 7 5 29 20 2 4 25 3 9 4 60 9 4 4 95 14 9 5 30 20 4 4 26 4 0 4 61 9 5 4 96 15 0 5 31 20 5 4 27 4 2 4 62 9 7 4 97 15 2 5 32 20 7 4 28 43 4 63 9 8 4 98 15 3 5 33 20 8 4 29 4 5 4 64 10 0 4 99 15 5 5 34 21 0 4 30 47 4 65 10 2 5 00 15 6 5 35 21 1 4 31 4 8 4 66 10 3 5 01 15 8 5 36 21 3 4 32 5 0 4 67 10 5 5 02 16 0 5 37 21 5 4 33 5 1 4 68 10 6 5 03 16 1 5 38 21 6 4 34 5 3 4 69 10 8 5 04 16 3 5 39 21 8
122. 1 2 3 4 If the bacterial density of the sample is unknown filter and plate out several volumes or dilutions in order to achieve a countable density The volumes and or dilutions should be expected to yield a countable membrane In addition select two additional quantities representing one tenth and ten times this volume respectively Separate filter holder units may be required during a set of samples These will be indicated in the bench sheet Do not use damaged or bent membrane filters Rinse the filter unit thoroughly with Peptone buffer to avoid cross contamination 9 QA QC Requirements 9 1 Before and After Blanks must be run with each set of samples tested 9 2 One duplicate per test series must be run 58 10 11 12 SOP Total Coliforms and E coli LFUCG Laboratory Page 59 of 219 Revision Number 1 Last Revised 09 09 Expected Results 10 1 KPDES Permit Requirements Currently there are no permit requirement on E coli Data Analysis and Calculations 11 1 See SOP Fecal Coliform 11 2 Blue colonies are counted as E coli and red colonies are other coliforms total coliforms are the sum of the two Bibliography 12 1 HACH Method 10029 Coliforms Membrane Filtration 2009 12 2 U S EPA Microbiological Methods for Monitoring the Environment Water and Wastes EPA 600 8 78 017 U S Environmental Protection Agency Environmental Monitoring and Support Laboratory Office of Research and
123. 1 7 Record results in bench sheet 8 The Laboratory Supervisor will determine if the standard is within the expected range 9 Measure 200 mL of Nanopure water into a clean 250 mL beaker and analyze as indicated in Section 8 1 This will be a Blank to confirm no chlorine carry over Record results in bench sheet 10 If chlorine is detected re run Blank until Below Detection Limit BDL is obtained Helpful Hints 1 Analysis results are directly proportional to sample volumes therefore it is very important that sample volume measurement is accurate 2 Clean conditioned electrodes are required for the production of sharp well defined endpoints that are needed for precise analysis Rinse electrodes thoroughly before and after each use with Nanopure water and store in Nanopure water 3 Routine use of the Electrode Cleaning and Conditioning procedure as described in Section 9 1 4 of the Operator s Manual will prevent problems 4 Glassware must be clean and free of chlorine demand see section 4 3 QA QC Requirements 9 1 9 2 9 3 A diluted standard 25 30 mg L and Blank s must be run once a week See Section 8 2 5 of all samples must be run in duplicate Data acceptance criteria 1 Results for the Standard must agree within 10 of the standard s known value 2 Duplicate values must agree within 5 3 Ifthese criteria are not met corrective action is indicated See Quality Assurance Program QA
124. 11 A7 2 5 Comparability Comparability is a term that expresses the measure of confidence that one data set can be compared to another and can be combined for the decision to be made Comparability may be assessed by comparing sampling methodology analytical methodology and units of reported data The standards of quality established in this QAPP are consistent with the previously collected data in the Wolf Run watershed collected under separate QAPPs All data to be utilized in the generation of the watershed based plan source and loading determinations will have been generated under an approved QAPP A7 2 6 Sensitivity Sensitivity is the capability of a method to discriminate between measurement responses representing different levels of the variable of interest Sensitivity is particularly important for ensuring that the measurement levels are sufficient to detect whether particular pollutants are present at levels that may cause impairment to the designated use For grab sampling and in situ measurements the sensitivity levels necessary for this program are specified in Table 6 For macroinvertebrate sampling all organisms are to be identified to the lowest possible taxonomic level possible in order to properly calculate the associated metrics A8 Training Requirements All volunteers involved in the sampling for this project shall have successfully completed the training workshops lead by a trainer registered with the KDOW Watershed Watc
125. 11 3 Ifa separation of the settleable and floating materials occurs do not estimate the floating materials 11 4 Detection limit 0 01 mL L 11 5 Settled Sludge mL of sludge in settled mixed liquor X 100 1000 Bibliography 12 1 U S EPA Method 160 5 Residue Settleable Matter Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 12 2 Standard Methods Part 2540 F Settleable Solids APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 12 3 Code of Federal Regulations CFR Guidelines Establishing Test Procedures for the Analysis of Pollutants 40 CFR 136 3 Title 40 Chapter 1 U S Environmental Protection Agency U S Environmental Protection Agency pg 5 337 2003 12 4 Simplified Laboratory Procedures for Wastewater Examination Water Pollution Control Federation Third Edition pg 17 18 1985 80 SOP TSS LFUCG Laboratory Page 81 of 219 Revision Number 3 Last Revised 09 09 Total Suspended Solids TSS EPA Method 160 2 Residue Non Filterable amp Total Suspended Solids Standard Methods Part 2540 D Scope Significance to Process and Application 1 1 This method is applicable to drinking surface and saline waters domestic and industrial wastes 1
126. 12 months from the date of purchase the electrode module is warrantied for a period of 6 months from the date of pur chase If repair adjustment or replacement is necessary and has not been the result of abuse or misuse within the 6 month period please return the Testr freight pre paid and correction will be made without charge Out of warranty prod ucts will be repaired on a charge basis Return of Items Authorization must be obtained from your OAKTON Distributor before returning items for any reason When applying for authorization please include information regarding the reason the item s are to be returned Note We reserve the right to make improve ments in design construction and appearance of products without notice Prices are subject to change without notice SBR We Watershed Watch Water Chemistry Sampling Methods For Field Chemistry and Lab Analysis audpe yo Upmord ay 10 asus sag SUE SAL UTA SAR avare opnibsogy Lv ee anpes ya isng Je padorjsap are svae oymbsoyy e83a ysy 103 93uez Geaq umuda ea os spay A asaig pucdag SISJEM PIOAR USTA PIL FS siyem Sunysy pool 107 man ddn ozs Bee USE Sou TOJ asus IGUIBO L 06 06 ae i YS PEGON 16 spur poe as yarad 103 spun yy Kpeunou dojasap seaze pue s3 3 3nox St non Aq papajo auey semeds YSY JUBJSISII JSO DU JO SRUNI paonpord uao are BunoA pounoyop ama papey aq pmo s339 ysu 5109
127. 124 4 94 171 5 29 218 3 90 32 4 25 79 4 60 125 4 95 172 5 30 219 3 91 33 4 26 80 4 61 127 4 96 173 5 31 220 3 92 35 4 27 81 4 62 128 4 97 175 5 32 222 3 93 36 4 28 83 4 63 129 4 98 176 5 33 223 3 94 37 4 29 84 4 64 131 4 99 177 5 34 224 3 95 39 4 30 85 4 65 132 5 00 179 5 35 226 3 96 40 4 31 87 4 66 133 5 01 180 3 97 41 4 32 88 4 67 135 5 02 181 3 98 43 4 33 89 4 68 136 5 03 183 3 99 44 4 34 91 4 69 137 5 04 184 4 00 45 4 35 92 4 70 139 5 05 186 1 SOP NH LFUCG Laboratory Page 8 of 219 Revision Number 1 Last Revised 09 09 Nitrogen Ammonia HACH Method Salicylate Method 10205 TNT 830 ULR 0 015 to 2 000 mg L NH3 N TNT 831 LR 1 to 12 mg L NH3 N TNT 832 HR 2 to 47 mg L NH3 N EPA Method 350 1 Scope Significance to Process and Application 1 1 Ammonia concentrations in wastewater samples are an indication of nutrient levels in the wastewater process stream The reduction of ammonia levels throughout the wastewater treatment process is highly important as plant effluent nutrient concentrations must be low enough See Sec 10 1 Permit Requirements so as to avoid detrimental effect on the receiving environment Low level ammonia nitrogen may be present in water naturally as a result of the biological decay of plant and animal matter Higher concentrations may be found in raw sewage and industrial effluents High concentrations in surface waters can indicate contamination from waste treatment facilities ind
128. 2 Gravimetric Dried at 103 105 C Issued 1971 Volatile Suspended Solids Method Residue Volatile EPA Method 160 4 Gravimetric Ignition at 550 C Issued 1971 Suspended Solids amp Volatile Suspended Solids Enter Date QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS Analyst Setting Up Analysis Presevation None required Maximum Holding Time 7 days Analyst Reading amp Calculating Analysis Log book Monday Tbmonsht xls TB Suspended Solids Grab era TOWN BRANCH amp WEST HICKMAN WASTEWATER TREATMENT PLANT Town Branch Laboratory 24 Hour Composite Samples Total Solids Method Residue Total EPA Method 160 3 Gravimetric Dried at 103 105 C Issued 1971 Total Volatile Solids Method Residue Volatile EPA Method 160 4 Gravimetric Ignition at 550 C Issued 1971 Total Solids amp Volatile Solids Enter Date Log Number Sample Name Additional Name Notations Date Sample Collected Time Analysis Started Tare Number Wt Tare amp Wet Sample Wt Tare Wt Tare amp Dried Solids Wt Tare amp Ashed Solids Date Analyses Performed QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS Analyst Setting Up Analysis Analyst Reading amp Calculating Analysis Log book Monday Tbmonsht xls TB Total Solids 24Hr vI d Total Solids amp Volatile Solids A gt Log Number Sample Name Additional Name Notations TOWN BRANCH WASTEWATER TREATMENT PLANT
129. 2 1 Executive Summary An initial dissolved oxygen DO reading is taken of the sample or dilution The sample is then incubated in the dark at 20 C for 5 days A final DO reading is then taken Initial and final dissolved oxygen values are entered into a spreadsheet that calculates the BOD and CBOD values which are expressed in milligrams per liter 2 2 Discussion The BOD test measures the amount of oxygen uptake caused by both the biodegradation by micro organisms of organic materials in wastewaters carbonaceous demand and the oxidation of nitrogen forms in wastewaters nitrogenous demand over a 5 day incubation period coupled with calculations to derive the Biochemical Oxygen Demand BOD of the sample tested The CBODs test involves the addition of a nitrification inhibitor to exclude nitrogenous demand allowing the measurement of just the carbonaceous demand CBOD Health amp Safety Precautions 3 1 All municipal and industrial wastewaters are potentially hazardous Gloves and goggles should be worn when dispensing these samples Sample Handling and Preservation 4 1 Collect sample in plastic or glass and store at 4 C 4 2 Run analysis within 48 hours 4 3 Grab samples If tested within 2 hours of collection no cooling is needed If testing cannot start within 2 hours cool to 4 C and test within 6 hours 15 SOP CBOD LFUCG Laboratory Page 16 of 219 Revision Number 5 Last Revised 09 09 4 4 Composite samples
130. 2 One duplicate per test series must be run 9 3 One Known positive must be run per test series 22 10 11 12 SOP WH Fecal Coliforms West Hickman WWTP Laboratory Page 23 of 219 Revision Number 4 Last Revised 09 09 Expected Results 10 1 KPDES Permit Requirements 200 CFU 100 mL for Monthly geometric mean GED 400 CFU 100 mL for Maximum Weekly GED In the event that the GED is exceeds the KPDES permit requirements notify the Plant Superintendent and the Laboratory Supervisor 10 2 Process Ranges lt 1 to gt 120 000 CFU 100 mL Data Analysis and Calculations 11 1 See SOP TB Fecal Coliforms for calculations Bibliography 12 1 U S EPA Microbiological Methods for Monitoring the Environment Water and Wastes EPA 600 8 78 017 U S Environmental Protection Agency Environmental Monitoring and Support Laboratory Office of Research and Development Washington DC 1978 Page 124 122 Kentucky Department for Environmental Protection Kentucky Division of Water and the Kentucky Division of Compliance Assistance Discharge Monitoring Report Manual 2009 August 10 2009 revision 28 pp 23 SOP WH TP West Hickman WWTP Laboratory Page 24 of 219 Revision Number 5 Last Revised 09 09 WH Total Phosphorus Analysis HACH Method 8190 PhosVer 3 with Acid Persulfate Digestion per EPA Method 365 2 Scope Significance to Process and Application Phosphorus in wastewater is almost always present in the f
131. 218 Chromium Hexavalent 1 5 Diphenylcarbohydrazide Method 0 03 to 1 00 mg L Cr Scope Significance to Process and Application 1 1 Measurement of the concentration of total and hexavalent Cr in industrial wastewater samples Summary of Method 2 1 Executive Summary Hexavalent chromium if present in industrial wastewater samples is measured by HACH DR5000 spectrophotometer Hexavalent chromium enters the water from industrial wastes from metal plating facilities and from cooling towers where chromate is used to inhibit corrosion 2 2 Discussion In the total chromium procedure all chromium in the sample is oxidized to the hexavalent chromium Cr The hexavalent chromium then reacts with 1 5 diphenylcarbazide to form 1 5 diphenylcarbazone The amount of red color formed with hexavalent chromium is directly proportional to the amount of chromium present in the sample Determine trivalent chromium by subtracting the results of a separate hexavalent chromium test from the results of the total chromium test Test results are measured at 543 nm Health amp Safety Precautions 3 1 All municipal and industrial wastewaters are potentially hazardous Gloves and safety glasses should be worn when dispensing these samples 3 2 Watch out for broken glass Sample Handling and Preservation 4 1 Collect samples in acid washed glass or plastic containers 4 2 To preserve samples for total chromium analysis adjust the pH to 2 or less
132. 332 UIDILIXPJA UINURUTA sonje Hd Suyra SH oyenbe pue ysy uo pid yo spaga proads awos saa mojaq 31qe ayy Hd quapuadap amyesoduiay sy eyyoBuea yde sormbas sagem Suryup 10 ssedoxd SUJDIJUISTP V VORPULOJYO Suel pax Y ULA Je 3enva Ayruryeyye pue yd amoo o ssecozd pawel e vogepa3eo JO 19p10 uy soaa Hd oypads ambas pauper 1938M0 58M pue Jaa ul paajoAur sdajs ayy yeuljead Jayemajsem Pue Jajem SuLapisuos usym aoueayisis jepeds sey ASiaudG SIP O YSy asneo uve oe yo yd e3e 101130 1 21 gO Se 331 Se 1949M0JH gpjo id Y 3e paza axo e pUsseid jou pynom uon Jo 1 Bu p ojdurexa 104 SODUEISQNS 38943 JO Aue Y SPAJ DIXO IYJ JUTULIDOP J IM 1932M aui jo Hd ou SWA AUO Jo MMIDIDUI emo ue umnununye WOM uauc Aew seawe TeLSNpul pue opsawop Teangpnouse WOH JJOUNY sropem aovpins ur puepoduit si ssaaord styg EMS HOY UY 1938913 soaz aonpord ystyM saourysqns aou 10 OM JO UOTPEUTQUIOD aly SIAJOAUT SU G SPA OSI BIaUAs saatoaut Pid joyoedunpeyua torito guengu SOW BUY 9 21qoyJ9au1 Sunpamp woog pue ysy 19J8MUysa1 yo ayy ayy 103 vopard apraoid oy sreodde y6 0 09 Jo a3uez pd y yoeduwy yeyueuruomaug H 301 Hd se passaidxe srs ALO ea gara Ed aya SOU ULIayap UD RNTOS eu agor apy uor ua8orpAy ay Jo UOgeusduo ayy uonnjos e jo ainyeu Surexpe o1seq 10 orproe ayy jo ammseaut e si yd tornos e ut Sunmo sassadaid peorSojorq pue peoruayo re pperuata spayye anea ud 991 Hd jo prowasnsesu
133. 50 mm Test Tubes Gelman 47 mm Magnetic Vacuum Filter Funnel 500 mL Vacuum Flask and a Vacuum Supply 3 Reagents Purity of Reagents HPLC grade chemicals where available shall be used in all reagents for Ion Chromatography due to the vulnerability of the resin in the columns to organic and trace metal contamination of active sites The use of lesser purity chemicals will degrade the columns Purity of Water Unless otherwise indicated references to water shall be understood to mean Type I reagent grade water Milli Q Water System conforming to the requirements in ASTM Specification D1193 Eluent Preparation for SYSTEM2 NITRATE Methods including Bromides using AG4 AG4 and AS4 columns All chemicals are predried at 105 C for 2 hrs then stored in the desiccator Weigh out 0 191 g of sodium carbonate Na CO3 and 0 286 g of sodium bicarbonate NaHCO and dissolve in water System 2 the chromatography module that contains the AG4 AG4 and AS4 Dionex columns to be sparged using helium of all dissolved gases before operation Eluent Preparation for SYSTEM2 NITRATE E Method using AG14 and AS14 columns Weigh out 0 3696 g of sodium carbonate Na2CO3 and 0 080 g of sodium bicarbonate NaHCO3 and dissolve in water Bring the volume to 1000 mL and place the eluent in the System 1 bottle marked for this eluent concentration The eluent must be sparged using helium as in the above reagent for System 2 Eluent Preparation for SY
134. 6 0 7 3 Data Analysis and Calculations 11 1 None required Bibliography 12 1 U S EPA Method 150 1 pH Electrometric Issued 1971 Editorial revision 1978 and 1982 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 12 2 HACH USEPA Electrode Method 8156 DOC316 53 01245 Edition 5 HACH Company Loveland CO 2008 12 3 Code of Federal Regulations CFR Guidelines Establishing Test Procedures for the Analysis of Pollutants 40 CFR 136 3 Title 40 Chapter 1 U S Environmental Protection Agency U S Environmental Protection Agency pg 5 337 2003 11 1 SOP WH Residual Chlorine West Hickman WWTP Laboratory Page 12 of 219 Revision Number 4 Last Revised 09 09 WH Total Residual Chlorine Analysis HACH AutoCAT 9000 Total Chlorine Amperometric Forward Titration procedure equivalent to EPA Method 330 1 Chlorine Total Residual Titrimetric Amperometric Issued 1978 Standard Methods Part 4500 Cl D Chlorine Residual Amperometric Titration Method 1 1 2 1 2 2 3 1 3 2 Scope Significance to Process and Application Disinfection by chlorination is considered to be the primary mechanism for the inactivation destruction of pathogenic organisms in wastewater treatment plant effluents and to prevent the spread of waterborne diseases to downstream users and the environment Final clarifier effluent
135. 6 2 1 6 2 2 6 2 3 6 2 4 For each test method the quality control measures described in this QAP are followed wherever applicable Additional test method quality control measures may be implemented providing they are more stringent than those in this QAP All quality control protocol and test procedures are assessed and evaluated on an on going basis Quality control procedures follow the direction provided in the test method SOP for evaluation of results and accept reject or qualify sample data based upon the acceptance criteria specified in the test method The laboratory establishes the evaluation procedure and acceptance criteria for a quality control procedure when not specified by the test method Whether specified in the test procedure or established by the laboratory the evaluation procedures and the acceptance criteria are documented either in this QAP or in the test method SOP If a quality control procedure results in the laboratory rejecting or qualifying sample data the problem is investigated appropriate corrective action implemented and the incident documented Method Blanks 6 3 1 6 3 2 Method blanks are prepared and analyzed with each batch of environmental samples and are carried through the entire analytical process The method blank is acceptable if it does not contain an analyte of interest at a concentration greater than the highest of the following a The MDL of the regulatory limit for that ana
136. 7 When time is up remove the tube from the heating block and immediately pull of the sample tube using a downward twisting motion Allow 15 minutes for tubes to cool 8 Rinse the walls of the collector tube Slowly return the collector tube to an upright position to gather all the droplets 9 Break away the top half of the collector tube Dilute to the 6 mL mark with Nanopure water 10 The distilled 6 mL sample in now ready to be analyzed 31 10 SOP Total Cyanide LFUCG Laboratory Page 32 of 219 Revision Number 3 Last Revised 09 09 8 1 2 Reaction 1 Fill sample cell with the 6 mL distilled sample 2 Add 0 580 mL of 2 5N HCI to sample cell cap and shake for 10 seconds 3 Add CyaniVer 3 powder pillow to the 10 mL in sample cell cap and shake for 30 seconds Wait an additional 30 seconds leaving the sample undisturbed 4 Add CyaniVer 4 powder pillow Shake for 10 seconds and immediately proceed to next step 5 Immediately add CyaniVer 5 powder pillow Shake the cell vigorously for 15 seconds 6 Set timer for 30 minutes 7 If there is any cyanide present the sample will turn blue 8 1 3 Using DR4000 spectrophotometer on positive reaction 1 Use Spec Color Standards kit to test and zero the instrument 2 Touch HACH Programs on DR4000 keypad and select program 1750 Cyanide 3 Place BLANK sample into cell holder Close the light shield Touch Zero to zero instrument 4 Place the prepared sa
137. 97 1 Direct Reading Titrator 0377 1 Test Tube 5 10 12 9 15 20 25 mL 0608 glass w cap 1 Water Sampling Bottle 60 mL glass 0688 DO WARNING Reagents marked with a are considered to be potential health hazards To view or print a Material Safety Data Sheet MSDS for these reagents see MSDS CD or www lamotte com To obtain a printed copy contact LaMotte by email phone or fax To order individual reagents or test kit components use the specified code numbers TEST PROCEDURE PART 1 COLLECTING THE WATER SAMPLE Rinse the Water Sampling Bottle Tightly cap the bottle and 0688 DO with the sample water x nae it to the desired depth Remove the cap and allow the Tap the sides of the bottle to bottle to fill dislodge any air bubbles a Retrieve the bottle and make Replace the pa while the sure that no air bubbles are bottle is still submerged trapped inside TEST PROCEDURE PART 2 ADDING THE REAGENTS Il Remove the cap from the bottle 8 drops of Manganous Be careful not to Sulfate Solution introduce air into the 4167 AND sample while adding Add 8 drops of the reagents Alkaline Potassium Iodide Azide 7166 Immediately add Cap the bottle and mix P by inverting several Allow the ae times A precipitate will to settle below the form shoulder of the bottle For Kit Code 7414 For Kit Code 5860 spoon 0697 to add one Sulfuric Acid 1 1 level measure of Sulfamic 6141WT Acid
138. A Dionex Chromeleon 6 8 Software Package Dionex 5 mL Sample Polyvials and Filter Caps 2 L Regenerant Bottles 5 mL Adjustable Pipettor and Pipettor Tips I mL Adjustable Pipettor and Pipettor Tips A Supply of Volumetric Flasks ranging in size from 25 mL to 2 L A Supply of 45 micrometer pore size Cellulose Acetate Filtration Membranes A Supply of 25x150 mm Test Tubes Test Tube Racks for the above 25x150 mm Test Tubes Gelman 47 mm Magnetic Vacuum Filter Funnel 500 mL Vacuum Flask and a Vacuum Supply 3 Reagents Purity of Reagents HPLC grade chemicals where available shall be used in all reagents for Ion Chromatography due to the vulnerability of the resin in the columns to organic and trace metal contamination of active sites The use of lesser purity chemicals will degrade the columns Purity of Water Unless otherwise indicated references to water shall be understood to mean Type I reagent grade water Milli Q Water System conforming to the requirements in ASTM Specification D1193 Eluent Preparation for SYSTEM2 TKN TKN Methods including Total Nitrogen using AG4A AG4A and AS4A_columns Weigh out 0 191 g of sodium carbonate Na CO3 and 0 143 g of sodium bicarbonate NaHCO and dissolve in water Bring the volume up to 1000 ml and place in the System 2 bottle labeled IC TKN 0 191 0 143 Sparge the eluent as in the above reagent for System 2 100X Sample Spiking Eluent prepared by using the above carbonate
139. AUPRE snopserey paappuon Haw g e yaa pagues susana ONINHUYV AA e 690 Toy Bunnseay woods 1 Ogg seg qu Gg Buydues TEA anag F 1 i IB A A T 1eCO des mas Wim asea did 6620 AH 97 PGR Bonet LLG OTO ORO Spey arg Dlr Tapu HRS 6914 1 qu sz STO O BONOS mejno upo qu OS EASA ANNAN SEa AL o eet H9829 pao Py unos 06 DO Lx GOES PRY pipop Mimssezog AMO TA SE MES a ot Cy EOE he Uapnjos MENG snougducyi qu 2 apoo Aanpuend RUI gran PRY IYI UP Jowan Y Suppeay ruq anope e s ojdwa pue PO Jayu AY JO YONBIYIPOO IPE ay sasn 219 2591 SHB agM JO JUSTOS uaBAXO Paaossip aya duna rap 404 FIL POD DOY POW OGAPPON LIM ISAL NUDAKO GAA TOSSIG eed bX ANGES ays Aq puecaap topes y 8 lg s 0191 UOYAs SOUT ONP SuLNp JABA p308 SN JO SUESROJOS SU PUE SSA MOL YAI SuuNp iow Jo oSeI0 S ayy Surjqeus POSLALO aq Avail mops WEIJS AJO APIO y syndur qiosqe 03 uays oy jo Appige DU sanpa ppa MoT penyen ayy en vogonpar y sasodind negan poe peigsnpu Bunama YSOWSSAL UONE LIL AQ SPUELIDP Od1AIS 01 SYONONHSUYOI WEP JO INSI E SE suBAMY Ag PesuRYO SI MOR eneu 94 BONO SIOQUO DPIS ASIJA PE IONPA OS PUL poysiojea TUpUNOUNS oq 1104 sIndUL QIosqB 0 WENS IYJ ayqeua ABUL MO jRinjeu ogg Sprejd pue spiune ap fo sjavasnbos mop oy Sunday Aq surs soos uo pedan Aeau mog ut sosuvys uy Spoo wo spos YOU TUSHANY noq 398 surejd poo
140. At atmospheric pressure and a temperature of 30 1 F the gas becomes an amber liquid about 1 5 times as heavy as water Chlorine available A measure of the total oxidizing power of chlorinated lime and hypochlorites Chlorination breakpoint Addition of chlorine to water or wastewater until the chlorine demand has been satisfied and further additions result in a residual that is directly proportional to the amount added beyond the breakpoint Chlorination free residual The application of chlorine or chlorine compounds to water or wastewater to produce a free available chlorine residual directly or through the destruction of ammonia or certain organic nitrogenous compounds Chlorine residual The amount of chlorine in all forms remaining in water after treatment to ensure disinfection for a period of time Coefficient of Variation An expression of standard deviation in terms as a percentage variance from the mean value The CV relates the Standard Deviation SD to the level at which the measurements are made CV SD X 100 Composite A sample made up of a collection of individual samples obtained at regular intervals Composite proportional A composite sample made up of sample whose volume is proportional to the flow at the time of collection 43 TB Laboratory QAP September 16 2009 Revision 1 Confidence Limits Or confidence interval refers to the upper and lower values of the range interval within which ra
141. Bases have a pH greater than 7 00 BOD Biochemical Oxygen Demand is a measure of the quantity of oxygen utilized in the biochemical oxidation of organic matter related to the oxygen requirements in chemical combustion being determined entirely by the availability of the material as a biological food and by the amount of oxygen utilized by the microorganisms during oxidation BOD is the initial quantity of oxygen used by polluted liquid immediately upon being introduced into water containing dissolved oxygen It may be exercised by end products of prior biochemical action or chemical substances avid for oxygen The BOD content is usually expressed in pounds per unit of time load of wastewater passing into a waste treatment system or to a body of water Biochemical Process The process by which the metabolic activities of bacteria and other microorganisms break down complex organic materials into simple more stable substances Biodegradation The destruction of mineralization of either natural or synthetic organic materials by the microorganisms populating soils natural bodies of water or wastewater treatment systems Carcinogen A material that either causes cancer to humans or animals Catalyst A substance that modifies slows or accelerates a chemical reaction without being consumed Cadmium Cd The main use of cadmium is in electroplating or galvanizing It is also used as a color pigment for paints and plastics and cathode ma
142. By McConnel Branch Prestons Cave Wolf Run Valley Park Vaughn s Branch Valley Park Cardinal Run Devonport Dr Wolf Run Wolf Run Park Vaughn s Branch Pine Meadow Park Vaughn s Branch Picadome Wolf Run Faircrest Dr Springs Branch Faircrest Drive Big Elm Tributary Harrodsburg Rd SW SW Wolf Run Lafayette Pkwy sw Duplicate sw Date Time Received By Date Time Temp Upon Receipt C ___ Measured By Containers Properly Preserved Yes No Headspace Yes No NA Bottles Intact Yes No COC Seals Intact Yes No NA Additional Documentation Attached Yes No Original COC To Laboratory Accompany Samples 8 Report COC Copy TRC Project File COC Copy TRC Laboratory Services Coordinator sje 04 11 11 THI o Macroinvertebrate Sample Chain of Custody AS AMAT Project Information Sheet Client Name _ _SEESSSS Project Administrator Project Number Due Date Sampling Site Location Stream Name County state O EcoRegion ________ Total Number of Samples Total Number of Containers _______ Reporting Requirements __ Laboratory Data Sheet __ Excel Spreadsheet __ MBI Calculations via __ e Submittal __ Hardcopy __ Both Samples Relinquished By Date Time Sample Received By Date Time Samples Relinquished By Date Time Sample Received By Date Time Comments Special Instructions of Qualitative or Collected Collection Ey Field Containers Sample Reference ID Quantitative
143. C dates if applicable will be noted on individual QA QC forms and maintained electronically in the Project File e Initials of the applicable party completing each task associated with sorting identification or quality control will be noted electronically in MacLIMS or on associated QA QC forms Wolf Run Watershed Page 55 of 67 Revision No 0 Based Plan Date April 11 2011 e QA checks will be documented on applicable forms and maintained in associated project files These forms include the Macroinvertebrate Sample Sorting Efficiency Form Macroinvertebrate Sample Taxonomy Precision Form and Macroinvertebrate Sample Taxonomic and Enumeration Efficiency Form B5 Quality Control Requirements B5 1 Field Quality Controls Field quality control checks for water chemistry will be collected at a frequency of one duplicate every sampling event Field duplicates must be randomly determined from the 12 sites and recorded on field datasheets or project logbooks The field controls shall be performed as follows A random number table see Appendix A will be used to select one sampling site such that all sample parameters are duplicated Two separate samples will be collected for each parameter The samples will be collected at the same time and at the same location One sample will be labeled as usual and the other sample will have the site name indicated as a duplicate On a form separate from the COC the site from which the duplicates
144. Calibrated By 8 d Enter Date 7 E Sample Name Date Samples Collected Time Analysis Started pH Standard Units Analyst Date Analysis Completed KPDES Permit Limits on Plant Effluent 6 0 mg L is the Lowest pH we can have on any given sample 9 0 mg L is the Highest pH we can have on any given sample Total Alkalinity Orion Research Incorporated Laboratory Products Group Log Number Sample Name Date Samples Collected Time Analysis Started Volume of Sample mL Dilution Factor D pH After Addition of Reagent Reading from Chart A Alkalinity Standard 10 0 1 0 Total Alkalinity A D mg L as CaCO Analyst Date Analysis Completed Presevation None required Analyze Immediately Total Hardness Sample Name Date Samples Collected Time Analysis Started Volume of Sample V mL Molarity of the Titrant M mL of Titrant Used A Total Hardness A mg L as Total Hardness as CaCO Analyst Date Analysis Completed 6 d TOTAL PHOSPHORUS ANALYSIS HACH TNT DR 5000 Date Time Sample Analysis Phosphorus Collected Started Conc in mg L as P i ES TB Raw Influent Duplicate EA LR E ft Return Activated Sludge 9 23154 SA S 23192 e 2 aa LR Le Analyst amp Calibrated By Date of Analysis Saturday January 00 1900 Interferences L
145. D bottle 2 Add 4 mL of BOD seed into each bottle 3 Siphon dilution water into BOD bottle until full 4 Read initial DO and record each sample on bench sheet 5 Replace lost volume of BOD bottle with dilution water until full and cap with stopper 6 Place plastic caps over BOD bottles to protect water seal 7 Rinse probe with lab water between samples 8 Incubate BOD bottles at 20 1 C for 5 days Check incubator temperature and adjust if needed For each incubator record in the daily logs both the date and daily temperatures and initial The daily logs are located next to BOD station 8 1 11 After 5 day incubation 1 Calibrate DO meter see SOP DO Section 8 2 Measure and record the 5 day DO values for each sample on the bench sheet and turn in for data entry see Section 11 Data Analysis and Calculations Helpful Hints 1 Samples that are caustic or acidic should be neutralized to pH 6 5 to 7 5 2 Samples containing residual chlorine should have chlorine removed by adding 10 drops of 10 Sodium sulfite Na2SO3 solution 3 For samples that are known to have high concentrations of solids make serial dilutions in 100 mL volumetric flasks using Nanopure laboratory water so as to yield a 40 to 60 DO uptake after 5 days QA QC Requirements 9 1 9 2 9 3 9 4 9 5 Calibrate DO meter at the beginning of each analysis day Recalibrate in the afternoon Run BOD Standard each batch 6 mL of 198 mg L GGA standard
146. Dissokred Oxygen O Sewage O Chemical Q Other OQ Flecks OQ Turbid O Other Odors QO Normal Q Chemical O Other Q Petoleum QO Sand a None Deposits O Shdze O Savrdust QO Paper fiber Q Relict shells O Other Looking at stones which are not deeply embedded are the undersides black m color QO Yes a Ho O Sewage O Anaerobic Oik O bsent Q Slight Moderate O Piofise ORGANIC SUBSTRATE COMPONENTS does not necessarily add up io 100 teristic Composition in Sampling Area nt iG om il oa Substrate Type Muck Mud Composition i Sampling Reac materials CPOM black very fine organic FPOM grey shell fragments HABITAT ASSESSMENT FIELD DATA SHEET HIGH GRADIENT STREAMS FRONT STREAM NAME LOCATION STREAM WDTH FT DEPTH FT PERENNIAL INTERMITTENT EPHEMERAL STATION RIVERMILE COUNTY STATE LAT LONG RIVER BASIN CLIENT PROJ ECT NO INVESTIGATORS CREW FORM COMPLETED BY DATE REASON FOR SURVEY TIME Habia Condition Category Parameter Optimal Suboptimal Marginal Poor 1 Epifaunal Greater than 70 of 40 70 mix of stable 20 40 mix of stable Less than 20 stable Substrate substrate favorable for habitat well suited for full habitat habitat availability habitat lack of habitat is Available Cover epifaunal colonization and fish cover mix of snags submerged logs undercut banks cobble or other stable habitat and at sta
147. F ALL QC RESULTS rra Total Solids amp Volatile Solids TOWN BRANCH amp WEST HICKMAN WASTEWATER TREATMENT PLANT Town Branch Laboratory 24 Hour Composite Samples Total Solids Method Residue Total EPA Method 160 3 Gravimetric Dried at 103 105 C Issued 1971 Total Volatile Solids Method Residue Volatile EPA Method 160 4 Gravimetric Ignition at 550 C Issued 1971 Enter Date ee 7 38 9 o u eee Log Number Sample Name Additional Name Notations Date Sample Collected Time Analysis Started Tare Number Tare amp Wet Sample W Tare W of Wet Sample Tare amp Dried Solids W Tare W gm gm W W gm gm gm Wt of Solids W W gm Total Solids CW W W W x 1 000 000 TS ppm Total Solids W WD W2 W x 100 TS Wt Tare amp Dried Solids W Wt Tare amp Ashed Solids W gm gm Wt Volatilized Solids W W gm Volatile Solids W W W gt W x 1 000 000 YS ppm Volatile Solids W3 WDWs Wp x100 YS Date Analyses Performed Analyst Setting Up Analysis Analyst Reading amp Calculating Analysis QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS ti a TOWN BRANCH amp WEST HICKMAN WASTEWATER TREATMENT PLANT Town Branch Laboratory Grab Samples Total Suspended Solids Method Residue Non Filterable EPA Method 160
148. LITTLE SANDY RIVER BASIN Little Sandy River at Grayson DO 0 0 ee ees O3216500 2 ee 44 Ohio River at Greenup Dam dd Bb Caste E ca RDA BIBI o 45 TYGARTS CREEK BASIN Fygaris Creek near Greenup Dc OBRITOOO o 53 KINNICONICK CREEK BASIN Kinniconick Creek at Tannery d 2 ee 03237250 0 54 LICKING RIVER BASIN Licking River near Salyersville d aaa eee DIARO aaa 5 Fox Creek Rock Lick Creck above Unnamed Tributary near Sharkey ooo 03250310 y a aa a a 56 Rock Lick Creek at State Highway 158 near Sharkey id 200 ee ee IBIS ca E 5 North Pork Licking River near Mt Olivet d 0 a a sl A South Fork Licking River Hinkston Creek near Carlisle lo O3282300 202 59 Licking River at Catawba Do 38253500 00 pu e a a A 68 Ohio River at Markland Dam d 00 a ee OIT 66 2k ae ee 61 KENTUCKY RIVER BASIN North Pork Kentucky River head of Kentucky River Leatherwood Creek at Daisy dd ee O3277408 2 A 62 North Fork Kentucky River at Jackson O O32800 ooo 63 Cutshin Crock at Wooton l OS28O700 2 aaa A 54 Middle Fork Kentucky River at Tallega d et OS281000 on oe eee ee ees 65 Kentucky River Red Bird River head of South Fork Kentucky River near Big Creek OREA aaa 55 Goose Creek at Manchester d alaaa ee OSZBHOO we 67 South Fork Kentucky River at Booneville Fo oo ee OF28150G od G Kentucky River at lock 14 at Heidelberg De OB2B2000 oo 9 Sturgeon Creek at Cressmomt 0 a a ee 03282040 ts nl cda Re dine 7 Red
149. MS4 indicates that sampling is scheduled but under the MS4 permit and not this project Revision No 0 Date April 11 2011 Wolf Run Watershed Based Plan Page 31 of 67 For the conductivity survey and watershed habitat assessments the watershed has been divided into twenty four stream segments as shown in Exhibit 3 and summarized in Table 9 TABLE 9 HABITAT ASSESSMENT STREAM SEGMENTS Stream Segment Mouth to Old Frankfort Pike Old Frankfort Pike to New Circle Rd New Circle Rd to Cambridge Dr Cambridge Dr to Versailles Rd Versailles Rd to Appomattox Rd Appomattox Rd to Faircrest Dr Faircrest Dr to Lafayette Pkwy Lafayette Pkwy to railroad tracks north of Southland Dr Railroad tracks to Nicholasville Rd Segment ID Wolf Run Wolf Run Wolf Run Wolf Run Wolf Run Wolf Run Wolf Run Wolf Run Wolf Run McConnell Branch Wolf Run to Preston s Cave Spring McConnell Branch McConnell Springs Branch through Stormwater Structure Vaughn s Branch Vaughn s Branch Wolf Run to Oxford Circle Oxford Circle to Versailles Rd Vaughn s Branch Versailles Rd to Summerville Rd Golf Course Fence Vaughn s Branch Picadome Golf Course Vaughn s Branch Vaughn s Branch Picadome Golf Course Fence to Gibson Ave Culvert Simpson Ave to railroad tracks Big Elm Tributary Sinkhole on Picadome Golf Course to Harrodsburg Rd Big Elm Tributary Harrodsburg Rd to r
150. Measurements and Meter Calibration Standard Operating Procedure Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky DOWSOP03014 KDOW 2009b Laboratory Procedures for Macroinvertebrate Processing and Taxonomic Identification and Reporting Kentucky Department of Environmental Protection Wolf Run Watershed Page 63 of 67 Revision No 0 Based Plan Date April 11 2011 KDOW 2009c Methods for Sampling Benthic Macroinvertebrate Communities in Wadeable Waters Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky KDOW 2010a 2010 Integrated Report to Congress on the Condition of Water Resources in Kentucky Volume II 303 d List of Surface Waters Kentucky Energy and Environment Cabinet Division Frankfort Kentucky KDOW 2010b Measuring Stream Discharge Standard Operating Procedure Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky DOWSOP03019 KDOW 2011 Sampling the Surface Water Quality in Lotic Systems Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky DOWSOP03015 KDOW Watershed Watch Water Chemistry Sampling Methods for Field Chemistry and Lab Analysis http www lrww org training chem test pdf Kentucky Waterways Alliance and the Kentucky Division of Water 2010 Watershed Planning Guidebook for Kentucky Communities 1st ed Kentucky Waterways Alliance and the Kentucky Divi
151. OP WH TP West Hickman WWTP Laboratory Page 27 of 219 Revision Number 5 Last Revised 09 09 Helpful Hints 1 Analysis results are directly proportional to sample volumes therefore it is very important that accurate sample volume measurements are made 2 The Total and Acid Hydrolyzable Test Vials are cuvettes to be analyzed spectrophotometrically and must provide a clear optical path Prior to reading clean the vials by wiping them down a Kim Wipe moistened with lab water and then wipe them with a dry Kim Wipe 3 When washing lab ware involved with this method use only phosphate free cleaning agents 1 1 HCL solution is recommended followed by thorough Nanopure lab water rinse Note Most of the lab ware used in this method is disposable QA QC Requirements 9 1 A Reagent Blank High Standard 1 0 mg L and a Low Standard 0 2 mg L must be run with every analytical run 9 2 A total of 5 of all samples must be run in duplicate 9 3 Data acceptance criteria 9 3 1 Analysis values for Standards must agree within 10 of the Standards known value or 0 12 mg L whichever is largest 9 3 2 Duplicate values must agree within 5 If these criteria are not met corrective action is indicated See Quality Assurance Program QAP Sec 15 Corrective Action Policies and Procedures Expected Results 10 1 KPDES Permit Requirements 1 West Hickman Wastewater Treatment Plant effluent limitations are a November 1 through April 30
152. P Sec 15 Corrective Action Policies and Procedures 25 10 11 12 SOP Residual Chlorine LFUCG Laboratory Page 26 of 219 Revision Number 4 Last Revised 09 09 Expected Results 10 1 KPDES Permit Requirements 10 2 KPDES Permit Limits on plant effluent residual chlorine at Town Branch WWTP is a maximum monthly average of 0 010 mg L with a daily maximum limitation of 0 019 mg L In the event that analysis results indicate values greater then KPDES permit requirements retest If the value indicated by the retest is greater than KPDES permit requirements Immediately notify the Plant Superintendent and Laboratory Supervisor Process Ranges Expected residual chlorine results on plant effluent samples will be less than 0 010 mg L typically the results are BDL below detection limit Data Analysis and Calculations 11 1 11 2 Concentration values are read directly from the AutoCAT unit s display all calculations are preformed internally The Laboratory Supervisor will determine if the results for the standard are within the expected range Bibliography 12 1 12 2 12 3 U S EPA Method 330 3 Chlorine Total Residual Titrimetric Amperometric Issued 1978 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 Standard Methods 4500 Cl D Chlorine Residual Amperometric Titration Method
153. PD value X X RPD 2e x 100 AX where X X2 means the absolute difference between X and X gt 7 Method Performance The method detection limit MDL should be established by determining seven replicates that are 2 to 5 times the instrument detection limit The MDL is defined as the minimum concentration that can be measured and reported with 99 confidence that the analyte concentration is greater than zero and is determined from analysis of a sample in a given matrix containing the analyte MDL Legit ce 99 S where t the t statistic for n number of replicates used for n 7 t 3 143 n number of replicates S standard deviation of replicates 8 Reference EPA SW 846 9056 Chapter 5 September 1994 U S EPA Method 300 0 March 1984 ASTM vol 11 01 1996 D 4327 Standard Test Method for Anions in Water by Chemically Suppressed Ion Chromatography 0 2010 addendum to 01 2009 Ion Chromatography of Water 1 Discussion Principle and iodine 3 Reagents Calibration Standards 1 Calibration Standard 1 Pipette 0 1 mL of 1000 mg L I stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume 2 Calibration Standard 2 Pipette 0 5 mL of 1000 mg L I stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume 3 Calibration Standard 3 Pipette 1 0 mL of 1000 mg L I stock standard into a 1000 mL volumetric flask
154. Pre weighed filters for TSS F92447MM 6 4 Oven 103 C to 105 C 6 5 Beakers stirrer tongs 6 6 Vacuum pump and vacuum flask 500 mL 6 7 Graduated cylinders 6 8 Desiccators Interferences del Too much residue on the filter will entrap water and may require prolonged drying 7 2 Too much residue on the filter may stop the movement of water through the filter Procedures 8 1 Steps 1 Calibrate balance using ASTM Class 1 weight set Typically 200 g 100 g 500 mg and 100 mg 2 Environmental Express filters are pre weighed An ID number and weight of filter are shown on the aluminum pan Record the ID number and the filter weight This is W1 3 Assemble the filtering apparatus with pre weighed filter and apply vacuum 4 Rinse filter with Nanopure water 5 Mix sample 6 Using a graduated cylinder measure the required sample volume V then gently and slowly pour into filter Rinse side of filter unit with Nanopure water 7 Placed filter and residue back in the original aluminum pan 8 Dry in oven 103 C to 105 C until constant weight is achieved 9 Allow pans to cool in desiccator for 20 minutes before weighing 82 8 2 10 11 SOP TSS LFUCG Laboratory Page 83 of 219 Revision Number 3 Last Revised 09 09 10 Weight of filter and residue is W2 11 EPA requires filters to be placed back in the oven an reweighed three times Helpful Hints 1 Drying filters overnight produces the best results
155. Q No evidence O Some potential sources RIPARIAN VEGETATION 12 meter buffer INSTREAM FEATURES AQUATIC VEGETATION WATER QUALITY SEDIMENT SUBSTRATE INORGANIC SUBSTRATE COMPONENTS should add up 100 O oulder f gt 256 mm 10 64 256 mm 2 5 10 2 64 mm 0 1 2 5 Sub Type drock Cobble Gravel Sand Silt Clay 0 06 2n0n gritty 0 004 0 06 mm 0 004 mm slick Q Field Pasture QO Ob vious sources O Agricultural O Residential Local Watershed Erosion QNone OModente O Heavy Indicat the dominant type and record the dominant species present O Trees O Shrubs O Grasses O Herbaceous dominant species present Estimated Stream Width m High Water Mark Proportion of Reach Represented hy Stream Moxp halozy Types OR R ORun Q Pool m Estimated Stream Depth Surface Velocity at thalweg Estimated Reach Length m Channelized OQ Yes a No Dam Present O Yes a No Canopy Cover a Partly open QO Partly shaded QO Shaded Indicat the dominant type and record the dominant species present QO Rooted emergent QO Rooted submergent QO Rooted floating Q Free Floating Q Floating Algae O Attached Algae dominant species present Portion of the reach with aquatic vegetation Water Odors QO Normal None QO Petoleum Q Fishy Water Surface Oik Q Slick OQShken OGlobs QNone OOther Turbidity Gf not meas ured Q Clear ienei O Opaque O Stamed Temperature C Specific Conductance
156. QAP and all standard operation procedures SOPs including analytical procedures and sample preparation procedures QAP Documentation Control Procedures 4 2 1 4 2 2 4 2 3 4 2 4 Each page of the QAP includes the title revision number effective date and page number Copies of previous versions of the QAP are archived and kept by laboratory management and are subject to the record keeping requirements in Section 14 When minor revisions are made to a section of the QAP the updated section is added to the QAP and the previous version is removed and archived for a minimum of five years Archived information shall be available to regulatory agencies SOP Documentation Control Procedures 4 3 1 4 3 2 4 3 3 4 3 4 4 3 5 All SOPs are assigned a unique name or code Each SOP document contains a revision number Each page of a SOP includes its unique name or code revision number effective date and current page number of total pages in section Copies of previous versions of SOPs are archived and kept by laboratory management for a minimum of five years These are subject to the record keeping requirements in Section 14 SOPs are available to laboratory personnel as part of a comprehensive lab manual New SOPs are added to the lab manual as they are issued When SOPs are revised the revision is added to the lab manual and the previous version is removed and archived Likewise any procedure no longer in effect
157. Quality Assurance Project Plan Wolf Run Watershed Based Plan EPA 319 h Grant No C9994861 09 Prepared By Third Rock Consultants LLC 2526 Regency Road Suite 180 Lexington KY 40503 859 977 2000 Prepared For Lexington Fayette Urban County Government Department of Environmental Protection 200 East Main Street Lexington KY 40507 859 425 2800 and Kentucky Department for Environmental Protection Division of Water 200 Fair Oaks Lane Frankfort KY 40601 502 564 3410 Date April 11 2011 Revision Date Revision No 0 This Page Intentionally Blank SECTION A PROJECT MANAGEMENT A1 Title and Approval Sheet Quality Assurance Project Plan for Wolf Run Watershed Based Plan PAE de fo oe Steve Evans QAPP Author and Project Quality Assurance Officer Third Rock Consultants LLC April 12 2011 Susan Bush Project Manager Lexington Fayette Urban County Government Date David Price Laboratory Manager Lexington Fayette Urban County Government Date Ken Cooke Volunteer Coordinator Friends of Wolf Run Brook Shireman Project Manager Kentucky Division of Water Date Date Lisa A Hicks Quality Assurance Officer Kentucky Division of Water Date Date Wolf Run Watershed Page 3 of 67 Based Plan Revision No 0 Date April 12 2011 This Page Intentionally Blank Wolf Run Watershed Page 4 of 67 Revision No 0 Based Plan Date April 12 2011
158. R BASIN Tennessee River at Hwy 60 near Paducah Ky d0 ee 0360907960 0 203 Clarks River at Almo d o o aaaea ee DIGIO ee 210 MASSAT CREEK BASIN Massac Cek near Paducah Ld 0 ee OIGH260 2 oa awe a 21i Ohio River at Metropolis IL 8 es PIEL o 212 BAYOU CREEK BASIN Bayou Creek Bayou Creek neas Heath 8 0 QIGLLBOO aoaaa 213 Bayou Creek near Grakamville d o o aaar O3GH8SO aaa aaa 214 Little Bayou Creek near Geahamville d a METI 2 a a 215 Ohio River at lock and dam 53 near Grand Chain IL 0 0 o aaa 09612500 l a aaaea 216 LOWER MISSISSIPPI RIVER BASIN BAYOU DE CHIEN BASIN Bayou De Chien near Clinton ds OTO24000 6 oe Bee he es 223 Dissolved j E m t 4 E A A E A oy g t a o OC 4 r et gt z s i nto Ys AA o 7 i D aS AS a o o PR ES l SY Po INTRODUCTION Aquatic animals need dissolved oxygen to live Fish invertebrates plants and aerobic bacteria all require oxygen for respiration Oxygen dissolves readily into water from the atmosphere until the water is saturated Once dissolved in the water the oxygen diffuses very slowly and distribution depends on the movement of the aerated water Oxygen is also produced by aquatic plants algae and phytoplankton as a by product of photosynthesis The amount of oxygen required varies according to species and stage of life Dissolved Oxygen levels below 3 ppm are stressful to most aquatic organisms Dissolved Oxygen levels below 2 or 1 ppm will not
159. RE PUBLISHED IN THIS VOLUME Continued Letters after station name designate type of data d discharge g stage c chemical b biological t water temperature s sediment Page STATION NUMBER OHIO RIVER BASIN Continued Ohio River Continued GREEN RIVER BASIN Continued Green River at lock 2 at Calhoun 0 es E Boh lies DARRO ooo 149 Fond River near Ape G4320S00 a ee ee 150 WABASH RIVER BASIN Wabash River at New Harmony IN e aa es O3378S0G a a pl TD 152 TRADEWATER RIVER BASEN Tradewater River at Olney BD e DIIBIDON re oe A 159 CUMBERLAND RIVER BASIN Martins Fork Lake at Martins Fork Dam near Smith de o WBAI7OB Le 160 Martins Fork near mika OF400800 oo 183 Cumberland River near Harlan d aaa D34000 o 190 Yellow Creek near Middlesboro De M4G2000 ee 191 Cumberland River at Pine St Bridge at Pineville KY GD ooo o ems RADI o 192 Cumberland River at Barbourville oo 03403500 0 0 93 Clear Pork at Santon De DIAOBP O oo 194 Cumberland River at Williamsburg dh OR4OG00G oo 195 Laurel River Lynn Camp Crock at Corbin d 0 OOW 2 aaa 196 Rockeasth River at Bilows d aaa aa H4400 aaa aaa 197 South Fork Cumberland River near Stearns Gi ee G34105000 ee 138 Beaver Creek near Monticello ee 03413200 aaa a 199 Little River near Cadiz ie O3438KK o BOD Barkley Keatucky Canal near Grand Rivers 8 O343R190 ee 201 Cumberland River near Grand Rivers ooa aa 03838220 202 TENNESSEE RIVE
160. River near Hazel Green ee en 03282300 o 74 Red River at Clay City id l o aa aaa ee o aa 7 Kentucky River at Jock 10 near Winchester ld ee PIRA ar e a 73 Dix River near Danville do RISOO aaa 4 Clarks Run near Danvile 3 OB 28S 200 eh anno 75 Kentucky River at tock 7 near High Badge ld oo aaa O328A500 o aaa 76 Kentucky River at lock 6 near Salvisa Do 03287000 o 77 Kentucky River at lock 4 at Frankfort 0 ee OB287500 2 aa aaa aaa FR Elkhorn Creek North Efkhorn Creek near Georgetown a a 03288000 el 79 North Elkhorn Creek at Georgetown UD OIBBBIOO naaa 80 Royal Spring at Georgetown Do oae DIRBU rei 81 South Etkhorn Creek near Midway dd O32RG300 aaa 82 Elkhorn Creek near Frankfon ds O3289500 ooo 83 Kentucky River at lock 2 at Lockport id ooo 03299500 aaa aa BA Bagle Creek at Glencoe d 0an aaa e le 85 HARRODS CREEK BASIN Harrods Creek near Prospect ce 0 Ta ad hc a NI eT ate RA IMA o 86 Viti SURFACE WATER STATIONS IN DOWNSTREAM ORDER FOR WHICH RECORDS ARE PUBLISHED IN THIS VOLUME Continued Letters after station pame a type of data d discharge Ug stage o chemical ib biological 0 water temperature s sediment Page STATION NUMBER OHIO RIVER BASIN Continued Ohio River Continucd GOOSE CREEK BASIN Goose Creek ut Old Westport Road rear St Matthews de C ooo oo O8292474 a aie a a EN 8 Goose Creek at US Hwy 42 near Glenview Acres fo e e dc eeo e aeh 9
161. SOLVED OXYGEN FACT SHEET Oxygen is critical to the survival of aquatic plants and animals and a shortage of dissolved oxygen is not only a sign of pollution it is harmful to fish Some aquatic species are more sensitive to oxygen depletion than others but some general guidelines to consider when analyzing test results are 5 6 ppm Sufficient for most species lt 3 ppm Stressful to most aquatic species lt 2 ppm Fatal to most species Because of its importance to the fish s survival aquaculturists or fish farmers and aquarists use the dissolved oxygen test as a primary indicator of their system s ability to support healthy fish WHERE DOES THE OXYGEN COME FROM The oxygen found in water comes from many sources but the largest source is oxygen absorbed from the atmosphere Wave action and splashing allows more oxygen to be absorbed into the water A second major source of oxygen is aquatic plants including algae during photosynthesis plants remove carbon dioxide from the water and replace it with oxygen Absorption Oxygen is continuously moving between the water and surrounding air The direction and speed of this movement is dependent upon the amount of contact between the air and water A tumbling mountain stream or windswept wave covered lake where more of the water s surface is exposed to the air will absorb more oxygen from the atmosphere than a calm smooth body of water This is the idea behind aerators by creating b
162. STEM2 TKN TKN Methods including Total Nitrogen using AG4A AG4A and AS4A columns Weigh out 0 191 g of sodium carbonate Na CO3 and 0 143 g of sodium bicarbonate NaHCO and dissolve in water Bring the volume up to 1000 ml and place in the System 2 bottle labeled JC TKN 0 191 0 143 Sparge the eluent as in the above reagent for System 2 100X Sample Spiking Eluent prepared by using the above carbonate bicarbonate ratios but increasing the concentration 100X Weigh out 1 91 g of NaCO and 2 86 g of NaHCO into a 100 mL volumetric flask 0 05 mL of this solution is added to 5 mL of all samples and standards to resolve the water dip associated with the fluoride peak Stock standard solutions 1000 mg L 1 mg mL Stock standard solutions may be purchased SPEX as certified solutions or prepared from ACS reagent grade materials dried at 105 C for 30 minutes Calibration Standards for the SYSTEM2 NITRATE except Bromide methods are prepared as follows 1 Calibration Standard 1 Pipette 0 1 mL of 1000 mg L NaNO stock standard 0 1 mL of 1000 mg L NaF stock standard 2 mL of 1000 mg L NaCl stock standard and 10 mL of 1000 mg L K SO stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume 2 Calibration Standard 2 Pipette 0 5 mL of 1000 mg L NaNO stock standard 0 5 mL of 1000 mg L NaF stock standard 5 ml of 1000 mg L NaCl stock standard and 20 mL of 1000 mg L K SO stock standard in
163. Samples Settled Sludge Time SST min 25 minutes mL L Settled Sludge Volume SSV mL L Settled Sludge Concentration SSC SSC 1000 x ATC SSV 0 0 DIV 0 DIV 0 DIV 0 DIV 0 DIV 0 SSVt mL L 0 5 10 15 20 25 30 40 50 Time min Settled Sludge Volume Curve A Settled Sludge Concentration Curve 30 minutes mL L 4 Hours mL L DIV 0 DIV 0 DIV 0 DIV 0 DIV 0 DIV 0 Power Settled Sludge Concentration Curve Power Settled Sludge Volume Curve Date Analysis Completed Centrifuge Spin Test Sludge Volume after 15 minute Centrifuge Spin mL Enter Date Activated Sludge Settled Volume Method Method 2510 C Settled Volume WEF Standard Methods 21 Edition Activated Sludge Zone Settling Rate Method Method 2710 E Zone Settling Rate WEF Standard Methods 21 Edition Sludge Volume Index Method Method 2710D Sludge Volume Index WEF Standard Methods 21 Edition Sludge Density Index Method Method 2710D Sludge Density Index WEF Standard Methods 21 Edition Centrifuge Spin Test Centrifuge Method for Estimating Suspended Matter WEF Simplified Laboratory Procedures for Wastewater Examination 3rd Edition 1985 Pg 30 QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS 9T U Average Mixed Liquor Total Suspended Solids eration Tank Mixed Liquor Concentration ATC i nalyst a
164. Spike Duplicate Recovery outside acceptance limits Acceptable results if associated Laboratory Control Sample is acceptable No qualifier Indicates matrix is adversely affecting the extraction or digestion of the analyte If the Matrix Spike recovery is below acceptable limits it may be likely that the reported results for the associated samples may be underestimated Conversely if the Matrix Spike results are high it may be likely that the reported results for the associated samples may be overestimated Laboratory Control Sample outside acceptance limits Reject results Indicates that the laboratory system is out of control Sample received exceeding proper temperature or preservation criteria Reject results Indicates preservatives or temperature requirements have not been met and the bias on the sample result is unknown The analyte was analyzed for but not detected Accept results Indicates that the result is less than the reporting limit Analyte exceeded calibration range Accept results Only reported in instances in which the calibration curve is exceeded and the sample cannot be reanalyzed Replicate Duplicate precision outside of acceptance limits Reject results unless it occurs on a matrix spike duplicate Indicates the precision is outside of normal acceptance criteria due to a lack of homogeneity or other factor Calibration criteria exceeded Reject results Indicates that th
165. Sterile blue sheets 6 17 Indicator tape 6 18 Autoclavable Nalgene squeeze bottles for peptone Interferences 7 1 Bacteria from the surrounding environment 7 2 Cross contamination from one sample to the next 7 3 Lack of aseptic techniques 18 Procedures 8 1 Steps 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 SOP WH Fecal Coliforms West Hickman WWTP Laboratory Page 19 of 219 Revision Number 4 Last Revised 09 09 Clean work area with Lysol disinfectant 20 solution Light Bunsen burner with striker Open sterile filter holder Use sterile blue sheet as a sterile field Indicator trip and tape should indicate that the filter has been sterilized Flame forceps and use it to remove the Indicator Strip without touching anything else except the strip Use Petri dishes with sterile pad already in dish Break open ampule of media and pour onto media pad Decant excess media and cover dish to protect sterile pad Place the bottom of the sterile filter holder onto the vacuum flask Flame forceps remove sterilized filter from packaging and place onto sterilized filter holder grid side up Do not touch the filter with anything except the forceps Place or clamp the top unit onto filter holder Gently mix sample In advance determine sample volume that will yield 20 60 fecal coliform units FCU If the volume of sample to be used is 0 1 to 5 mL pour approximately 10 mL of pe
166. Total as P mg L PO P EPA 365 2 Ammonia as N mg L NH3 N EPA 350 1 Nitrate as N mg L NO3 N EPA 300 0 Nitrite as N mg L NO N SM 4500 NO B Total Kjeldahl Nitrogen as N mg L TKN N SM 4500 Norg C Indicates minimum laboratory precision for all parameters except in situ measurements For in situ this indicates field precision For hydrogeomorphic sampling the surveying precision of cross sections and profiles shall be 0 01 ft for vertical readings and 0 1 ft for horizontal readings The laser level precision shall be less than 3 0 mm 30m Precision for pebble count readings will be such that each data point measures within 1 unit of the narrative particle description or 0 5 phi units on the gravelometer A7 2 2 Accuracy Accuracy is a measure of overall agreement between a measurement and a known value Accuracy includes an evaluation of bias which is a systematic or persistent distortion of a measurement process that causes errors in one direction Accuracy is quantified by calculating the percent recovery YR of a known quantity of an analyte under a particular test method as follows R V x100 V where Vm Vi measured value determined by analysis true value as calculated or certified by a manufacturer No water quality field samples will be collected in order to evaluate accuracy However internal laboratory QC samples will be analyze
167. Under sample type click on either Calibration Standard or Sample depending on what is being run e Under the Method section the method name must be entered To do so double click on the highlighted area under Method scroll through the list of methods and double click on the method of interest f Next under the Data File section enter the name of the data file g Finally in the Dil area type in the dilution factor if different from 1 Do this for all standards blanks quality controls duplicates and samples to be run under this schedule h Save the schedule and obtain a printout of it i Standardize the Dionex Ion Chromatography System by running the standards Standard 1 Standard 2 and Standard 3 Run the QC standards Run the prepblank and DI water blank Run the samples duplicates and blanks Run the QC standards at the end 5 Calculations A Calculations are based upon the ratio of the peak area and concentration of standards to the peak area for the unknown Peaks at the same or approximately the same retention times are compared Once the method has been updated with the current calibration this is calculated automatically by the software using linear regression Remember that when dilutions are being run the correct dilution factor must be entered B Manual calculations are based upon the ratio of the peak and concentration of standards to the peak area for the unknown when the software will not automatical
168. Use the same criteria as for grab samples starting at the end of compositing Samples should be at 4 C At no time should an analyst test a 24 hour composite sample after the 48 hour holding period Reagents 5 1 Sodium Sulfite solution 0 025 N Instill 0 1575 g 0 0001 g Sodium sulfite into 100 mL volumetric flask and bring to mark with Nanopure lab water Note This solution is not stable prepare daily 5 2 HACH BOD Nutrient Buffer Pillows 3 L and 6 L 5 3 BOD Seed Inoculum Polyseed 5 4 NCL Glucose Glutamic Acid BOD Standard 198 30 5 mg L 5 5 HACH Nitrification Inhibitor with dispenser cap 5 6 Nanopure laboratory water Equipment amp Lab Ware 6 1 300 mL disposable BOD bottles Environmental Express 6 2 BOD bottle stoppers and plastic caps 6 3 HACH HQ40d Portable Meter with LBOD101 probe 6 4 Control Co Digital Barometer 6 5 Fisher Scientific Isotemp Incubator Model 304 at 20 C 1 C 6 6 9L glass dilution water bottle 6 7 Siphon hose silver treated blue hose and valve 6 8 Graduated cylinders to measure samples 250 and 500 mL 6 9 Squeeze bottle for dispensing dilution water 6 10 Squeeze bottle with lab water to rinse probe between initial DO readings 6 11 500 mL and 1 L Erlenmeyer flasks 6 12 10 mL and 500 mL beakers 6 13 Barant Co vacuum pressure aeration system with hose and diffuser 6 14 Labsystems adjustable 1 5 mL finnpipette Interferences 7 1 Greases and oils in the sample 7 2
169. a yong jo sdoap q ppe 1420 did aya Bas q dag Us panguaos aq pa g dag u unag YONI M1 se Jund JOT p Sp Ox WUE JNS Sy dea pur sayan sy MACU Y E MOTOS DUIE AISA e 01 PNP 40 02 UAOIQARO R ap pun PATI o Jaun aya ssead djmaza aqa ap Zupeys Apu ayy GRD aqm uopean syl JO BOY 190100 34 GRY 4010101 ayp asu menusu BONE Sys LE paquasap MUUTU Su Ol 6914 BORNHOS mayson y AUTOS yna LEO AICM Bujpery 1004 241 ig 2 Y dng 12 UTI ayu 10303 pue tq das unopod z dag dois ooi nue AIA e Apeoxe MBS pax ALP JO 30105 943 LON C9qU ay dun pue jies ayy UAL 204 JU QT ap o 6670 HANA BOE aya id l HNPIIGI YZ 359 L O DESO LETITIA ENESCO LEAT IRANEN DNASE aon te pauuopiad aq 01 s 2INpadosd 3903 Mya BRE AUGIWioge 10 vopn Buns B 01 ALY Pava uays pur pray ap ul pa pue paiayo gt sq uta soydures quazass PUJ AGOMPSuna aanpadold 153 jeme IYI URO 01 JessaD3U JOU 3 GUUBI SILA up paxy UBaq sey ajdwes aya IU HNS 1993 BUI Pe you flan s4aycsoun sq pue ajdwes 1918 aya 129 09 po to dass jo uouadmo 34 Burmeog oydwes 34 Jo TUBJUOS usB AXO 343 UO Surpusdep dopasp yA 3003 aBUBs0 UMQIG GI MO R ALA Y PMOs sip savy munidad sya put 3ua3eda aun UH XH OF BABYS pu pue anog aya des amog Zugdwues ay 01 0979 19Pr007 pp DIUIBANS jo amsent jasa uo ppe 2690 upods fuunseow Y 1 ay Juen 9 Buyposacid 230 0q 9pNOg aya JO JOpmays ap mojag Is 0 aedinaid ays mony uno Ba ngidang Vy
170. a collection efforts in the watershed to produce the loading calculations for Chapter 4 of the Wolf Run Watershed Based Plan The methods to be utilized in performing these tasks are listed in the sections below B2 2 6 1 Flow Measurement The procedure for flow measurement is explained in B2 2 1 Flow measurements will be conducted according to the KDOW s Measuring Stream Discharge Standard Operating Procedure KDOW 2010b Velocity and flow area measurements must manually be recorded in a bound field book or on other appropriate field data sheets using indelible waterproof ink and waterproof paper Discharge values will be calculated in the office according to the equations specified in KDOW 2010b One duplicate measurement will be recorded per sampling event Wolf Run Watershed Page 51 of 67 Revision No 0 Based Plan Date April 11 2011 B2 2 6 2 Grab Sampling Grab sampling will be conducted according to the Kentucky Division of Water s Sampling the Surface Water Quality in Lotic Systems KDOW 2011 The methods specific to this collection effort are described below One field duplicate sample will be collected for all parameters per sampling event Samplers should put on powderless latex or nitrile gloves prior to sampling Grab samples should be collected in the centroid of flow in a section of stream in which indicators of complete mixing are evident The sampler should face upstream and approach the site from downstream ens
171. a monthly average of 1 mg L and a weekly average of 2 mg L b May 1 through October 31 there are no effluent limitations on Total Phosphorus Plant effluent composite samples are analyzed daily Monthly and weekly averages are reported In the event that analysis results indicate values greater than the KPDES permit requirements retest If the value indicated by the retest is greater than KPDES 27 11 12 10 2 SOP WH TP West Hickman WWTP Laboratory Page 28 of 219 Revision Number 5 Last Revised 09 09 permit requirements Immediately notify the Plant Superintendent and the Laboratory Supervisor Process Ranges Typical phosphorus concentration values for plant influent vary primarily due to rainfall Within the treatment process phosphorus concentrations can vary due to microbiological processes involving the release and uptake of phosphorus forms Typical values for each plant are West Hickman Influent 2 mg L to 12 mg L West Hickman Effluent lt 1 0 mg L Data Analysis and Calculations 11 1 Concentration values are read directly from the DR 4000 spectrophotometer Bibliography 12 1 HACH DR 4000 Procedure Manual EPA approved Method 8190 Phosphorus Total HACH Company Loveland CO 12 2 Standard Methods Part 4500 P Phosphorous APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control
172. able substrate frequently disturbed or removed Poor lt 20 stable habitat lack of habitat is obvious substrate unstable or lacking Parameter 2 Embeddedness Embeddedness describes the extent to which rocks and snags are covered or sunken into the silt sand mud or biofilms algal fungal or bacterial mats of the stream bottom Generally as rocks become embedded the surface area available to macroinvertebrates and fish for shelter spawning and egg incubation is decreased assess in the upstream or central portions of riffles Optimal Rocks are 0 25 surrounded by fine sediment Layering of cobble provides diversity of niche space Suboptimal Rocks are 25 50 surrounded by fine sediment Marginal Rocks are 50 75 surrounded by fine sediment Poor Rocks are gt 75 surrounded by fine sediment Parameter 3 Velocity Depth Regime The best streams in most high gradient regions will have all of the following patterns of velocity and depth 1 slow deep 2 slow shallow 3 fast deep and 4 fast shallow the occurrence of these four patterns relates to the stream s ability to provide and maintain a stable aquatic environment Investigators may have to scale deep and shallow depending upon the stream size a general guideline is 0 5 m between shallow and deep Optimal All 4 regimes present Suboptimal Only 3 of the 4 regimes present if fast shallow is missing score lower than if missing other regimes Marginal On
173. ach 1 0 megOhm cm at 25 C 12 TB Laboratory QAP September 16 2009 Revision 1 7 1 7 2 7 3 Section 7 Verification Practices Performance Evaluation PE Testing 7 1 1 7 1 2 Samples are analyzed for this laboratory facility as appropriate for the mandatory USEPA DMR QA Laboratory Performance Evaluation Study PE samples are analyzed once per year where appropriate samples are available for each test method each matrix and each analyte included in its scope of accreditation as required by the provisions in the DMRQA Announcement Letter 308 Letter as well as the requirements detailed in the U S EPA National Standards for Water Proficiency Testing Studies Criteria Document December 30 1998 PE samples are processed without any extraordinary care as the results obtained will be considered typical of the laboratory s performance PE samples are treated as unknown samples according to guidelines described in Section 11 All directions are followed without changing sample preparation dilution or analysis The laboratory s personnel do not engage in inter laboratory communications regarding PE sample results or attempt to obtain the true values of the PE samples prior to reporting at the designated deadline for the PE Study All unacceptable results for PE samples are investigated by a standardized procedure Appropriate corrective actions are implemented where assignable error was found When assignable err
174. acteria e Sample Preservation f Chemical Treatment Transport of Samples to the Laboratory a Documenting changes in custody of the sample b Drop Off Centers C Runners Laboratory Analysis Data Management Quality Control and Assurance a How Watershed Watch Assures the Quality of Its Data b Duplicate Samples and Field Blanks 1 Introduction This document describes standard operating procedures of Watershed Watch in Kentucky for deriving reliable data about water quality samples obtained from streams for laboratory analysis by its Volunteer Monitor participants This section of the document will provide background on the program explain its organization and introduce its sampling programs a Background Watershed Watch in Kentucky Watershed Watch in Kentucky educates citizens in watershed and stream science and trains them to gather scientific data about streams Watershed Watch has these statewide program objectives e Provide citizens with an array of scientific data and an understanding of stream science that helps them better appreciate the quality status of a stream for which they are concerned e Create an annual synopsis of the overall quality of surface waters on a state and basin basis and e Involve citizens who are knowledgeable about water quality in watershed planning protection and restoration activities b Overview Watershed Watch s Synoptic Sampling Program A major purpose of the Synoptic Asses
175. ailroad tracks via Bob O Link Dr Big Elm Tributary Nicholasville Rd to behind Central Baptist Hospital Cardinal Run Wolf Run to Versailles Rd Cardinal Run Versailles Rd to End of Chinquapin Ln Upstream of Parkers Mill Rd Wolf Run under Alexandria Dr and Old Frankfort Pike to pond Gardenside Tributary Unnamed Tributary B1 2 Sampling Design Rationale B1 2 1 Karst Hydrograph Characterization The Wolf Run watershed has significant karst development which must be considered during loading calculations because it can influence the decision making process during development of the action plan In particular local karst deviation from surface watershed boundaries adds drainage area to Wolf Run Based on dye traces a substantial fraction of both the Vaughn s Branch and main stem of Wolf Run sub watersheds are captured by the Prestons McConnell Spring Basin Recker and Meiman 1990 and Spangler 1992 During base flow and drier conditions most of the surface water in the karst influenced fractions of these sub watersheds is directed to Prestons Spring During high flow conditions the surface component of the discharge becomes greater as the karst system conduit limits are approached To determine the influence of the karst system storm event and base flow gaging of key locations will be conducted to determine the discharge and the nature of the hydrograph Revision No 0 Date April 11 2011 Wolf Ru
176. ain and supervise Laboratory Technicians Ability to establish and maintain effective working relationships with regulatory agencies suppliers industries that discharge waste into the sanitary sewer system and fellow employees TB Laboratory QAP Appendix C September 16 2009 Revision 1 Communications Who Title Communicate About What How Often Director Reports data Occasionally Deputy Director Reports date special requests Weekly to daily Municipal Engineer Reports data computers Daily Pretreatment Manager Data special requests Daily to weekly Plant Operations Supervisors Data operations Daily Sludge Disposal Supervisors Data operations Daily Engineering Technicians Special requests Weekly Administrative Office Assistants General office work Daily Vendors Suppliers Purchasing pricing discount Weekly Labs from other cities Operation Problems Occasionally State Inspectors Operations paperwork Monthly EPA Inspectors Operations paperwork Occasionally Commercial Labs Data on an industry Monthly Special Requirements e May be required to possess a valid driver s license Physical strength and agility to allow considerable walking lifting climbing and working with samples that are odorous and hazardous Must be able to work weekends and holidays and perform on call duty Must be able to operate Urban County Government equipment and vehicles in a safe prudent and responsible manner All positions require drug testin
177. alculate the total number of colonies from all the plates and the total volume of sample used for all the plates Use these totals to calculate the number of coliforms per 100 mL Example 10 Blue colonies 50 mL Sample 5 Blue colonies 40 mL Sample 3 Blue colonies 10 mL Sample Fecal Coliforms 100 mL E i 18 50 40 10 C Plates with no Blue colonies e Do not use zero in the calculations Place the number one in the equation and use the largest volume of sample Report as less than lt Example 0 Blue colonies 50 mL Sample 0 Blue colonies 40 mL Sample 0 Blue colonies 10 mL Sample 51 SOP Fecal Coliform LFUCG Laboratory Page 52 of 219 Revision Number 3 Last Revised 09 09 D Countable plates with more than 60 Blue colonies e Ifonly one plate has been set up calculate as shown but place a approximately equal to sign in front of the answer Fecal Coliforms 100 mL x100 z 190 e Ifmore than one plate has been set up use the plate with the highest dilution the lowest sample volume Place an approximately equal to sign in front of the answer Example 150 Blue colonies 50 mL Sample 100 Blue colonies 40 mL Sample 80 Blue colonies 10 mL Sample Fecal Coliforms 100 mL x10 800 E Uncountable plates with more than 60 Blue colonies TNTC e Ifa sample contains colonies that are too numerous to count conduct enough dilutions in these tests to obtain discrete real number values Reporting a no
178. alls within analysis working range 0 01 1 00 QC is purchased from ERA Ortho P QC stock solution Using a commercially available Quality Control solution dilute to desired range and record manufacturers name lot and date Blank Reagent Grade DI Water 5 Procedure A Prepare the spectrophotometer by turning on the lamp and allowing it to warm up for at least one hour See the Spectrophotometer GLP for a detailed listing of necessary computer commands B Standards Prep 1 Prepare a series of phosphorus standards from the phosphorus standard solution 10 mg L according to the following table dilute to volume with water Volume of standard mL Standard concentration ppm Final Volume mL 0 5 0 02 250 1 0 05 200 5 0 10 500 5 0 20 250 10 0 50 200 20 0 80 250 50 0 1 00 500 2 These standards must be prepared daily B Sample Prep 1 Ifthe samples were not filtered in the field follow below procedure to do so now a b Begin by rinsing all filtering apparatuses with water magnetic filter funnel magnetic filter membrane and suction flask Place the magnetic filter membrane tightly on the suction flask and turn on the vacuum This will remove any water remaining in the filter funnel After a few seconds turn off the vacuum pump Using small tweezers place a cellulose acetate filter on each of the magnetic filter membranes and turn on the vacuum pump Place a magnetic filter funnel on top of each mag
179. alysis is applicable to investigations of stream pollution raw water sources and wastewater treatment systems 1 2 The fecal coliform analysis differentiates between coliforms of fecal origin Summary of Method 2 1 Executive Summary The sample is filtered through a Millipore membrane filter The filter is placed on a filter pad containing media in a sterile Petri dish The samples are then incubated at 44 5 C 0 2 C for 24 hours 2 hours Colonies are counted and fecal coliform calculations are performed 2 2 Discussion Fecal coliforms are defined as gram negative non spore forming rods The major species is Escherichia coli which indicates fecal pollution and the presence of enteric pathogens Colonies produced by fecal coliform bacteria are various shades of blue Non fecal coliform colonies are gray to cream colored Health amp Safety Precautions 3 1 3 2 3 3 3 4 All municipal and industrial wastewaters are potentially hazardous Gloves and safety glasses should be worn when dispensing these samples Possible exposure to enteric pathogens Care must be taken to avoid undue exposure A flame is used to sterilize forceps Maintain the area around the flame clear Contaminated used Petri dishes and lab equipment must be placed in Biohazardous waste container This Biohazardous waste container is autoclaved before disposal Sample Handling and Preservation 4 1 4 2 4 3 Samples should be collected in clean st
180. amage LC50 The concentration of a chemical in air or water that causes death to 50 of the animals Lead Pb Lead is the most ubiquitous toxic metal It is found everywhere in food the air soil and water Sources include lead based paint in old dwellings combustion of lead containing auto exhausts or industrial emissions Lead accumulates in bone and teeth The target organs are the kidneys nervous and reproductive systems Mean The average or sum of a group of observed values divided by the total number of observations Median The middle value of a series of numbers arranged in ascending or descending order Note If the distribution is not skewed Mercury Hg The central nervous system is the major site of toxicity from exposure to elemental mercury Milligrams per Liter A unit of the concentration of water or wastewater constituents It is 0 001 g of the constituent in 1 000 mL of water It has replaced the unit formerly used commonly parts per million to which it is approximately equivalent in reporting the results of water and wastewater analysis MSDS Material Safety Data Sheet Mutagen A material that induces genetic changes in the DNA of chromosomes Nickel Ni Nickel is a respiratory tract carcinogen Nitrogen An essential nutrient that is often present in wastewater as ammonia nitrate nitrite and organic nitrogen The concentrations of each form and the sum total nitrogen are expressed 45
181. ample Preservation This method cannot be performed on samples preserved in acid Because of this the samples should be prepped ASAP 2 Safety Wear a lab coat gloves and protective eyewear when prepping this experiment to avoid possible exposure to harmful substances 3 Apparatus CEM MARS Microwave Digestion Unit Advanced Composite Vessels ACV Graduated Cylinder Wash Bottle Automatic Pipettor 4 Reagents Purity of Reagents Reagent grade chemicals shall be used in all tests Unless otherwise indicated all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society Other grades may be used provided it is first ascertained that the reagent is sufficiently high in purity to permit its use without lessening the accuracy of the determinations Purity of Water Unless otherwise indicated references to water shall be understood to mean Type I reagent grade water Milli Q Water System conforming to the requirements in ASTM Specification D1193 Borate Buffer Solution Dissolve 61 8 g H3BO3 and 8 0 g NaOH in a 1 L volumetric flask containing at least 500 mL of DI water Swirl to mix and bring to volume Make fresh every 3 months Digestion Reagent Dissolve 20 1 g of K2S20s and 3 g of NaOH in a 1 L flask containing at least 500 mL of DI water Swirl to mix and bring to volume Make fresh every 3 months Quality Control Commercially available wastewater TKN standard
182. amples that contain turbidity only may be filtered through a membrane filter and analyzed using the hexavalent procedure Results are reported as dissolved hexavalent chromium 3 Samples without color or turbidity do not require sample blanks 8 2 Helpful Hints 1 Make sure to correct the test results for volume dilutions 2 Wipe off any liquid or fingerprints from TNT tube 9 QA QC Requirements 9 1 None required 37 10 11 12 SOP Cr 6 LFUCG Laboratory Page 38 of 219 Revision Number 3 Last Revised 09 09 Expected Results 10 1 Report positive reactions to supervisor immediately 10 2 KPDES Permit Requirements Depends on the particular industry being sampled Data Analysis and Calculations 11 1 None required Bibliography 12 1 HACH Water Analysis Handbook Method 8023 Chromium Hexavalent 1 5 Diphenylcarbohydrazide Method 2 Edition 1992 HACH Company Loveland CO 122 HACH DOC316 53 01035 Chromium Total and Hexavalent 1 5 Diphenylcarbohydrazide Method 10218 Chromium Hexavalent and Method 10219 Chromium Total TNTplus 854 2008 HACH Company Loveland CO 12 3 Standard Methods Part 3500 B Chromium Colorimetric Method APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 38 SOP LAB D O LFUCG Laboratory Page 39
183. and HQ40d meter 2 Turn the HQ40d meter on Push the Down arrow 3 Make sure that the meter is set to measure to measure pH 4 In three separate beakers or appropriate containers prepare fresh buffers of pH 7 0 4 0 and 10 0 5 Place probe in pH 7 0 buffer yellow color coded 6 Turn on stir plate 7 Press READ and wait until a stable reading is obtained lock icon 8 Rinse probe with Nanopure water 9 Place probe in pH 4 0 buffer red color coded 10 Turn on stir plate 11 Press READ and wait until a stable reading is obtained lock icon 12 Rinse probe with Nanopure water 13 Place probe in pH 10 0 buffer blue color coded 14 Turn on stir plate 8 2 8 3 15 16 17 18 19 20 SOP WH pH West Hickman WWTP Laboratory Page 9 of 219 Revision Number 3 Last Revised 09 09 Press READ and wait until a stable reading is obtained lock icon Rinse probe with Nanopure water Press DONE and the meter will display all data gathered Make sure that the calibration slope is acceptable typically 58 3 mV per pH unit at 25 C Press STORE twice to accept calibration Rinse the electrode in Nanopure water and blot dry prior to sample measurement Rinse the electrode with Nanopure between measurements to minimize contamination Sample Measurement 1 2 3 4 Put the electrode in the sample In the field readings are taken directly Turn on stir plate and press READ F
184. and total dissolved solids or the portion of total solids that passes through a filter Solids analyses are important in the control of biological and physical wastewater treatment processes and for assessing compliance with regulatory agency effluent limitations 2 2 Discussion A well mixed aliquot of sample is quantitatively transferred to a pre weighed evaporating dish evaporated to dryness at 103 C to 105 C and weighed to determine total solids Health amp Safety Precautions 3 1 Watch out for broken glass from crucibles cylinders and beakers 32 Wastewater samples should be considered potentially hazardous Use proper personal protective equipment 3 3 Crucibles can be hot 103 C to 105 C use proper gloves when handling Sample Handling and Preservation 4 1 Collect samples in plastic or glass containers 4 2 Nopreservative required 4 3 Maximum holding time 7 days at 4 C Reagents 5 1 Drierite 8 mesh 5 2 Nanopure Grade water 85 SOP Total Solids LFUCG Laboratory Page 86 of 219 Revision Number 3 Last Revised 09 09 Equipment amp Lab Ware 6 1 Denver Instrument Analytical Balance 6 2 ASTM Class 1 weight set 6 3 Vycor dishes or flat bottom crucibles 6 4 Oven 103 C to 105 C 6 5 Plastic 150 mL beakers 6 6 Stirrers 6 7 Tongs 6 8 Desiccators Interferences 7 1 Non representative particles such as leaves sticks fish and lumps of fecal matter should be excluded from the sample 7 2 Flo
185. and tracking including shipping receipts transmittal forms and internal routing and assignment records 5 Sample preparation including cleanup and separation procedures sample identification codes volumes weights instrument printouts and calculations 6 Sample analysis 7 Equipment receipt use specification operating conditions and preventative maintenance 8 Calculations and statistical formulas used by the laboratory including written procedures for calculations raw data and supporting information used for each calculation correct use of significant figures and identification of the least precise step in accord with limitations of the measurement system 9 Procedure to verify that the reported data is free from transcription and calculation errors 10 Data handling including reduction review confirmation interpretation assessment or validation and reporting 28 TB Laboratory QAP September 16 2009 Revision 1 14 3 14 2 2 11 QC measurements including procedure to select samples on which to perform QC measurements and assessment of method performance Other records retained by the laboratory include 1 All original raw data whether hard copy of electronic for calibrations analyst s worksheets and data output from instruments or equipment 2 Copies of final reports 3 Archived SOPs 4 Correspondence with sample submitters 5 Corrective action reports audits and audit responses
186. ar the bottom of a watershed where data will be most representative of the condition of the watershed b Site Selection Maps The following maps are used during training to assist Volunteer Monitors and Trainers with Site Selection Kentucky Atlas and Gazetteer ISBN Number 0 89933 216 1 Topozone http www topozone com Set to DD DDDD coordinates Arcview Shape Files including Counties Roads and Streams with current Watershed Watch Site List c Rationale Because site selection in Watershed Watch attempts to balance the interest of the Volunteer Monitor in a particular stream reach with the program s objective of collecting information about watershed conditions site selection occurs as part of Volunteer Monitor training so that trainers can encourage participants to Join a team at an existing site Open a new site at a location that will represent the condition of an undocumented watershed or Choose a stream reach that will represent the condition of their stream of interest d Accessibility and Appropriateness The site selection unit in Watershed Watch training identifies the following factors as important in site selection Proximity to existing Watershed Watch sites Access to the site using public rights of way and or the permission of the property owner Physical safety in accessing the stream via the streambank Wadeability of the stream Representativeness of the stream reach channel morphology and riffles
187. arator column are packed with low capacity strongly basic anion exchanger Ions are separated into discrete bands based on their affinity for the exchange sites of the resin The last column is a suppressor column that reduces the background conductivity of the eluent to a low or negligible level and converts the anions in the sample to their corresponding acids The separated anions in their acid form are measured using an electrical conductivity cell Anions are identified based on their retention times compared to known standards Quantitation is accomplished by measuring the peak area and comparing it to a calibration curve generated from known standards Sensitivity Ion Chromatography values for anions ranging from 0 to approximately 40 mg L can be measured and greater concentrations of anions can be determined with the appropriate dilution of sample with deionized water to place the sample concentration within the working range of the calibration curve Interferences Any species with retention time similar to that of the desired ion will interfere Large quantities of ions eluting close to the ion of interest will also result in interference Separation can be improved by adjusting the eluent concentration and or flow rate Sample dilution and or the use of the method of Standard Additions can also be used For example high levels of organic acids may be present in industrial wastes which may interfere with inorganic anion analysis Two comm
188. arbons that volatilize at temperatures below 80 C The method covers the range from 5 to 100 mg L of extractable material Organic Refers to volatile combustible and sometimes biodegradable chemical compounds containing carbon atoms carbonaceous bonded together and with other elements The principal groups of organic substances found in wastewater are proteins carbon hydrates and fats and oils OSHA Occupational Safety Health Administration ppb Parts per billion ppm Parts per million pH A measure of the hydrogen ion concentration in a solution expressed as the logarithm base ten of the reciprocal of the hydrogen ion concentration in gram moles per liter On the pH scale 0 14 a value of 7 at 25 C represents a neutral condition Decreasing values below 7 indicate increasing hydrogen ion concentration acidity increasing values above 7 indicate decreasing hydrogen ion concentration alkalinity Hydrogen ion concentration is the weight of hydrogen ion in moles per liter of solution Hydrogen ion concentration is commonly expressed as the pH value which is the logarithm of the reciprocal of the hydrogen ion concentration Phosphorus An essential chemical element and nutrient for all life forms Occurs in orthophosphate pyrophosphate tripolyphosphate and organic phosphate forms Each of these forms and their sum total phosphorus is expressed as mg L elemental phosphorus The method covers the determination of
189. arge amounts of turbidity may cause inconsistent results in the test because the acid present in the powder pillows may dissolve some of the suspended particles and because of variable desorption of orthophosphate from the particles Aluminum gt 200 mg L Arsenate Chromium gt 100 mg L Copper gt 10 mg L Iron gt 100 mg L Nickel gt 300 mg L extreme pH Silica gt 50 mg L Silicate gt 10 mg L Sulfide gt 90 mg L Zinc gt 80 mg L Ora TOWN BRANCH WASTEWATER TREATMENT PLANT Town Branch Laboratory 24 Hour Composite Samples Total Suspended Solids Method Residue Non Filterable EPA Method 160 2 Gravimetric Dried at 103 105 C Issued 1971 Volatile Suspended Solids Method Residue Volatile EPA Method 160 4 Gravimetric Ignition at 550 C Issued 1971 Suspended Solids amp Volatile Suspended Solids Enter Date NO ime Analysis Started are Number JERE 5 aja ae 3 3 2 oz ols oN 2 z ejo ola ala o B 2 mL W gm ajg 218 SE R e S Ss 915 o jo Qa un e z 8 Il W gm W2 Wi gm TSS mg L Wt Tare amp Dried Solids Wa ew Ee ees ei gt Ww mm Ea eee o o a KPDES Permit Limits on Plant Effluent Analyst Setting Up Analysis 30 mg L for Monthly Average 45 mg L for Maximum Weekly Average Presevation None required Maximum Holding Time 7 days Analyst Reading amp Calculating Analysis QUALITY CONTROL MANAGER IS TO RECEIVE A COPY O
190. ass boiling beads to each beaker Mark beakers at top of liquid with a Sharpie Add 1 mL of ammonium peroxydisulfate solution and 1 mL of H SO 31 69 to each marked beaker Place beakers on the large hot plates that are located in the hood Turn the Temp knob on the hot plates to HI Let each sample blank standard duplicate or QC stay on the hot plate until its volume decreases to 10 mL This process takes approximately 1 to 1 hours Do not allow the samples to completely evaporate Allow each sample to cool in the hood Add a drop of phenolphthalein indicator solution to each sample Add 1 mL of 10 N NaOH to each sample Continue adjusting the pH s by adding 1 N NaOH until each sample becomes faint pink in color The pH is approximately 10 at this point Bring samples back to colorless by adding 1 N H280 to each sample The pH is approximately 4 at this point Bring each sample s volume back up to the mark with water Filter each of the samples using the acid washed ceramic funnels and 1 um paper filters Pour 25 mL of each sample into its corresponding 4 1 2 oz plastic beaker Add 5 mL of combined reagent to the sample and mix thoroughly D Sample Analysis 1 The computer by comparing the concentration of each calibration standard against its absorbance can plot a calibration curve The correlation coefficient must be gt 0 994 to be acceptable If above criteria is not met the standards
191. at are necessary depending on the use to which volunteer generated data will be put Potential Data Rigor Requirements Compliance SOP and Use of Samplers QAPP pre pre KDOW approved SOP approved by by KDOW KDOW A Consultation Written Tier Data Use with KDOW Study Plan with federal standards Incident Reporting Education Programs Local Awareness Watershed I Screening Local Planning Activities Effectiveness De Monitoring TMDL Monitoring wm KR mK KK RK OK AA K IKIO X X 0 IV Use Support x x x x x x Determination X Required KDOW Kentucky Division of Water SOP Standard Operating Procedure O Optional QAPP Quality Assurance Project Plan TMDL Total Maximum Daily Load Watershed Watch is designed to meet the data rigor of Tier IL 2 Training a Standard Sampling Curriculum Volunteer Monitors who grab samples or supervise the sampling streamside are required to complete a Standard Sampling Training Module developed by the Training Committee and approved by the Science Advisors Committee of the ICC that addresses e Sample container handling Sample collection Sample preservation Sample transport and storage Documentation and chain of custody record completion QA QC procedures including duplicate samples and field blanks Communication with Event Coordinators and lab staff The module includes a demonstration ideal
192. atershed Habitat Assessment Streams ccccescceeseeesseceeceeeceeeeeeeeeenseees 33 List of Tables Table 1 Project Roles and Responsibilitics ia aos 11 Table 2 Monitoring Activity Overview ccccesccesecessceececsseceeceeeceeacecsaeceseceeeeenaeeesaeens 13 Table 3 Sampling Equipment Summary as acc ir 16 Table4 Project Schedule id a A a ai 21 Table 5 Summary of Data Quality Objectives and Standard Operating Procedures 23 Table 6 Acceptance Criteria for Water Chemistry and In Situ Measurements 24 Table 7 Completeness Goals of Sampling Activities ooonnncononcnoocnnoonconccconacann cono ncnnncnns 26 Table 8 Sampling Locations E ad 31 Table 9 Habitat Assessment Stream Segment oooccnnoconococonoconnnonnnoononoonccnonocananonnnconncnns 32 Table 10 Sample Preservation and Hold Time oooooonccnnocanocccicocononcoonoconcccono cono nonononnnonns 36 Table 11 Summary of Sampling Methods for Macroinvertebrates ooooonconinnnnnnncinmmm 41 Table 12 Field Equipment Calibration and Maintenance oooccnocnncnnocnnocconacononononninncnnnens 57 Wolf Run Watershed Page 7 of 67 Revision No 0 Based Plan Date April 12 2011 Table 13 Watershed Assessment and Management Reports ooooconocccnonccocononancnnnoconacnnos 60 Table 14 Data Qualifiers and Response cccccccecsseceseceseceeeeeeseecaecneeseeeenseecsaeeneenaes 62 List of Figures Figure 1 Wolf R
193. ating oil and grease if present should not be included in the sample Procedures 8 1 Steps 1 Clean and dry dishes in oven overnight 2 Remove dishes from oven and put into desiccator for at least 20 minutes 3 Calibrate Analytical Balance using ASTM Class 1 weight set 4 Weigh dish This is W 5 Add approximately 50 mL of mixed sample into the dish 6 Weigh dish and sample This is W2 7 Turn on fume hood 8 Leave samples in oven overnight 9 Remove dishes from oven and put into desiccator for at least 20 minutes 10 The next day calibrate Analytical Balance using ASTM Class 1 weight set 11 Weigh dish and dry sample This is W3 86 SOP Total Solids LFUCG Laboratory Page 87 of 219 Revision Number 3 Last Revised 09 09 8 2 Helpful Hints 1 Do not allow dishes to sit out in open air before weighing 2 Record oven temperature date and time Make sure to initial records 9 QA QC Requirements 9 1 None required 10 Expected Results 10 1 KPDES Permit Requirements 1 None required 10 2 Process Ranges Typical values total solids mg L for each plant are Town Branch W A S Thickener 3 68 Raw Sludge to Thickener 0 41 0 97 Digested Sludge 1 49 1 84 Belt Press Cakes 15 35 19 68 West Hickman Return Activated Sludge 0 79 1 16 W A S to Thickener 0 79 1 16 Belt Press Cakes 16 45 18 94 11 Data Analysis and Calculations 11 1 Total Solids mg L W3 W W2 W1
194. ation Operation Operation Operation September 16 2009 Analysis Requirements TB Laboratory QAP Appendix A Revision 1 Sample Name 1 Primary Digester 2 Primary Digester 3 Primary Digester Digested Sludge Belt Feed and Wastewater Belt Feed Solids Filtrate Filter Belt Press Belt 1 Cake Solids Belt 2 Cake Solids Belt 3 Cake Solids Belt 4 Cake Solids Filter Belt Press Cake Analysis pH Volatile Acids Total Alkalinity VA ALK Ratio Total Solids Volatile Solids pH Volatile Acids Total Alkalinity VA ALK Ratio Total Solids Volatile Solids pH Volatile Acids Total Alkalinity VA ALK Ratio Total Solids Volatile Solids pH Total Solids Volatile Solids September 16 2009 Analysis Requirements Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Removal of Volatile Solids Operation Total Solids TSS Total Phosphorus Total Solids Total Solids Total Solids Total Solids Metals Total Operation Operation Operation Operation Operation Operation Operation Operation TB Laboratory QAP Appendix A Revision 1 September 16 2009 Table A2 West Hickman WWTP Analysis List Sample Name Raw Influent Plant Effluent Raw Influent Combined Inf
195. atory management reviews raw data reports quality control data any discrepancies and corrective actions on a regular basis This review helps establish any recurring problems that require further investigation and action 34 TB Laboratory QAP September 16 2009 Revision 1 16 1 16 2 16 3 16 4 Section 16 Procedures for Permitting Departures from Documented Policies and Procedures Scope Departures from documented policies and procedures may include but not limited to e use of analytical methodology which is not KYDEP or U S EPA approved e use of samples which are not properly sampled or preserved for intended purpose analysis of samples outside the required holding times deviations from analytical or other laboratory SOPs deviations from standard QC practices use of alternative calibration practices reporting data which is not compliant with KYDEP or U S EPA analytical or QC requirements Requests for and Approval of Departures Requests for allowing departure from documented policies and procedures are directed to the Laboratory Supervisor The Laboratory Supervisor shall evaluate the reasons for such departures The Quality Assurance officer is consulted for all matters that may affect the quality of analytical data Written approval by the Laboratory Supervisor is required before such departures are made The Laboratory Supervisor documents and files all departures and their duration Permanent departures are documen
196. base of its neck with sample and turn on the self contained stirring unit switch located on top of the probe Assure that there are no air bubbles on the surface of the probe tip Press Read the screen will display Stabilizing and a progress bar will scroll from 0 to 100 Reading stability is indicated by the appearance of a Padlock icon in the upper left corner of the display screen 41 10 11 8 2 SOP LAB D O LFUCG Laboratory Page 42 of 219 Revision Number 5 Last Revised 09 09 5 Record the indicated value turn the stirrer off remove the probe and rinse tip with Nanopure water and proceed to the next sample or store until needed 6 DO NOT store probe in the BOD bottle containing water Probe can be stored dry on the bench top Helpful Hints 1 The meter is designed to be maintenance free when needed clean the exterior with a damp cloth 2 The probe s maintenance consist of maintaining the probe tip clean frequent rinsing with Nanopure water is sufficient 3 DO NOT scrub the sensor cap or lens 4 DO NOT use any organic solvents on the sensor cap or probe body QA QC Requirements 9 1 Meter must be calibrated a minimum of once per analysis day 9 2 Permit sample hold times must be 15 minutes or less 9 3 Probe condition must be properly maintained through routine cleaning See Section 8 2 Helpful Hints Expected Results 10 1 KPDES Permit Requirements 7 0 mg L is the lowest D
197. be recorded legibly on another line or above or below the original info If a separate sheet is necessary for new Wolf Run Watershed Page 27 of 67 Revision No 0 Based Plan Date April 11 2011 information the original sheet should be attached to the new sheet and initialed and dated The following field documents shall be used in this project e Site Characterization Form High Gradient Stream Data Sheet for Habitat Assessment Conductivity Survey Field Data Sheet Pebble Count Field Data Sheet Water Quality Chain of Custody Macroinvertebrate Chain of Custody Sample Labels Field Rite in the Rain Notebook Field Reference Reach Notebooks Field Meter Calibration Logs Copies of these documents are found in Appendix A where applicable All raw data collected in the field will ultimately be submitted in the chemical or biological data package However all field notes including the location and frequency of QC sampling in situ measurements and calibration and maintenance logbooks will be retained for the duration of the grant period Where possible all field in situ measurements will be recorded on the datasheet or chain of custody However if necessary results or notes may be maintained in a field notebook Equipment calibration and maintenance logs will be documented and recorded per procedure specifications A9 2 Laboratory Documentation and Records Chemical laboratories are required to maintain a curren
198. bicarbonate ratios but increasing the concentration 100X Weigh out 1 91 g of Na CO and 1 43 g of NaHCO into a 100 mL volumetric flask 0 05 mL of this solution is added to 5 mL of all samples and standards to resolve the water dip associated with the fluoride peak Borate Buffer Solution Dissolve 61 8 g H BO and 8 0 g NaOH in a 1L volumetric flask containing at least 500 mL of DI water Swirl to mix and bring to volume Make fresh every 3 months Digestion Reagent Dissolve 20 1 g of K SOx and 3 0 g of NaOH in a IL flask containing at least 500 mL of DI water Swirl to mix and bring to volume Make fresh every 3 months Quality Control Commercially available wastewater TKN standard Environmental Resource Associates Ready To Use Wastewater QC Standards Cat 743 Arvada CO 1 800 ERA 0122 Glutamic Acid Stock Standard C Hs NH2 COOH 100 ppm Dry Glutamic Acid in oven at 105 C for 24 hours Cover and place in dissector until cool Dissolve 1 051g in DI water and dilute to 1L preserve with 2mL chloroform CHCl Store in refrigerator for no longer than 6 months Stock standard solutions 1000 mg L 1 mg mL Stock standard solutions may be purchased SPEX as certified solutions or prepared from ACS reagent grade materials dried at 105 C for 24 hours Nitrate Stock Standard NO3 N 1000 ppm dry Potassium Nitrate KNO3 in oven cover and place in dissector until cool Dissolve 0 7218g in DI water and bring
199. ce Lexington Fayette Urban County Government 301 Lisle Industrial Avenue Lexington Kentucky 40511 859 425 2415 dprice lfucg com Jason Backus Kentucky Geological Survey 228 Mining amp Mineral Resources Building University of Kentucky Lexington KY 40506 0107 859 323 0555 jbackus uky edu Ken Cooke Friends of Wolf Run 639 Cardinal Lane Lexington Kentucky 40503 859 940 8234 ken cooke kbcnet1 com Brooke Shireman KY Division of Water Lisa A Hicks KY Division of Water 200 Fair Oaks Lane Frankfort KY 40601 200 Fair Oaks Lane Frankfort KY 40601 502 564 3410 502 564 3410 brooke shireman ky gov lisa hicks ky gov Wolf Run Watershed Based Plan Page 9 of 67 Revision No 0 Date April 12 2011 A4 Project Task Organization This Quality Assurance Project Plan QAPP prepared by Third Rock Consultants LLC Third Rock is to be reviewed and approved by the Kentucky Division of Water KDOW and the Lexington Fayette Urban County Government LFUCG This QAPP establishes the planning implementation and assessment procedures necessary to meet the minimum data quality objectives DQOs for the monitoring of the Wolf Run watershed Third Rock is committed to producing quality data that will assist the KDOW and LFUCG in obtaining the information necessary to facilitate the development of a Wolf Run Watershed Based Plan This QAPP is designed to provide a compl
200. ceps Maintain the area around the flame clear Contaminated used Petri dishes and lab equipment must be placed in Biohazardous waste container This Biohazardous waste container is autoclaved before disposal Sample Handling and Preservation 4 1 4 2 4 3 Samples should be collected in clean sterile glass or plastic containers If chlorine is in the sample containers should be treated with 4 drops of 10 Sodium thiosulfate before autoclaving Run test immediately after sampling or preserve sample at 4 C for a maximum of 6 hours 17 SOP WH Fecal Coliforms West Hickman WWTP Laboratory Page 18 of 219 Revision Number 4 Last Revised 09 09 Reagents 5 1 Peptone powder 5 2 Peptone buffer solution pH 7 00 0 1 stored at 4 C 5 3 m FC media with rosolic acid for fecal coliforms stored at 4 C 5 4 Sodium thiosulfate 10 solution 5 5 Lysol disinfectant 20 solution Equipment amp Lab Ware 6 1 Vacuum flask 6 2 Millipore single use 47 mm Petri dishes with pads 6 3 Millipore sterilized 47 mm filter 6 4 Forceps 6 5 4 5 X 9 inch sterile sampling bags 6 6 Bunsen burner and striker 6 7 Pipettes and sterile tips 6 8 Sterilized filter holder plastic or glass 6 9 Gable topped water bath at 44 5 C 0 2 C 6 10 Thermometer 6 11 ASTM Thermometer 6 12 Tower Steam Indicator Strips 6 13 ODO Clave Heat Activated Deodorant Pads 6 14 Autoclavable Biohazard waste bags and deposit box 6 15 Autoclave 6 16
201. ch OO S ae T T S TT TTT Oi Data Entry and Analysis OO MT pp Report Completion PY ft 4 Hydrogeomorphic Assessments Cross sections profiles and ite cm MIOS BERR Data Analysis Mm fT Report Completion UA OS eee B Water Quality Monitoring Monthly Sampling 10 imme E coli Geomean Sampling mmm f 7 T fy ty tft ft ft E Y Data Entry and Review Mr eC k eee Loading Calculations and Source Determinations Report Completion SDs aa Watershed Based Plan Chapter 3 Monitoring ST Chapter 4 Analysis O Bante Chapter 5 BMPs Chapter 6 Strategy O SSS SSS T i Chapter 7 Implementation TTT Water quality monitoring will be conducted monthly beginning in May and continuing until February 2012 At least two of the events are to be considered wet weather and two of the events are considered dry weather Representative dry weather sampling conditions are defined by an antecedent period of 5 days during which there is no rainfall Representative wet weather sampling conditions are defined by a period of at least 72 hours of dry weather preceding a rain event with a total accumulation of at least 0 1 inch Sampling during wet weather will occur on the hydrographic rise Additional sampling Wolf Run Watershed Page 21 of 67 Revi
202. chival system Hard copy files will be stored onsite under secure conditions No data shall be publicly disseminated unless first reviewed and approved for release by the Project Team including the Grantee Project Manager QA Manager and FOWR Sampling Coordinator Prior to that time data will be managed by Third Rock Subsequent to final approval Project Team members may distribute the results as appropriate SECTION C ASSESSMENT AND OVERSIGHT Assessment and response actions are necessary to ensure that this QAPP will be implemented as approved For a general summary of these assessments see Table 13 If at any time a project team member finds an error or non conformance in the QAPP the QAPP will be revised and redistributed to those on the distribution list subsequent to approval The KDOW QA officer may freely review all field and laboratory techniques as requested Any identified problems will be corrected based on recommendations by the KDOW QA Officer Wolf Run Watershed Page 59 of 67 Revision No 0 Based Plan Date April 11 2011 TABLE 13 WATERSHED ASSESSMENT AND MANAGEMENT REPORTS QAPP Revision KDOW Audit Frequency As necessary As requested Purpose Address non conformances lor errors in the QAPP Ensure conformance to project objectives Parties Responsible For Performing Project Team Members KDOW Responding QA Manager Parties of concern Reporting Method Distribution of amen
203. ciency Form Client Name Sample ID Third Rock Project Original Taxonomist Second Taxonomist Original Date Completed Review Date Completed Organisms Enumerated Taxonomist 1 Organisms Enumerated Taxonomist 2 Percent Difference in Enumeration PDE n n2 n n2 x 100 Difference in Enumeration PDE n organisms counted by Taxonomist 1 no organisms counted by Taxonomist 2 Percent Taxonomic Disagreement PTD PTD 1 comppos N X 100 ComPpos number of taxonomic agreements see Taxonomic Comparison Form N total number of organisms Comments Reviewed By Date Updated 4 29 10 Third Rock Consultants LLC Macroinvertebrate Sample Taxonomy Precision Form Client Name Sample ID Third Rock Project Agreements Revered By Date Updated 4 29 10 25262728 293031 32 91011 12 13 14 15 16 17181920 21 22 23 24 5678 1234 10M00 MOFA oOowow N 0 10 KROMO Nom 0 010 N WwW N OM O 1010010 NW Ot omoaoow MANDOS Povon Mano 10m KNOY Mi MA 9400mMu moo tn 000 Is OM oO HOS NAM NN Ww 0 0 MAL 10 0 010 NOAM N oer MOD NNOOW MOomo QOON ownmwa ane mam NO STW oso FRY DOO Otono ON NA om st ON 0m mm ammo AANAD 0100 mM Mm OW WwW 00 0 Mm0oONnO0O NI STD mana OMNOM AwWn 00 Ongo MOMAN ower ore onoo
204. cies and Procedures references procedures for taking corrective actions when matrix spikes do not meet acceptance criteria 6 5 Laboratory Control Samples 6 5 1 6 5 2 6 5 3 6 5 4 6 5 5 For each test method laboratory control samples LCS are analyzed at a minimum of one per batch The results of the LCS analyses are used to determine batch acceptance Standards for preparing LCS samples are obtained from a second source The matrix spike sample may be used as an LCS when the matrix spike acceptance criteria are as stringent as the LCS acceptance criteria and a LCS has not been prepared and analyzed for the sample batch Each analytical SOP references quality control criteria to use in determining discrepancies and accepting data when laboratory control samples do not meet acceptance criteria TB Laboratory QAP September 16 2009 Revision 1 6 6 6 7 6 5 6 Section 15 Corrective Action Policies and Procedures references procedures for taking corrective actions when laboratory control samples do not meet acceptance criteria Matrix Spike Duplicates and Sample Duplicates 6 6 1 6 6 2 6 6 3 6 6 4 6 6 5 6 6 6 Matrix spike duplicates or sample duplicates are performed at a rate of one per 20 or fewer environmental samples per matrix type per sample extraction or preparation procedure The sample used for the matrix spike duplicate is the same as used for the matrix spike When sample duplicate
205. city readings will be averaged over a time period of 25s 45s depending on in stream conditions If the water depth is gt 2 5 feet at a station indicate the depth 0 2 or 0 8 associated with each of the two velocity measurements Record the ending edge LEW or REW as well as the depth and velocity if these exist If the stream cannot be safely waded or if a flow meter is not accessible floats can be used to estimate stream velocity needed for stream discharge computation All measurements using this procedure should be flagged as estimated on field data sheets and on final data reports The following steps are used in these conditions 1 Find a long relatively straight section of stream that allows a travel time of 20 seconds A shorter time can be used if these conditions cannot be met 2 Select two cross sections along the reach one at the top and one at the bottom 3 Measure the width of the stream at the cross sections and in a few areas between the cross sections to obtain an average width If the stream is not wadeable estimate the width Record the width on the field data sheet 4 Estimate how far an object will float in 20 seconds and stretch a tagline along the stream bank to account for that distance A distance of 30 50 feet is ideal A shorter run length may be used if these conditions cannot be met 5 Based on the width divide the stream into 2 3 longitudinal profiles Measure or estimate the depths at these profiles
206. cted and any corrective actions taken e Maintain a state of increased vigilance 7 4 3 Warning limit trend exceedance occurs when two or more consecutive results for the laboratory control standard exceed the warning limit A general response to a trend exceedance includes the following e Inform the immediate supervisor of the warning limit trend exceedance e Conduct a systematic investigation as soon as possible to locate the source of the problem e Take appropriate corrective action when a problem is located e Document warning limit exceedance including the details of the occurrence whether a problem was detected and any corrective actions taken 7 4 4 The laboratory has a written response plan for the analyst to follow in the event of a failure of a laboratory control standard or other criteria This plan is found in Section 15 Corrective Action Policies and Procedures 7 4 5 SOPs for test methods and lab procedures are reviewed on an annual basis The designated Quality Assurance Officer and Laboratory Supervisor performs reviews 14 TB Laboratory QAP September 16 2009 Revision 1 8 1 Section 8 Equipment Procedures for Calibration Verifications and Maintenance Equipment Calibration 8 1 1 8 1 2 An initial calibration is performed on instrumentation and equipment as specified in the test method Calibration standards are traceable to a National Standard where available The procedures for calibratio
207. cted the stream by altering watershed hydrology and sediment transport patterns The large amount of impervious surface has greatly reduced the capacity of the watershed to capture and filter rainfall Higher runoff rates mean that runoff reaches the stream channels more quickly flashier flows and peak discharge rates are higher compared to an undeveloped watershed for the same size rainfall event These effects are known as hydromodification Hydromodification can also be direct modification of a stream for purposes of flood control navigation sediment control infrastructure protection etc such as Wolf Run Watershed Page 34 of 67 Revision No 0 Based Plan Date April 11 2011 channelization armoring and removal of riparian vegetation Channel erosion and bank failure is often caused or exacerbated by hydromodification activities Nine hydrogeomorphic monitoring sites have been preliminarily identified throughout the watershed where quantitative data will be collected to measure channel change in representative reaches It is expected that the nine hydrogeomorphic monitoring sites represent stream reaches that are susceptible to the effects of hydromodification are in need of management to stop further degradation and would be good locations to implement remediation Assessment will include a series of spatially integrated high resolution cross section and longitudinal profile surveys and streambed substrate evaluation to determine
208. d and updates will be made as needed to keep this document up to date and relevant The Town Branch Laboratory as part of the Lexington Fayette Urban County Government LFUCG prepared this document to serve as a clearinghouse of information related to the operation of the Laboratory housed at Town Branch WWTP The Laboratory serves the e Town Branch WWTP KPDES Permit No KY0021491 e West Hickman WWTP KPDES Permit No KY0021504 e Blue Sky WWTP KPDES Permit No KY0027286 The laboratory is operated in accordance with the Federal Register 40 CFR Part 122 136 et al Primary references include e EPA 600 4 79 020 Methods for Chemical Analysis of Water and Wastes U S Environmental Protection Agency Office of Research and Development Washington DC 1982 e EPA 600 8 78 017 Microbiological Methods for Monitoring the Environment Water and Wastes U S Environmental Protection Agency Environmental Monitoring and Support Laboratory Office of Research and Development Washington DC 1978 e Standard Methods for the Examination of Water and Wastewater APHA American Public Health Association Standard Methods 21st edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 TB Laboratory QAP September 16 2009 Revision 1 1 1 1 2 1 3 Section 1 Quality Policy Statement Quality Policy Statement This Quality Assurance Plan QAP provides a written plan of operation for the
209. d hardness Samples for total phosphorus ortho phosphorus total kjeldahl nitrogen and nitrate will be delivered to the Kentucky Geological Survey laboratory Volunteers will perform field measurements of turbidity dissolved oxygen specific conductance temperature and pH Third Rock will accompany the volunteers during each event to conduct discharge monitoring and collect the field filtered ortho phosphorus sample Also due to the short time period in which wet weather events can be collected on the hydrographic rise two wet weather sampling events will be collected solely by Third Rock staff If for some reason volunteers are not able to perform the sampling Third Rock will collect additional sampling events Efforts will be made to avoid collecting samples on Thursday as this is the busiest day at the Town Branch laboratory In addition to the monthly sampling volunteers will collect an additional four events for E coli and fecal coliform to evaluate the geometric mean for the primary contact period A Third Rock staff member will accompany the volunteers during each event to conduct discharge monitoring Only flow and E coli and fecal coliform will be collected during these events The LFUCG Town Branch laboratory will analyze the samples Subsequent to the completion of all sampling results will be compiled and analyzed in a final Wolf Run Watershed Monitoring Report Further this data will be used in conjunction with other dat
210. d to determine if the project standards listed in Table 4 are met For benthic macroinvertebrate samples vouchers are collected Wolf Run Watershed Based Plan Page 25 of 67 Revision No 0 Date April 11 2011 to ensure accuracy Field photographs are used to document accuracy for habitat assessment For the conductivity survey the GPS units used to document locations shall be accurate to at least 20 feet and the latitude and longitude shall be recorded in decimal degrees to six decimal places in datum NAD83 A7 2 3 Representativeness Representativeness is the degree to which data accurately and precisely represent an environmental condition Representativeness is largely a product of proper selection of sampling sites within the watershed and proper execution of the methodology For instance per the sampling method grab samples are to be collected from the thalweg and not from the bank in order to ensure representativeness Representativeness is also ensured by collection under the specified sampling conditions Representative dry weather sampling conditions are defined by an antecedent period of 5 days during which there is no rainfall Representative wet weather sampling conditions are defined by a period of at least 72 hours of dry weather preceding a rain event with a total accumulation of at least 0 1 inch Sampling during wet weather will occur on the hydrographic rise Representative conditions for macroinvertebrat
211. dard and sample Because bromide and nitrate elute very close together they can potentially interfere with each other It is advisable not to have Br NO3 ratios higher than 1 10 or 10 1 if both anions are to be quantified If nitrate is observed to be an interference with bromide use of an alternate detector e g electrochemical detector is recommended Method Interferences may be caused by contaminants in the reagent water reagents glassware and other sample processing apparatus that lead to discrete artifacts or elevated baseline in ion chromatograms Samples that contain particles larger than 0 45 micrometers and reagent solutions that contain particles larger than 0 20 micrometers require filtration to prevent damage to instrument columns and flow systems If a packed bed suppressor column is used it will be slowly consumed during analysis and therefore will need to be regenerated Use of either an anion fiber suppressor or an anion micro membrane suppressor eliminates the time consuming regeneration step by using a continuous flow of regenerant Because of the possibility of contamination do not allow the nitrogen cylinder to run until it is empty Once the regulator gauge reads 100 kPa switch the cylinder out for a full one The old cylinder should them be returned to room 19 for storage until the gas company can pick it up Make sure that the status tag marks the cylinder as EMPTY Sample Handling and Preservation Sampl
212. ded QAPP Corrective Action Response Laboratory Demonstration of Performance Prior to initial analysis Ensure analyst is capable of performing the method to specifications Laboratory QA Director Laboratory Analysts Internal Lab documentation Laboratory Internal Audits Annually at minimum Ensure conformance to methods regulations and procedures Laboratory QA Director Laboratory Analysts Internal Lab documentation Progress Assessment Quarterly Evaluate the status on project related objectives and concerns Grantee Project Manager or designee Section 319 h Nonpoint Source Project Progress Report Volunteer Field Sampling Audit Once during project Assess volunteer sampler conformance to proper sampling and documentation protocols QA Manager or designee Volunteer Samplers Trainers Field Sampling Audit Checklist Analytical Results Review Subsequent to each sampling event Evaluate the conformance of laboratory data to project IDQOs QA Manager or designee Laboratory QA Director Laboratory Data Quality Checklist Quality Evaluation Once End of Project Evaluate the quality assurance and compare the data produced to project DOQIs QA Manager or designee KDOW QA Officer Grantee Project Manager Final Monitoring Reports To ensure conformance with this QAPP and the applicable re
213. dentify significant changes in conductivity levels to pinpoint sources of pollution Oakton Instruments Waterproof TDSTestr and ECTestr Series Instructions http www 4oakton com Manuals ConductivityTDS TDS_ECTestrmnl pdf Macroinvertebrate Collection and Identification Calculation of the Macroinvertebrate Bioassessment Index MBI Macroinvertebrates have varying tolerances for water pollution and therefore can serve as long term indicators of water quality KDOW 2009b Laboratory Procedures for Macroinvertebrate Processing and Taxonomic Identification and Reporting Kentucky Department of Environmental Protection Division of Water Frankfort Kentucky KDOW 2009c Methods for Sampling Benthic Macroinvertebrate Communities in Wadeable Waters Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky KDOW 2008 Methods for Assessing Biological Integrity of Surface Waters in Kentucky Kentucky Department of Environmental Protection Division of Water Frankfort Kentucky Habitat Assessment Provide a semi quantified evaluation of the general habitat of the stream Barbour M T J Gerritsen B D Snyder and J B Stribling 1999 Rapid Bioassessment Protocols for Use in Streams and Wadeable Rivers Periphyton Benthic Macroinvertebrates and Fish Second Edition EPA 841 B 99 002 USEPA Office of Water Washington D C Hydrogeomorphic Sampling Determine the degree to which s
214. diate corrective action and immediately notifies in writing the parties that receive the data Analytical Quality Control Standards All analytical quality control standards that are used are traceable to a National Standard Reagents Reagents are prepared using reagent grade chemicals or better Each reagent container received by the laboratory is documented by marking the container with an adhesive label and indelible ink Each marking label indicates the date received date opened and any applicable expiration date Glassware Glassware used for purposes that may subject it to damage from heat or chemicals is made of borosilicate glass Glassware used for volumetric measurement purposes is Class A rated Laboratory Pure Water The Town Branch Laboratory uses Nanopure grade water Tap water is purified through a series of steps including coarse filtration water softening chlorine removal filtration reverse osmosis purification and 4 cartridge Nano pure purification process The nano pure system provides continuous conductivity readings of the of the final product Conductivity values range between 17 5 and 18 0 megOhm Readings below this range indicate spent cartridges and a need to service the unit In addition the resistivity of the Nanopure water is checked periodically with a calibrated conductivity meter Resistivity values of the laboratory pure water are at least 0 5 megOhm cm at 25 C Filters are replaced when the values re
215. ding depth depends on the size of the person sampling the stream s velocity and depth and the streambed material Caution should always be used when wading streams deeper than three feet Additional caution should be used when the streambed is composed of loose or slippery material Algae coated cobbles can be slippery and as dangerous as ice A personal floatation device should be worn when wading streams three feet or greater in depth The sampler approaches the sampling site from a downstream location walking upstream to the sampling site to avoid disturbing bottom sediments that could contaminate the water quality sample An ideal wading location is in the center of the stream and at the head of a riffle so that water current produces a good flow past the sampling point c Sampling for parameters other than bacteria The sampler first contaminates gloves if worn with stream water Sample bottles are then contaminated with stream water Pre marked sample bottles are rinsed once with stream water The sample bottle is then lowered from the surface to the bottom of the stream until the sample bottle touches the stream bottom without disturbing sediments Upon reaching the bottom the bottle is raised to the surface matching the transit rate when the bottom was lowered Repeat until the bottle is filled with stream water Rinse the bottle cap in the stream and cap the bottle d Sampling for bacteria The sampler first contaminates gloves
216. e 6 16 Sterile blue sheets 6 17 Indicator tape 6 18 Autoclavable Nalgene squeeze bottles for peptone Interferences 7 1 Bacteria from the surrounding environment 7 2 Cross contamination from one sample to the next 7 3 Lack of aseptic techniques 55 Procedures 8 1 Steps 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 SOP Total Coliforms and E coli LFUCG Laboratory Page 56 of 219 Revision Number 1 Last Revised 09 09 Clean work area with Lysol disinfectant 20 solution Light Bunsen burner with striker Open sterile filter holder Use sterile blue sheet as a sterile field Indicator trip and tape should indicate that the filter has been sterilized Use Pall petri dishes with sterile pad already in dish Break open m ColiBlue ampule of media and pour the contents evenly over the absorbent pad and place the lid on the Petri dish Decant excess media and cover dish to protect sterile pad Place the bottom of the sterile filter holder onto the vacuum flask Flame forceps remove sterilized filter from packaging and place onto sterilized filter holder grid side up Do not touch the filter with anything except the forceps Place or clamp the top unit onto filter holder Gently mix sample In advance determine sample volume that will yield 20 60 fecal coliform units FCU If the volume of sample to be used is 0 1 to 5 mL pour approximately 10 mL of peptone int
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218. e Dil area type in the dilution factor if different from 1 Do this for all standards blanks quality controls duplicates and samples to be run under this schedule h Save the schedule and obtain a printout of it i Standardize the Dionex Ion Chromatography System by running the standards Standard 1 Standard 2 and Standard 3 Run the QC standards Run the prepblank and DI water blank Run the samples duplicates and blanks Run the QC standards at the end 5 Calculations A Calculations are based upon the ratio of the peak area and concentration of standards to the peak area for the unknown Peaks at the same or approximately the same retention times are compared Once the method has been updated with the current calibration this is calculated automatically by the software using linear regression Remember that when dilutions are being run the correct dilution factor must be entered Manual calculations are based upon the ratio of the peak and concentration of standards to the peak area for the unknown when the software will not automatically calculate the unknown concentration Peaks at the same or approximately the same retention times are compared The unknown concentration can be calculated from using this ratio Remember that when dilutions are being run that the correct dilution factor must be entered before you will get the correct result C When possible the unknown should be bracketed between two knowns and the calculat
219. e Standard Operating Procedures section describes all procedures currently in use by the laboratory Included in this section are each method s SOP number document name source and whether it is listed in 40 CFR Part 136 as an approved method 9 2 Standard Operating Procedures SOPs The SOPs are incorporated in this Quality Assurance Plan and may be obtained from the laboratory management In addition each laboratory staff member is issued a manual containing all current SOPs A laboratory copy is used for updates and changes between revisions 19 TB Laboratory QAP September 16 2009 Revision 1 10 1 10 2 10 3 Section 10 The Laboratory s Physical Facilities Including Services and Resources Building The Town Branch Laboratory operated under the Lexington Fayette Urban County Government is located in the Town Branch Administration building 301 Lisle Industrial Avenue Lexington Kentucky The Town Branch Laboratory performs routine monitoring for Town Branch Wastewater Treatment Plant West Hickman WWTP and Blue Sky WWTP several industrial pretreatment samples and samples brought in from other outside sources The Administration building housing the laboratory was constructed in 1970 Currently the laboratory and offices occupy 5 735 square feet of floor space The laboratory originally occupied 2 370 square feet of floor space In 2004 the lab was expanded to include an additional 3 365 square feet of floor space The
220. e collector person receiving sample 26 TB Laboratory QAP September 16 2009 Revision 1 13 1 13 2 13 3 13 4 13 5 Section 13 Sample Tracking and Storage Procedures Scope A clear sample tracking record allows any questions concerning sample integrity to be answered during any step of the process Samples are stored in areas which isolate samples sufficiently to prevent cross contamination with other samples reagents or standards Procedures for sample handling and tracking may vary depending upon sample origin Sample integrity and reliable test data are ensured when valid laboratory procedures are established and strictly followed Sample Tracking Record 13 2 1 Sample logs bench sheets and preparatory records are clearly marked to identify all personnel associated with each sample 13 2 2 Chain of custody forms or bench sheets must be completed to include use of preservation and sample containers required by approved test method 13 2 3 No samples are accepted without proper documentation Samples are checked to insure that the container is compatible with the intended analysis Proper Storage and Avoidance of Cross contamination of Samples 13 3 1 Storage facilities are provided for samples to prevent cross contamination and are consistent with sample preservation requirements of the method 13 3 2 Samples are stored away from all standards reagents food and other potentially contaminating sources Securit
221. e four digit number listed on the upper left corner of the reagent label in the contents list and in the test procedures 14 USE PROPER ANALYTICAL TECHNIQUES Use test tube caps or stoppers not your fingers to cover tubes during shaking or mixing Wipe up any reagent chemical spills immediately Tightly close all containers immediately after use Do not interchange caps from containers 15 4 Hold dropper bottles vertically upside down and not at an angle when dispensing a reagent Squeeze the bottle gently to dispense the reagent one drop at a time Thoroughly rinse test tubes before and after each test Avoid prolonged exposure of equipment and reagents to direct sunlight Protect reagents from extremes of temperature DISSOLVED OXYGEN KIT CODE 7414 Instructions 0688 DO DISSOLVED OXYGEN KIT CODE 5860 Instructions 0688 DO 17 SHORT FORM INSTRUCTIONS Read all instructions before performing test Use this guide as a quick reference oo a ee A 10 11 12 13 Fill Water Sampling Bottle 0688 DO Add 8 drops of Manganous Sulfate Solution 4167 Add 8 drops of Alkaline Potassium lodide Azide 7166 Cap and mix Allow precipitate to settle Use the 1 0 g spoon to add Sulfamic Acid Powder 6286 or add 8 drops of Sulfuric Acid 1 1 6141 WT Cap and mix until reagent and precipitate dissolve Fill test tube 0608 to the 20 mL line
222. e laboratory system is out of control D2 Validation and Verification Methods The QA Manager will use the Field Sampling Audit Checklist and the Laboratory Data Checklist Appendix A to document the conformance of the data to this QAPP This review will be submitted to the KDOW along with the data The QA Manager will be responsible for making any final decisions concerning data quality and acceptability All final reports will receive an internal peer review to evaluate the content calculations and data analysis in the report The reports will also undergo an internal grammatical review to look for grammatical errors and formatting Lastly the final report will receive a review from the Project Team prior to submission to the KDOW to ensure that all project objectives are achieved Revision No 0 Date April 11 2011 Wolf Run Watershed Based Plan Page 62 of 67 D3 Reconciliation with User Requirements and Data Quality Objectives In the final report descriptions of all relevant background information summary water body details monitoring results recommended solutions and implementation plans will be detailed Included in this document will be an overall assessment of the data quality and the uncertainty involved in the results SECTION E REFERENCES AND CITATIONS Barbour M T J Gerritsen B D Snyder and J B Stribling 1999 Rapid Bioassessment Protocols for Use in Streams and Wadeable Rivers Periphyton Benthic
223. e most productive habitat in the stream niche i e riffle Multi habitat samples are intended to identify other taxa present in the stream that may not be collected in the semi quantitative sampling These two sample types must be kept separate for effective diagnosis of impairment A summary of the collection techniques used for wadeable and headwater streams is shown in Table 11 and further described in the following sections It is important to keep in stream habitat intended for benthic macroinvertebrate sampling intact and undisturbed until the single and multi habitat samples have been collected Wolf Run Watershed Page 40 of 67 Revision No 0 Based Plan Date April 11 2011 Therefore field personnel must avoid walking through areas designated for collection of benthic macroinvertebrates until sampling has been completed Failure to use caution could result in sample degradation After collections are completed large sticks and leaves will be washed in the field inspected for organisms and discarded Rocks will be elutriated and hand washed into a bucket and 600um sieve This process will be repeated until a manageable amount of debris and organisms relative to size of sample container can be preserved for laboratory sorting Samples may be partially field picked using a white pan and fine tipped forceps The sample container will be preserved with 95 ethanol While at the sampling location all macroinvertebrate samples will rece
224. e reducing agent The bisulfite treatment will also eliminate this interference High silica concentrations cause positive interference Sample Handling and Preparation If possible a filtered aliquot should be used If the analysis cannot be performed the day of collection the sample should be preserved by the addition of 2 ml concentrated H SO per liter and refrigerated at 4 C Recommended holding time is 48 hours Suspended solids should be removed by filtration Note Samples should be filtered PRIOR to preservation 2 Safety Safety glasses gloves and a lab coat should be worn while performing this analysis due to the use of and possible exposure to strong acids 3 Apparatus Varion 50 Spectroscopy system Filtration Apparatus Gelman 47mm magnetic filter funnel Suction flasks connected in series to a vacuum system Reservoir for the filtrate 500 mL Trap which prevents liquid from entering the vacuum system 1000 mL Cellulose acetate filters Micron Separations Inc 47 mm 0 45 micron cellulose acetate filter membrane Analytical balance capable of weighing to the nearest 0 0001 g Drying oven Desiccator 4 1 2 oz plastic beakers Must be single use only Rinse three times with DI water 4 Reagents Purity of Reagents Reagent grade chemicals shall be used in all tests Unless otherwise indicated all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical
225. e sample bottle B2 2 6 4 In situ Measurements Volunteers will perform field measurements of turbidity dissolved oxygen specific conductance temperature and pH The sampling methods for temperature and pH are specified in the Watershed Watch Water Chemistry Sampling Methods for Field Chemistry and Lab Analysis Appendix B The temperature must be recorded to an accuracy of 0 5 C and pH to an accuracy of 0 5 SU Instructions for the dissolved oxygen and specific conductivity methods are specified in the instruction manuals associated with the meter test kits see Appendix B Turbidity will be evaluated through a visual assessment and indicated as clear slightly turbid turbid or other Results will be recorded on the chain of custody Appendix A During the two wet weather sampling events collected by Third Rock Hydrolab multimeters will be used to record the dissolved oxygen specific conductance temperature and pH The procedures specified in In situ Water Quality Measurements and Meter Calibration Standard Operating Procedure KDOW 2009a will be used in these measurements Results will be recorded in the field notebook At one site per sampling event replicate measurements will be made on all in situ parameters except turbidity B3 Sample Handling and Custody Requirements The sample handling and custody procedures are compatible with the SOP Sample Control and Management KDOW 2009c B3 1 C
226. e sampling are established by the respective index periods for sampling In addition macroinvertebrate samples will not be collected during periods of excessively high or low flows or within two weeks of a known scouring flow event Other anomalous conditions or unusual land uses at the time of sampling will be recorded in the field notebook A7 2 4 Completeness Completeness is a measure of the amount of valid data needed to be obtained from a measurement system The completeness goals for each of the sampling types are summarized in Table 7 Dry weather is expected to produce no flow conditions at several sites during the sampling period TABLE 7 COMPLETENESS GOALS OF SAMPLING ACTIVITIES At each site a dry weather event and measurements from the first flush to past the peak flow during a wet weather event Minimum of 500 sites with at least one in each of the 24 stream segments Macroinvertebrate Collection All six sites Habitat Assessment Minimum of one site from each of the 24 stream segments Hydrogeomorphic Sampling All nine sites two surveys Five samples in 30 days for E coli At least two dry weather and two wet weather events at all sites no flow conditions are expected during dry ant hot weather conditions at several headwater sites Karst Hydrograph Characterization Conductivity Survey Grab sampling Wolf Run Watershed Page 26 of 67 Revision No 0 Based Plan Date April 11 20
227. e stock is located in the Room Temp Fridge ULR Low Standard 1 01 mg L Combine 1 00 mL of the 10 1 mg L High Standard with 9 0 mL Nanopure water HR High Standard 10 1 mg L Phosphate Standard solution 100 mg L to 200 mL volumetric flask Dilute to 200 mL with Nanopure water QA QC Requirements 10 1 10 2 10 3 A High Standard 10 1 mg L and a Low Standard 1 01 mg L must be run with every analytical run A total of 5 of all samples must be run in duplicate Data acceptance criteria 10 3 1 Analysis values for Standards must agree within 10 of the Standard s known value 10 3 2 Duplicate values must agree within 5 If these criteria are not met corrective action is indicated See Quality Assurance Program QAP Sec 15 Corrective Action Policies and Procedures 75 SOP TP LFUCG Laboratory Page 76 of 219 Revision Number 1 Last Revised 09 09 11 Expected Results 11 1 KPDES Permit Requirements 1 Town Branch Wastewater Treatment Plant has no effluent limitations on Total Phosphorus Plant effluent composite samples are analyzed daily Monthly and weekly averages are reported 2 West Hickman Wastewater Treatment Plant effluent limitations are a November 1 through April 30 a monthly average of 1 mg L and a weekly average of 2 mg L b May 1 through October 31 there are no effluent limitations on Total Phosphorus Plant effluent composite samples are analyzed daily Monthly and we
228. e the approximate spacing of verticals divide the stream width by the number of desired verticals Importantly the stream discharge computed using the average velocity in one vertical shall not exceed 10 of the total stream discharge Therefore it may be necessary to space verticals more closely together in areas that are deeper or that have a greater velocity than the majority of the stream Conversely the spacing of verticals may be farther apart in areas that are shallower or have lower velocity compared to the majority of the stream Uniform spacing across the tape measure will only be used if the stream is of relative uniform depth and velocity regimes Although vertical spacing can vary verticals will never be spaced less than 0 2 feet apart As a result of this minimum spacing small streams with a flowing width of less than 2 2 feet will have less than 12 verticals and can have as few as one vertical during very low stream flow A standard top setting wading rod will be used to measure water depth and confirm the proper location of the flow meter sensor within the water column The wading rod will be adjusted to the appropriate depth which is marked in 0 1 foot increments along the rod It Wolf Run Watershed Page 37 of 67 Revision No 0 Based Plan Date April 11 2011 is appropriate to further estimate depth to the 0 05 foot increment level despite the wading rod not being marked to this level When water depth is lt 2 5 feet v
229. ease Setting TDS Factor TDSTestrs only The TDSTestrs let you select a TDS factor of 0 4 to 1 0 1 Open battery compartment With meter on press the HOLD key then press the INC key INC key is inside battery compartment see diagram at left 2 Press the INC or DEC keys to adjust the TDS factor 3 After 3 seconds without a key press the dis play flashes 3 times then shows ENT Tester accepts TDS factor and returns to measure ment mode 4 Replace battery cap Changing Batteries 1 Open battery compartment lid end with lanyard loop 2 Remove old batteries replace with fresh ones Note polarity shown in battery compartment and in picture at right 3 Recalibrate after battery change Tester Maintenance e To improve performance clean the electrodes by rinsing them in alcohol for 10 15 minutes Remove white plastic cup insert to clean vis cous solutions e Replace all batteries if low battery indicator appears or if readings are faint or unstable e If you experience drift periodically let elec trode fully dry When you need a new electrode see Electrode Replacement at right Specifications Testr TDS Low TDS Hi EC Low 0 to 0 to 1990 10 00 1990 ppm ppt pS TDS Factor 0 4 to 1 0 selectable Calibration Standard Range Calibration 1 Point calibration range is 30 of factory default parameter ATC EC Hi 0 to 50 C 2 per C 0 to 50 C
230. eated must be delivered to the laboratory within six hours from the time of collection a Documenting changes in custody of the sample When the Supervising Sampler takes a sample directly to the laboratory she or he signs times and dates the Chain of Custody form in the left column when custody is relinquished to the laboratory The staff member of the laboratory who receives the sample similarly signs times and dates the form opposite the signature of the person relinquishing it Identical times and dates on the same line means the sample changed custody without an intermediate step which would disqualify the sample from regulatory use b Drop Off Centers Because of the vast number of Watershed sites sampled on the same day and the few number of receiving laboratories Drop Off Centers may be established if these criteria are met e The instructions that accompany sample bottles identify the person responsible for the drop off center and provide directions contact telephone number and specific times of operation when the responsible person will be available to accept samples and 10 e The center has sufficient refrigeration cooler space to immediately chill samples transferred from Volunteer Monitors coolers Cc Runners Runners may be designated to collect samples from Drop Off Centers or Volunteer Monitors in the field Sample runners are responsible for e Communicating with volunteers and drop off locations
231. eceseeeescecseeceeeseeeeeaeecaeees 18 A6 1 5 Hydrogeomorphic Assessment 0 ccccccecsseceseceseeeescecesecesecseeeeeaeecnseecsaeees 18 A6 1 6 Water Quality Monitoring ns 19 A6 2 Project Timetable nirna ir E e E E R TA 19 A7 Data Quality Objectives DQOs and Criteria for Measurement Data 22 Ad Data Quality ObJECtIVES nersini ces 22 A7 2 Data Quality Indira ini heen aa 24 TD Me PRC CIS ON en suas 24 PPI 2 TNC CME ACY r RE 23 ADO Representativeness A n dase a a ation 26 K TS EE SEEE EE S A EE 26 A7 2 5 Comparability eenen n e a ca ew hee E T a wettest 27 PGP DO Sensitivity senesaetudatax tea st vin EEE deed vente EEE wenden as 27 AS Training Requirements ccccsssccssssccssssccssscecssccecssscecssecesssecesssscesssseessanees 27 A9 Documentation and Records ccceeccesesseeseeseeeeecesecesecaeeeseeeeeeeeeaeceeeeneeeeeeeees 27 A9 1 Field Documentation and Records ooooocooccnoccnonoconncconccconoconn nono nonnnocono cano nonnnconnons 27 A9 2 Laboratory Documentation and Records oooconoccnocococcconcononconncconoconn cono nconccconacno 28 A9 3 Quality Documentation and Final ReportS ooonnocinccniccnoncnnonccnonoconocono nina ccnnncnos 29 SECTION B DATA GENERATION AND ACQUISITION cooooccoccciconocnconccnnccnnono 30 B1 Sampling Process Design cocci ed A 30 B1 1 Sampling Site and Reach LeGations s cssjccs ass xtssvesdchbestedessvesscesagtsestadertiaaedaases 30 B1 2 Sa
232. ecommendation for the use of HACH method 10360 Revision 1 1 January 2006 ATP Case N04 0013 Report on the Validation of Proposed EPA Method 360 3 Luminescence for the Measurement of Dissolved Oxygen in Water and Wastewater August 2004 HACH Company Loveland CO Lachat Micro Dist User Manual Method Cyanide in Waters MICRO DIST Cyanide 1 Lachat Instruments HACH Company Loveland CO Orion Research Incorporated Laboratory Products Group Standard Methods 2320 B APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 51 TB Laboratory QAP September 16 2009 Revision 1 Standard Methods 2340 C APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Standard Methods Part 2540 B Total Solids dried at 103 C to 105 C APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Standard Methods Part 2540 D Total Suspended Solids Dried at 103 C to 105 C APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21
233. ecreation swimming OR Ohio River NC No Criteria SCR Secondary Contact Recreation boating and fishing Source Division of Water Ambient Monitoring Database 1985 1994 4 Temperature In addition to having its own toxic effect temperature affects the solubility and in turn the toxicity of many other parameters Generally the solubility of solids increases with increasing temperature while gases tend to be more soluble in cold water Temperature is a factor in determining allowable limits for other parameters such as ammonia Methodology The simplest field method is to use a thermometer however electronic thermal sensing devices are available with continuous read outs Environmental Impact The Federal Water Pollution Control Administration 1967 referred to temperature as a catalyst a depressant an activator a restrictor a stimulator a controller a killer one of the most important and most influential water quality characteristics to life in water An important physical relationship exists between the amount of dissolved oxygen in a body of water and its temperature Simply put the warmer the water the less dissolved oxygen and vice versa Figure 2 shows the relationship Figure 2 Effect of Temperature on Dissolved Oxygen A 3 pa e i i For this reason heat or thermal 2 6 8 10 Dissolved Oxygen mg L pollution may be a problem especially in shallow slow moving
234. ective Action Policies and Procedures 12 SOP NH LFUCG Laboratory Page 13 of 219 Revision Number 1 Last Revised 09 09 10 Expected Results 10 1 KPDES Permit Requirements 1 Town Branch Wastewater Treatment Plant effluent limitations Weekly average 3 mg L May 1 October 31 Monthly average 2 mg L May 1 October 31 Weekly average 10 5 mg L November 1 April 30 Monthly average 7 mg L November April 30 2 West Hickman Wastewater Treatment Plant effluent limitations Weekly average 6 mg L May 1 October 31 Monthly average 4 mg L May 1 October 31 Weekly average 15 mg L November 1 April 30 Monthly average 10 mg L November 1 April 30 In the event that analysis results indicate values greater then KPDES permit requirements retest If the value indicated by the retest is greater than KPDES permit requirements Immediately notify the Plant Superintendent and the Laboratory Supervisor 10 2 Process Ranges Typical ammonia values vary a great deal throughout the wastewater treatment process depending on sample location and environmental conditions i e high rainfall events The following are typical Ammonia values found in process waters Raw Influent 0 mg L to 25 mg L Plant Effluent 0 mg L to 2 0 mg L 11 Data Analysis and Calculations 11 1 Concentrations are read directly from the DR5000 spectrophotometer Ensure that test results are corrected for volume dilutions 13
235. ed Time started Within 15 min limit Enter Date Volatile Acids Enter Date L 2 3 4 5 6 7 1 8 9 p m 1i 2 3 Log Number Run e O E A pr TE A A MA Standard gt Date Samples Collected __ ___ ___ fimeamiyisStartea too v VolumeofSampe m pro NE NormatityoftheNaon TT AR Volume of NaOH Used A A P RecoweryFactor Volatile Acid A N 60 000 V F nats S T Al ate Analysis Completed TE Make Dilutions for all sample with Total Alkalinity gt 225 mg L CaCO Total Alkalinity Control Limits are from 93 to 107 mg L on the 100mg L Standard Standards pH should be 4 41 0 05 after reagent addition d TOWN BRANCH amp WEST HICKMAN WASTEWATER TREATMENT PLANT Town Branch Laboratory Samples Nitrogen Ammonia ULR TNT 830 HR TNT 832 DR 5000 Nitrogen Ammonia Date Sunday October 18 2009 Reading Sample Dilution Date Sample Collected Time Analysis Started 2 g E z S ua U i 2321 2321 23146 23149 23153 23192 E 0 19 09 Low Standard 1 0 mg L 0 19 09 High Standard 10 0 mg L 10 18 09 TB Raw Influent Sun 10 18 09 TB Plant Effluent Sun 10 18 09 TB Creek Above Plant 10 18 09 23194 10 18 09 23137 10 17 09 TB Raw Influent Sat kac 23138 10 17 09 TB Plant Effluent Sat i AR E i a U na s AA U s
236. ed to be at or near method detection limits should be included Duplicates should also be collected where high concentrations are expected 1 Duplicate Samples Watershed Watch uses concurrent duplicate samples to assess variability in sample collection processing and analysis Supervising Samplers for the sites selected by the random selection process receive a pre marked duplicate sample container in addition to the pre marked sample containers with instructions for taking and submitting a duplicate sample All other procedures for samples are followed for Duplicate Samples 2 Field blanks Watershed Watch uses field blanks to assess for bias from contamination of the sample during any stage of sample collection processing and analysis Supervising Samplers for the sites selected by the random selection process receive a pre marked field blank container in addition to the pre marked sample container The Supervising Sampler is instructed to obtain bottled water in a food store and pour the amount required for a sample into the container pre marked for the field blank sample at the site and time the routine sample is taken All other procedures for samples are followed for field blanks An example of instructions to Supervising Samplers for taking field blanks may be found in Appendix G 12 Watershed Watch Chain of Custody Record Sample Stream Name Date sample taken Sampling Location correct or add location info if
237. efore and after filtration of a set of samples 2 Before any sample is filtered place a sterile filter in the filter holder unit 3 Add 50 mL peptone buffer to filter unit 4 Turn on vacuum and filter the buffer this will be the Before Blank 5 Remove and plate filter as indicated in Section 8 1 6 Proceed with sample filtration and plating 7 Runa Known Positive after all samples have been filtered See Section 8 3 8 Place a sterile filter in the filter holder unit 9 Add 50 mL peptone buffer to filter unit 10 Turn on vacuum and filter the buffer this will be the After Blank 11 Remove and plate filter as indicated in Section 8 1 12 Log results initials time and date in the Microbiology bench sheet Known Positive 1 2 3 4 5 6 After all samples have been filtered a Known Positive is filtered and plated to ensure growth Place a sterile filter in the filter holder unit Add 10 20 mL peptone buffer to filter unit then pipet 1 0 mL of mixed liquor or suitable sample with known fecal coliforms into filter unit Turn on vacuum and filter the sample this will be the Known Positive Remove and plate filter as indicated in Section 8 1 Log results initials time and date in the Microbiology bench sheet 48 SOP Fecal Coliform LFUCG Laboratory Page 49 of 219 Revision Number 3 Last Revised 09 09 8 4 Peptone Buffer Preparation 1 2 3 4 5 6 7 Measure 1 0 g Peptone powd
238. eionized water into a third container Rinse the electrode in the water rinse it in first container of standard then dip it into the second turn on the TDSTesir and allow the display to stabilize Using a small screwdriver adjust the trimmer located on the back of the unit until the display reads Me the same value as the standard Rinse the electrade in the tap Me or deionized water and proceed with testing TDS or CONDUCTIVITY TESTING Remove cap Press ON OFF button to tum on Dip the elecuode end into the test solution Allow time for the Automatic Temperature Compensation to correct the readings for solution temperature changes Note the full reading once the display stabilizes Press the ON OFF button to shut off Replace cap MAINTENANCE To improve performance clean the stainless steel electrodes by periodically rinsing them in alcohol for 10 14 minutes Replace ali 4 batteries if the display becomes faint or disappears or it the readings are unstable or never change CHANGING BATTERIES Flip up the battery compartment lid see box side panels Remove old batteries and replace with fresh ones noting polarity as shown in the battery compartment Note no battery connector wares to break SPECIFICATIONS MODELA MN i MN MN MN 19800 00 19800 10 19806 20 19800 30 TPSTostr 1 TDS Testy 2 TOSTestr 3 TDS Testr 4 Range G 19Xppm 10 10 00pnt O199uS 0 19 90m5 iGopm G30opt_ i ias
239. ekly averages are reported In the event that analysis results indicate values greater than the KPDES permit requirements retest If the value indicated by the retest is greater than KPDES permit requirements Immediately notify the Plant Superintendent and the Laboratory Supervisor 11 2 Process Ranges Typical phosphorus concentration values for plant influent vary primarily due to rainfall Within the treatment process phosphorus concentrations can vary due to microbiological processes involving the release and uptake of phosphorus forms Typical values for each plant are Town Branch Influent 4 mg L to 9 mg L Town Branch Effluent 2 mg L to 4 mg L West Hickman Influent 2 mg L to 12 mg L West Hickman Effluent lt 1 0 mg L 12 Data Analysis and Calculations 12 1 Concentration values are read directly from the DR5000 spectrophotometer 76 13 SOP TP LFUCG Laboratory Page 77 of 219 Revision Number 1 Last Revised 09 09 Bibliography 12 1 12 2 12 3 12 4 12 5 12 6 12 7 HACH DOC316 53 01124 Phosphorus Reactive Orthophosphate and Total Phosphorus TNTplus 843 HACH Company Loveland CO 2008 HACH DOC316 53 01125 Phosphorus Reactive Orthophosphate and Total Phosphorus TNTplus 844 HACH Company Loveland CO 2008 HACH DOC316 53 01126 Phosphorus Reactive Orthophosphate and Total Phosphorus TNTplus 845 HACH Company Loveland CO 2008 HACH DRS5000 Procedure Manual HACH Company
240. elating the number of times each value is obtained to each value Values are generally listed in ascending order on X axis and number of times the value occurs on Y axis Gaussian distribution Normal distribution curve when data from biologic measurements are plotted according to their frequencies a bell shaped curve is usually obtained In all distributions 2 SD from the mean represents 95 45 of the population and 3 SD 99 73 1 SD 68 Grab A single sample of wastewater taken at either a set time or flow Gravimetric A means of measuring unknown concentration of a water quality indicator by weighing 44 TB Laboratory QAP September 16 2009 Revision 1 Halogenated Organics A general term for organic molecules that contain one or more halogen atoms Halogens Chemical elements either individually or collectively composing group VIIB of the periodic table i e Fluorine Chlorine Bromine Iodine and Astatine Hardness A characteristic of water imparted primarily by salts of calcium and magnesium such as bicarbonates carbonates sulfates chlorides and nitrates that causes curdling and increased consumption of soap deposition of scale in boilers damage in some industrial processes and sometimes objectionable taste It may be determined by a standard laboratory titration procedure or computed from the amounts of calcium and magnesium expressed as equivalent calcium carbonate Hepatotoxic Causing liver d
241. elocity is measured at 0 6 of the depth below the water surface at each vertical A standard top setting wading rod will automatically adjust the probe to this height When water depth is gt 2 5 feet discharge is measured at 0 2 and 0 8 of the total depth below the water s surface at each vertical To set the rod at the 0 2 depth position the setting rod at half the water depth To set the rod at the 0 8 depth position the setting rod at twice the water depth An average of these two readings will be used as the average velocity for the vertical The wading rod will be held perpendicular to the water surface and the instrument will be parallel to the stream flow The individual making the measurements will stand at least 1 5 feet away from the wading rod and 3 inches downstream of the tagline in a way that alters the stream flow as little as possible Rocks logs or other obstructions will not be moved during the measurement process as this may cause the stream flow to change in an area of the stream where velocity has already been measured Once the process of measuring velocity has begun the stream will not be altered Record the location of the starting edge on the field data sheet LEW or REW If the starting edge has a water depth record this No velocity measurements will be made at the starting or ending edges Facing upstream place the wading rod behind the tape measure at each vertical and record the location and stream depth Velo
242. elometer GPS Laser level amp tripod 100ft amp SOft tapes RiverMorph on Rugged Reader GPS Site Characterization Form 0 75 inch rebar Hammer Tape measure Surveying rod Field notebook Water Quality Monitoring and E coli Geomean Sampling Field Measurements EC Conductivity PockeTesters Dissolved Oxygen Water Quality Test Kit LaMotte Code 7414 2 pH Wide Range Indicator Kits LaMotte P 5085 and P 5100 Armored Thermometers 5 to 45 C in 0 5 C increments All Sampling Sample coolers Ice Plastic food storage bags Sample jars and preservatives Powderless latex or nitrile gloves Chain of custody Permanent marker Clear masking tape Blue or black ink pen Flow measurement Marsh McBirney Flo Mate Portable Flowmeter or equivalent Stopwatch Tape measure 100 feet in 1 10ft increments Top setting wading rod Five gallon bucket Field Notebook Field Filtration 47mm magnetic filter funnel 1L Nalgene flask Teflon or Tygon tubing Forceps 0 45um sterile membrane filters Deionized water Wolf Run Watershed Based Plan Page 16 of 67 Revision No 0 Date April 11 2011 A6 1 1 Karst Hydrograph Characterization To determine the influence of the karst system on the discharge and the nature of the stream hydrograph simultaneous gaging of the three affected tributaries and a major sinkhole will be performed during base flow conditions and during a wet weather event Temporary water level gages pressure
243. ent Program Coordination Manage the LFUCGs laboratories for testing the quality of waters released from three different wastewater treatment plants Maintain and evaluate data on these plants Create and modify programs to sort store and calculate data monitor trends and generate graphs on personal computer Help other departments set up programs to use data provided by the laboratory Work with operations staff of three plants and our engineers to help them use the data provided by the laboratory Make suggestions as to how the data could be used to deal with operational problems TB Laboratory QAP Appendix C September 16 2009 Revision 1 Sample Preparation Testing and Analysis Check and evaluate all lab data Run standard to make calibration curve to establish quality of the test Train technicians to run analyses and supervise the procedures Determine how samples are to be prepared for analysis Supervise the sample preparation Determine all laboratory analysis procedures to be used in the analysis of samples Train the lab personnel on how to use these procedures and supervise their use Set up and run sophisticated bacteriology chemical and microbiology analyses that can only be run by the laboratory supervisor record and report the data Miscellaneous Travels to West Hickman WWTP Laboratory to calibrate equipment and or run analyses on request Maintains special laboratory programs such as safety quali
244. equired for analysis will vary with sample strength and chosen increment value During analysis the display graphs the progress of the titration Upon completion the unit will display the resulting concentration value and calculated confidence limits press OK to accept results 12 Record the results on the Total Chlorine Residual bench sheet In the case of the PTE sample also log in the provided location the time sampled time received and time analysis began Note If sample hold time time sampled to time analysis begins exceeds 15 minutes the analysis is void and must be rerun beginning with resampling 13 Select END if done with analysis or Continue to proceed to the next sample to be analyzed Note More detailed general information on the AutoCAT unit can be found in the operator s manual with details on the Forward Amperometric procedure starting on page 101 The manual is located on the shelf adjacent to the AutoCAT unit 24 8 2 8 3 SOP Residual Chlorine LFUCG Laboratory Page 25 of 219 Revision Number 4 Last Revised 09 09 Chlorine Standard Analysis 1 Obtain a Chlorine Standard Solution 25 30 mg L ampoule from Chemical Storage fridge 2 Carefully break top off ampoule 3 Pipette 1 0 mL of standard into 1000 mL volumetric flask 4 Bring to 1000 mL with Nanopure water 5 Measure 200 mL of standard solution into beaker with stir bar 6 Run titration as indicated in Section 8
245. er into 1L volumetric flask Bring to volume with Nanopure water Mix well Pour Peptone buffer into Nalgene autoclavable squeeze bottle Take a sample of the buffer and measure pH it should be 7 00 0 1 Loosely screw caps dispensers onto squeeze bottles Autoclave Peptone buffer solutions Allow to cool then transfer squeeze bottles to Micro fridge 8 5 Helpful Hints 1 2 3 4 If the bacterial density of the sample is unknown filter and plate out several volumes or dilutions in order to achieve a countable density The volumes and or dilutions should be expected to yield a countable membrane In addition select two additional quantities representing one tenth and ten times this volume respectively Separate filter holder units may be required during a set of samples These will be indicated in the bench sheet Do not use damaged or bent membrane filters Rinse the filter unit thoroughly with Peptone buffer to avoid cross contamination QA QC Requirements 9 1 Before and After Blanks must be run with each set of samples tested 9 2 One duplicate per test series must be run 9 3 One Known positive must be run per test series 49 10 11 12 SOP Fecal Coliform LFUCG Laboratory Page 50 of 219 Revision Number 3 Last Revised 09 09 Expected Results 10 1 KPDES Permit Requirements 200 CFU 100 mL for Monthly geometric mean GED 400 CFU 100 mL for Maximum Weekly GED In the event t
246. erating Procedure Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky DOWSOP03019 KDOW 2009b Sampling the Surface Water Quality in Lotic Systems Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky DOWSOP03015 LaMotte Dissolved Oxygen Water Quality Test Kit Instruction Manual Code 7414 5860 LaMotte Company Chestertown Maryland www lamotte com Price David J 2009 Quality Assurance Plan QAP and Standard Operating Procedures SOPs Lexington Fayette Urban County Government Division of Water Quality Town Branch Laboratory Kentucky Geological Survey Standard Operating Procedures See Appendix B Wolf Run Watershed Based Plan Revision No 0 Date April 11 2011 Page 23 of 67 A7 2 Data Quality Indicators When measurement performance or acceptance criteria can be stated in quantitative terms they are called data quality indicators DQI The quality of field and analytical data is most often assessed in terms of the DQIs including precision accuracy bias representativeness comparability completeness and sensitivity A7 2 1 Precision Precision is the measure of agreement among repeated measurements of the same property under identical or near identical conditions It is usually calculated as a range standard deviation or relative percent difference RPD Relative percent difference will be the primary measure of precision for laborat
247. erature C Is Difference Less Than 0 2 Y or N Dissolved Oxygen Calibration Point Po Calibrated By Dissolved Oxygen ono d gt e d os do oa d A e es d 9 d o u Tog Number pa aime SS Date Samples Collected EE Ea 10 19 09 Time Analysis Started Dissolved Oxygen Reading mg L Analyst Date Analysis Completed 10 19 09 10 19 09 10 19 09 PTE Dissolved Oxygen QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS Time sampled Within 15 min limit Time received Presevation None required Analyze Immediately Time started KPDES Permit Limits on Plant Effluent 7 0 mg L is the Lowest Dissolved Oxygen we can have on any given sample L d Microbiology TOWN BRANCH amp WEST HICKMAN WASTEWATER TREATMENT PLANT Town Branch Laboratory Total Coliforms Method EPA 600 8 78 017 Microbiological Methods for Monitoring the Environment Water and Wastes page 108 Fecal Coliforms Method EPA 600 8 78 017 Microbiological Methods for Monitoring the Environment Water and Wastes page 124 Fecal Streptococci Method EPA 600 8 78 017 Microbiological Methods for Monitoring the Environment Water and Wastes page 136 1 2 3 5 7 8 9 10 11 12 13 14 Log Number Blank 23177 Separate Known Blank Sample Name Before TB PTE TB PTE TB PTE TB A Crk Filter WHPTE WHPTE Positive Analysis Sample Volume Colonies Counted Colo
248. erile glass or plastic containers If chlorine is in the sample containers should be treated with 4 drops of 10 Sodium thiosulfate before autoclaving Run test immediately after sampling or preserve sample at 4 C for a maximum of 6 hours 44 SOP Fecal Coliform LFUCG Laboratory Page 45 of 219 Revision Number 3 Last Revised 09 09 Reagents 5 1 Peptone powder 5 2 Peptone buffer solution pH 7 00 0 1 stored at 4 C 5 3 m FC media with rosolic acid for fecal coliforms stored at 4 C 5 4 Sodium thiosulfate 10 solution 5 5 Lysol disinfectant 20 solution Equipment amp Lab Ware 6 1 Vacuum flask 6 2 Millipore single use 47 mm Petri dishes with pads 6 3 Millipore sterilized 47 mm filter 6 4 Forceps 6 5 4 5 X 9 inch sterile sampling bags 6 6 Bunsen burner and striker 6 7 Pipettes and sterile tips 6 8 Sterilized filter holder plastic or glass 6 9 Gable topped water bath at 44 5 C 0 2 C 6 10 Thermometer 6 11 ASTM Thermometer 6 12 Tower Steam Indicator Strips 6 13 ODO Clave Heat Activated Deodorant Pads 6 14 Autoclavable Biohazard waste bags and deposit box 6 15 Autoclave 6 16 Sterile blue sheets 6 17 Indicator tape 6 18 Autoclavable Nalgene squeeze bottles for peptone Interferences 7 1 Bacteria from the surrounding environment 7 2 Cross contamination from one sample to the next 7 3 Lack of aseptic techniques 45 Procedures 8 1 Steps 1 2 3 4 5 6 7 8
249. ers will be installed at each of the six gaging stations These gages will be installed inside PVC pipe attached to a firmly anchored stake or permanent instream structure with an elbow facing downstream to eliminate bias from velocity based pressures If water levels become elevated enough to make streams unwadeable and flow measurements unfeasible the water level recorded by the loggers may be useful in estimating stream discharge The water level recorded by the loggers could be used along with stream cross section measurements and an estimation of surface velocity i e float method to estimate discharge during any un wadeable parts of the wet event The discharge data collected in this study will be used to improve modeling of the watershed discharge based on the USGS gage and land use to incorporate the redirection of the flow through the karst system The results will be summarized in the Karst Hydrograph Characterization in the Wolf Run Watershed final report due by May 31 2012 B2 2 2 Conductivity Survey Trained volunteer samplers under the direction of the FOWR Sampling Coordinator will conduct the conductivity survey The Sampling Coordinator will schedule the survey such that flow conditions at the USGS gage at the mouth of Wolf Run are between 0 5 and 5 cfs In order to limit the temporal variations in the conductivity levels efforts will be made to conduct the entire survey within a one week period unless interrupted by
250. ersees data collection planning and reviews data Lisa Hicks KDOW KDOW QA Officer Administratively oversees QAPP conditions may assist in review of data Susan Bush LFUCG Grantee Project Oversight of project Manager Gerry Fister Third Rock Project scheduling and coordination to meet time line and budget goals Development of the QAPP ensure QAPP compliance conduct audits review and approve all data generated preparation of QA reports Coordination of water quality sample collection events with volunteer staff bottle preparation and labeling laboratory communication on hold times and data results Coordination of volunteer sampling activities training volunteers per QAPP specifications Chemistry laboratory analysis for water quality samples Project Manager Steve Evans Third Rock QA Manager Marcia Wooton Third Rock Sampling Coordinator Ken Cooke Friends of Wolf Run David Price LFUCG Jason Backus Kentucky Geological Survey Volunteer Sampling Coordinator Laboratory Director Laboratory Services Manager Chemistry laboratory analysis for water quality samples Oversee and conduct field biological sampling biological data review identification of benthic samples oversee macroinvertebrate quality assurance Macroinvertebrate Laboratory Chief Taxonomist Bert Remley Third Rock A5 Project Definition Background Wolf Run was first listed a
251. ery ten samples the following should be included a 1 DI water blank b 1 Duplicate of any one sample c 1 Quality Control sample calibration check A C Calibration and Sample Analysis Say OV Set up the instrument with proper operating parameters established in the operation condition procedure The instrument must be allowed to become thermally stable before proceeding This usually takes 1 hour from the point on initial degassing to the stabilization of the baseline conductivity To run samples on the Dionex Ion Chromatography System a Make a run schedule on the PeakNet Software Section labeled SEQUENCE b Double click the mouse on the SYS 2 to display the Scheduler Area The name of the calibration standards must be entered under the sample name section as Standard 1 Standard 2 and Standard 3 Note Level must be changed to the corresponding standard level or the calibration will be in error Example Standard 1 Level 1 Standard 5 Level 5 c Next enter QC blanks QC samples duplicates QC and blanks in that order d Under sample type click on either Calibration Standard or Sample depending on what is being run e Under the Method section the method name must be entered To do so double click on the highlighted area under Method scroll through the list of methods and double click on the method of interest f Next under the Data File section enter the name of the data file Finally in th
252. es Preserve the sample with 1 25 mL of 12 5N NaOH for analysis within 14 days of collection Reagents 5 1 CyaniVer 3 CyaniVer 4 and CyaniVer 5 reagent powder pillows 5 2 Releasing agent 7 11M sulfuric acid 0 79M magnesium chloride solution 5 3 Trapping solution 0 950M standardized NaOH 54 2 5N HCl 30 SOP Total Cyanide LFUCG Laboratory Page 31 of 219 Revision Number 3 Last Revised 09 09 Equipment amp Lab Ware 6 1 Lachat Micro Dist heating block 6 2 Lachat Micro Dist collector tubes membranes and caps 6 3 Seal press 6 4 1 inch sample cells for as many sample as being analyzed 6 5 Fixed 0 580 mL pipette and tip 6 6 Adjustable 3 00 mL pipette and tip 6 7 Squirt bottle with Nanopure water 6 8 0 75 mL and 1 59 mL repipetor bottles 6 9 Spec Color Standards kit 6 10 HACH DR 4000 1 inch Cell Adapter 6 11 HACH DR 4000 Spectrophotometer Interferences 7 1 Chlorine 7 2 Metals 7 3 Oxidizing agents 74 Reducing agents 7 5 Turbidity Procedures 8 1 Steps 8 1 1 Distillation 1 Allow Micro Dist heater block to warm up to 120 C 2 Add 1 59 mL of trapping solution in each collector tube 3 Cap tube with membrane 4 Add 6 mL of sample in sample tube and add 0 75 mL releasing agent 0 95M NaOH 5 Immediately place the sample tube in the seal press Seal the collector tube to the sample tube using the pressing motion of the seal press 6 Place tubes on the preheated block and set timer for 30 minutes
253. es oximes semi carbazones and some refractory tertiary amines Total Kjeldahl is defined as the sum of free ammonia an organic NHa 2S 4 under the conditions of digestion Nitrogen Organic Nitrogen chemically bound in organic molecules such as proteins amines and amino acids Nitrogen Organic Kjeldahl Defined as the difference obtained by subtracting the free ammonia value of Nitrogen Ammonia from the Total Kjeldahl Nitrogen value This may be determined directly by removal of ammonia before digestion Nitrogenous Oxygen A quantitative measure of the amount of oxygen required for the Demand NOD biological oxidation of nitrogenous material such as ammonia nitrogen and organic carbonaceous oxygen demand has been satisfied Non Filterable Residue Suspended solids Non Volatile Residue Fixed solids 46 TB Laboratory QAP September 16 2009 Revision 1 Oil and Grease In wastewater a group of substances including fats waxes free fatty acids calcium and magnesium soaps mineral oils and certain other non fatty materials The type of solvent and method used for extraction should be stated for quantization The method includes the measurement of hexane extractable matter from waters industrial wastes and sewages It is applicable to the determination of relatively non volatile hydrocarbons animal fats and waxes grease and other types of greasy oily matters The method is not applicable to measurement of light hydroc
254. es are removed from the eluent line to the pumps Press OFF ON on the pump to turn it off Turn the valve on the Priming Block clockwise remove the syringe and expel the air bubbles from the syringe Reinsert the syringe filled with eluent into the Priming Block Open the valve on the Pressure Transducer and the valve on the Priming Block with the eluent filled syringe still attached This is accomplished by turning both counterclockwise Press PRIME on the pump and push the contents of the syringe into the Priming Block After the eluent has been injected into the Priming Block press OFF ON to turn the prime pump off and to close the valves on the Pressure Transducer and Priming Block Remove the syringe from the Priming Block Scroll to the mL min on the screen for the pump For the GP50 type 2 mL min and press ENTER For the IP25 type 1 2 mL min and press ENTER Press OFF ON to turn on the pump at the appropriate rate The pressure should soon stabilize between both pumpheads after two minutes of pumping time If the pressure between pumpheads has a difference gt 20 psi then shut down the pump and repeat steps 2 14 to remove air bubbles and prime the pumps Once the pump has a pumping pressure difference between pumpheads of lt 20 psi then go to the computer and enter PeakNet 17 On the computer turn on the Chromeleon 6 8 browser then choose System 2 all other anions including Bromide and TKN 18 Go to last run se
255. es shall be delivered to Third Rock for identification according to Laboratory Procedures for Macroinvertebrate Processing and Taxonomic Identification and Reporting KDOW 2009b After identification macroinvertebrate sampling results Wolf Run Watershed Page 43 of 67 Revision No 0 Based Plan Date April 11 2011 will be evaluated through calculation of several community metrics prescribed by KDOW 2008 Community metrics include taxa richness EPT mayfly stonefly and caddisfly richness total number of individuals modified percent EPT individuals modified Hilsenhoff biotic index mHBI percent Ephemeroptera percent primary clingers and percent Chironomidae plus Oligochaeta aquatic worms Results of community metrics at each station will be combined to compute a Macroinvertebrate Bioassessment Index MBI score ranging from 0 worst to 100 best MBI scores will be compared to scoring criteria developed by KDOW to arrive at water quality ratings of Very Poor Poor Fair Good or Excellent For wadeable streams watersheds greater than 5 mi of the Bluegrass Bioregion a MBI score below 20 is Very Poor from 21 to 40 is Poor from 41 to 60 is Fair from 61 to 79 is Good and greater than 70 is Excellent For headwater streams watersheds less than 5 mi of the Bluegrass Bioregion a MBI score below 18 is Very Poor from 19 to 38 is Poor from 39 to 50 is Fair from 51 to 57 is Good and greater than 58 is Excellent KDOW 2008
256. es should be collected in glass or plastic bottles that have been thoroughly cleaned and rinsed with reagent water The volume collected should be sufficient to ensure a representative sample and allow for replicate analysis if required Most analytes have a 28 day holding time with no preservative and cooled to 4 C Nitrite nitrate and orthophosphate have a holding time of 48 hours Combined nitrate nitrite samples preserved with H2SO to a pH lt 2 can be held for 28 days however pH lt 2 and pH gt 12 can be harmful to the columns It is recommended that the pH be adjusted to pH gt 2 and pH lt 12 just prior to analysis Note Prior to analysis the refrigerated samples should be allowed to equilibrate to room temperature for a stable analysis 2 Apparatus Dionex DX500 Dionex CD20 Conductivity Detector Dionex GP50 Gradient Pump Dionex Eluent Organizer Dionex AS40 Automated Sampler Dionex ASRS Ultra Self Regenerating Suppressor Dionex Ionpac Guard Column AG4A AG9A or AGI4A Dionex Ionpac Analytical Column AS4A AS9A or AS14A Dionex Chromeleon 6 8 Software Package Dionex 5 mL Sample Polyvials and Filter Caps 2 L Regenerant Bottles 5 mL Adjustable Pipettor and Pipettor Tips I mL Adjustable Pipettor and Pipettor Tips A Supply of Volumetric Flasks ranging in size from 25 mL to 2 L A Supply of 45 micrometer pore size Cellulose Acetate Filtration Membranes A Supply of 25x150 mm Test Tubes Test Tube Racks for the above 25x1
257. es to a very titration tube cap pale yellow Gently swirl the tube during the tiration to mix the contents Carefully remove the Add 8 drops of Titrator and cap Do Starch Indicator not to disturb the Solution Titrator plunger 4170WT The sample should turn blue Continue I titrating until the blue color Cap the titration tube Insert the tip of disappears and the Titrator into the the solution opening of the becomes titration tube cap colorless A I H Read the test result directly from the scale where the large ring on the Titrator meets the Titrator barrel Record as ppm Dissolved Oxygen Each minor division on the Titrator scale equals 0 2 ppm ETTET Z TEST PROCEDURE If the plunger ring reaches the bottom line on the scale 10 ppm before the endpoint color change occurs refill the Titrator and continue the titration Include the value of the original amount of reagent dispensed 10 ppm when recording the test result When testing is complete discard titrating solution in Titrator Rinse Titrator and titration tube thoroughly DO NOT remove plunger or adapter tip EPA COMPLIANCE To qualify as an EPA accepted test and to achieve the greatest accuracy the Sodium Thiosulfate Solution 0 025N 4169 must be standardized daily This procedure follows Standard Methods for the Examination of Water and Wastewater Number
258. es will be sampled in order to obtain three 3 replicates in each substrate type where available silt sand and fine gravel This sub habitat will be sampled for both headwater and wadeable sites Aufwuchs Sample Small invertebrates associated with this habitat will be obtained by washing a small amount of rocks sticks leaves filamentous algae and moss into a medium sized bucket half filled with water The material will then be elutriated and sieved with the nitrex sampler mesh Three replicates will be conducted This sub habitat will be sampled only for wadeable sites Rock Picking Benthic macroinvertebrates will be picked from 15 rocks large cobble small boulders 5 each from riffle run and pool in wadeable streams and 5 small boulders from pools in headwater streams Selected rocks will be washed in a bucket half filled with water and then carefully inspected to remove organisms Wood Sample For wadeable streams pieces of submerged wood ranging from roughly 3 to 6 meters 10 to 20 linear feet and ranging from 5 15 cm 2 6 inches in diameter will be individually rinsed into the wash bucket For headwater streams only 2 linear meters will be sampled Pieces of wood will be inspected for burrowers and crevice dwellers and will be removed with fine tipped forceps Large diameter well aged logs will be inspected and handpicked with fine tipped forceps B2 2 3 3 Macroinvertebrate Identification and Analysis Macroinvertebrate sampl
259. ete plan for achieving all project data quality objectives However effective communication is essential to ensure that all parties properly implement the plan Any project related quality feedback questions or concerns should be communicated to the project administrator or quality manager to facilitate appropriate analysis and resolution The implementation of the monitoring plan requires the effective operation of the project team Figure A 1 Wolf Run Watershed Monitoring Organizational Chart identifies the parties that comprise the Project Team and the lines of authority and communication under which this team operates The specific roles and responsibilities of each key party are documented in Table 1 FIGURE 1 WOLF RUN WATERSHED MONITORING ORGANIZATION CHART KDOW KDOW QA Officer Project Manager Lisa Hicks Brooke Shireman LFUCG Grantee P roject Manager Susan Bush Third Rock Third Rock Project Manager QA Manager Gerry Fister Steve Evans Friends of Wolf Run Third Rock i Third 7 l LFUCG n nade Survey acroinvertebrate aboratory Services Laboratory Laboratory Director Manager David Price Bert R emley J ason Backus Sampling C oordinator Sampling Coordinator Ken Cooke Marcia Wooton Wolf Run Watershed Page 10 of 67 Revision No 0 Based Plan Date April 11 2011 TABLE 1 PROJECT ROLES AND RESPONSIBILITIES Brooke Shireman KDOW Project Title KDOW Project Manager Responsibility Administratively ov
260. etic acid solution 2 Add 50 mL of prepared acetic acid solution to 1 L volumetric flask and bring to 1 L with Nanopure water final acetic acid concentration 100 mg L 3 Measure 250 mL of diluted acetic acid solution and distill as shown in Section 8 1 4 Titrate drop wise with 0 1 N Sodium Hydroxide NaOH using the Brand Digital Buret II until first persistent pink color is obtained 5 Calculations a volume of NaOH required 0 1N 60000 250 mL Recovery factor f a b where b 100 mg L Helpful Hints 1 If there is no color change it means no Sulfuric acid was added QA QC Requirements 9 1 None required Expected Results 10 1 KPDES Permit Requirements 1 None required 10 2 Process Ranges 1 Town Branch Digesters ranges are 35 73 mg L 2 If volatile acids ratio is high for plant operations run analysis again Data Analysis and Calculations 11 1 mg volatile acids as acetic acid L mL NaOH 0 1N 60 000 mL sample f Where f recovery factor 92 SOP Volatile Acids LFUCG Laboratory Page 93 of 219 Revision Number 3 Last Revised 09 09 12 Bibliography 12 1 12 2 Standard Methods Part 5560 C Distillation Method APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 HACH Water Analysis Handbook Method 8291 Volat
261. evision Number 3 Last Revised 09 09 pH Electrometric EPA Method 150 1 pH Issued 1971 Editorial revision 1978 and 1982 Scope Significance to Process and Application 1 1 At a given temperature the intensity of the acidic or basic character of a solution is indicated by a pH or hydrogen ion activity 1 2 ApH meter is accurate and reproducible to 0 1 pH unit with a range of 0 to 14 and equipped with a temperature compensation adjustment Summary of Method 2 1 Executive Summary The pH of a sample is determined electrometrically using either a glass electrode in combination with a reference potential or a combination electrode 2 2 Discussion There is no color change during analysis pH stands for power of hydrogen a measure of hydrogen ion concentration in solution Health amp Safety Precautions 3 1 Watch out for broken glass from beakers and cylinders 3 2 Wastewater samples should be considered potentially hazardous Use proper personal protective equipment Sample Handling and Preservation 4 1 Samples should be analyzed as soon as possible within a 15 minute time window 4 2 Sample containers should be filled completely and kept sealed prior to analysis Reagents 5 1 Buffer Solution pH 4 00 color coded red 5 2 Buffer Solution pH 7 00 color coded yellow 5 3 Buffer Solution pH 10 00 color coded blue 5 4 Buffer Solution pH 6 86 5 5 Nanopure Grade Laboratory Water 5 6 Reference Electrode Fil
262. f Reagent B into the cooled vial Immediately close the Reagent B container Screw a grey DosiCap C onto the vial Invert the capped vial 2 3 times to dissolve the reagent in the DosiCap Wait 10 minutes When the timer expires invert the vial again 2 3 times Clean the vial with a Kim Wipe and insert it into the DR5000 cell holder The instrument reads the barcode then selects and performs the correct test Results are in mg L PO No instrument Zero is required Note and record the indicated values on the bench sheet 8 2 TNTplus 843 Reactive Phosphorous LR 0 15 4 50 mg L PO 1 2 3 4 Carefully pipet 2 0 mL of sample into the vial Pipet 0 2 mL 200 uL of Reagent B into the vial Immediately close the Reagent B container Screw a grey DosiCap C onto the vial Invert the capped vial 2 3 times to dissolve the reagent in the DosiCap 71 8 3 8 4 5 6 7 8 SOP TP LFUCG Laboratory Page 72 of 219 Revision Number 1 Last Revised 09 09 Wait 10 minutes When the timer expires invert the vial again 2 3 times Clean the outside of the vial with a Kim Wipe and insert it into the DR5000 cell holder The instrument reads the barcode then selects and performs the correct test Results are in mg L PO4 No instrument Zero is required Note and record the indicated values on the bench sheet TNTplus 844 Total Phosphorous LR HR 0 5 5 0 mg L PO P 1 2 3 4 5 6 7 8 9 10 11
263. f blank B2 initial DO reading of blank D initial DO reading of sample D2 5 day DO reading of sample S volume of seed used in blank P volume of seed per BOD sample bottle V volume of sample in BOD bottle Then by Calculation B B2 depletion of blank D D2 depletion of sample B B2 S DO used ml of seed F seed correction B B2 S P C D D2 F depletion corrected for seed BOD or CBOD C 300 V 20 SOP CBOD LFUCG Laboratory Page 21 of 219 Revision Number 5 Last Revised 09 09 12 Bibliography 12 1 U S EPA Method 405 1 Biochemical Oxygen Demand 5 Days 20 C Issued 1971 Editorial revision 1974 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 12 2 Standard Methods 5210 A and 5210 B Biochemical Oxygen Demand BOD APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 21 1 SOP Residual Chlorine LFUCG Laboratory Page 22 of 219 Revision Number 4 Last Revised 09 09 Total Residual Chlorine Analysis HACH AutoCAT 9000 Total Chlorine Amperometric Forward Titration procedure equivalent to EPA Method 330 3 Chlorine Total Residual Titrimetric Amperometric Issued 1978 Standard Meth
264. f oxygen that is dissolved in a water sample 1 2 This method is recommended for samples containing intense color or turbidity which interferes with the Winkler method 1 3 This method is recommended for work in the field as the equipment is portable allowing hold times to be minimized 1 4 KPDES Permit Limits on Plant Effluent Required a minimum of 7 0 mg L 1 5 Dissolved Oxygen concentration levels are very important in both process and plant effluents In process dissolved oxygen is required by various organisms and the plant effluent dissolved oxygen levels must be conducive to the receiving environment and within permit limits See Section 10 1 Summary of Method 2 1 Executive Summary Dissolved Oxygen is measured directly by a HACH model HQ40d portable meter and HACH model LDO101 rugged field dissolved oxygen probe After the meter indicates a stable reading the operator analyst records the value 2 2 Discussion The HACH LDO system uses a sensor coated with a luminescent material Blue light from an LED is transmitted onto the sensor surface exciting the luminescent material which then emits red light as it relaxes The presence of DO in the process shortens the time it takes for the red light to be emitted By measuring the time lapse between when the blue light was transmitted and the red light is emitted a correlation is made to the concentration of DO in the effluent or other solution Between measurements a red LED is used a
265. f sample into the vial Immediately proceed to step 3 Flip the DosiCap Zip over so that the reagent side faces the vial Screw the cap tightly onto the vial Shake the capped vial 2 3 times to dissolve the reagent in the cap Verify that the reagent has dissolved by looking down through the open end of the DosiCap Zip Wait 15 minutes After 15 minutes invert the sample an additional 2 3 times to mix The color remains constant for an additional 15 minutes after the timer expires Thoroughly clean the outside of the vial with a Kim wipe Insert the prepared vial into the DR5000 cell holder Slide the lid closed The instrument reads the barcode then selects and performs the correct test Results are in mg L NH3 N 10 7 3 7 4 7 5 SOP NH LFUCG Laboratory Page 11 of 219 Revision Number 1 Last Revised 09 09 TNT 832 HR 2 to 47 mg L NH N 1 Carefully remove the protective foil lid from the DosiCap Zip Unscrew the cap from the vial 2 Carefully pipet 0 2 mL 200 uL of sample into the vial Immediately proceed to step 3 3 Flip the DosiCap Zip over so that the reagent side faces the vial Screw the cap tightly onto the vial 4 Shake the capped vial 2 3 times to dissolve the reagent in the cap Verify that the reagent has dissolved by looking down through the open end of the DosiCap Zip 5 Wait 15 minutes 6 After 15 minutes invert the sample an additional 2 3 times to mix 7 The color remains c
266. fied Acetic Acid Both reagents are located adjacent to the AutoCAT unit 5 3 Phenylarsine Oxide Standard Solution 0 00564 N 5 4 Chlorine Standard Solution 25 30 mg L as Cly Equipment amp Lab Ware 6 1 HACH AutoCAT 9000 Chlorine Amperometric Titrator 6 2 Beakers 250 mL 6 3 Graduated Cylinders 250 mL 6 4 1 mL fixed volume Finnpipette and 1 mL tips 6 5 Stirring bars Interferences 7 1 Accurate determinations of free chlorine cannot be made in the presence of Nitrogen trichloride or Chlorine dioxide Td Some organic chloramines can also interfere 13 Free halogens other than chlorine also will titrate as free chlorine 7 4 Interference from copper has been noted in samples taken from copper pipe or after heavy copper sulfate treatment of reservoirs 7 5 Contamination of probe by metal ions such as copper silver iron interfere with amperometric titrations Fouled electrodes will not produce sharp endpoints 13 SOP WH Residual Chlorine West Hickman WWTP Laboratory Page 14 of 219 Revision Number 4 Last Revised 09 09 7 6 Extended sample hold times volatilization from mechanical agitation and exposure to various light sources can affect results 7 7 At very low temperatures there is slow response of cell and longer time is required but precision is not compromised Procedures 8 1 Steps 1 Prior to testing pre rinse all glassware and stir bars with sample Do not rinse with Nanopure once pre rinsed 2 Using
267. flow Stream gt Karst Flow Karst Basin Wolf Run Watershed i E a Adjoining Karst Basin D yw a Lo 13 S a i a Al Sl N A N a T x E E g N gt en D 2 G E Exhibits QAPP_Exhibit_2 WolfRun Mapping GIS QAPP_ KY 10 030_LFUCG Exhibit 2 Karst System Hydraulic Monitoring Wolf Run Watershed Based Plan Lexington Fayette County Kentucky Map Document P Project_Files Kentucky TABLE 3 SAMPLING EQUIPMENT SUMMARY Monitoring Activit Equipment Karst hydrograph characterization Marsh McBirney Flo Mate Portable Flowmeter Stopwatch Tape measure 100 feet in 1 10ft increments Top setting wading rod Five gallon bucket Field Notebook 5 Level TROLL 1 Baro TROLL RuggedReader and communication cables PVC pipe elbow and caps Steel cable Lap top computer Pliers Wrench Hammer Metal fasteners Steel fence post Conductivity survey Digital Camera Field Datasheet EC Conductivity PockeTesters or equivalent Benthic Macroinvertebrate Collection GPS 600um mesh 0 25 meter wide rectangular net or kick seine 800 x 900um D frame dip net U S Number 10 sieve U S Number 30 sieve 2 600um mesh wash buckets Medium sized bucket 300um nitex sampler mesh Fine tipped forceps 95 ethyl alcohol White picking pans Sample jars Habitat Assessment Hydrogeomorphic Assessment Digital Camera High Gradient Habitat Assessment Field Data Sheet Grav
268. freezing until analyzed Sample preservation instructions are included with the sample bottles mailed or delivered to the Supervising Sampler prior to each sampling event f Chemical treatment If a sample requiring acidification chemical treatment will not be delivered to the laboratory within six hours of its collection from the stream the following procedures are required Glass ampoules containing the preservative and appropriately protected for shipping are distributed by the Sampling Event Coordinator with the sampling containers and instructions to Supervising Samplers Instructions are sent that include these precautions Preservatives in the glass ampoules are highly concentrated acids that must be handled carefully Even a small drop of the solution can burn your skin Use of latex gloves and safety glasses is highly recommended Rinse each ampoule with water several times before discarding The following instructions are given 1 After filling the container carefully snap the neck of the ampoule and add it to container 2 Label the container with the letter N for Nitric Acid or S for Sulfuric Acid as appropriate 3 Place the container on ice 4 Carefully rinse the empty preservative ampoules before discarding 8 Transport of Samples to the Laboratory Chilled samples should be delivered to the laboratory as soon as possible bacteria samples and samples that require acidification but have not been tr
269. g before employment and will require a pre employment physical as stated in Ordinances 2114 b and 23 16 Pursuant to the Drug Free Workplace Act of 1988 and to sections 21 52 22 34 and 23 50 of the Code of Ordinances all employees must remain drug and alcohol free when reporting to work while at work and while engaged in any work related activities Based on Federal Regulation 19 10 some positions in this classification are eligible for and will be offered the hepatitis vaccinations In addition employees will be required to sign a statement stating they have accepted or declined the hepatitis vaccination TB Laboratory QAP Appendix C September 16 2009 Revision 1 Class Title LABORATORY TECHNICIAN Reports To Laboratory Supervisor Plant Operations Supervisor or other supervisor Supervision Exercised None General Function Performs technical work of considerable difficulty in conducting a variety of chemical bacteriological and industrial waste analyses for wastewater treatment plants to assure compliance with local State and Environmental Protection Agency permits Essential Functions Sample Gathering Preparation e Collects samples and makes sure that samples collected by others are in accordance with government regulations e Prepares wastewater sludge and pretreatment samples for analyses e Cleans laboratory equipment and work area e Sterilizes bacteriological equipment e Calibrates laboratory equipment
270. g pue Ruameds tof MO pasvasoar pasu SUOL Ysy ATAS 0 Fupooy ARLA enfo spaou Wn 1341 941 ajdturxe Jog pueg sy o stuownu jo powysriojdo og pue doroNpo dsl YIMOoId Joy suoped MOL myeu oy uo puadap suturas 1290 pue ur sejd pue speuminy esd 01 JUD WO OSJE PUE IBO oy SULIMP AIBA TA SLIBOJS JO SMOL EYEN PUQuIio nata MENDE 943 uy 9ABUSQ J SIOP MOH sdi puodas tod JIA Ur painswoul st AGJA Jaye DIJO pasds oy 97 SU JO ponad UOAIT E JIAO SABR JALAM FEU SDUBISIP A SI NDO O A PETNE Og OSTE UBS JOEA NP UI POLLO euoyeu JO JUNOWR Y INNOD LRM Y JO DILE MOY AJRIPOLULE ou duisn Ag psu Aep Jad suoje dor nu do sj9 puooas 10d 393 AGRI UY pamseotu ST MOJA UI Jo Junone UDALE Y IDAO SABIVYOSIP JOAN IO WARIS Y JVM JO IUINJOA HY SL MOTT GUT STE TBY AA MOLA y AJA 10 MOT JAA JRULIOU 313M SMOY gi mouy 07 pasu aa repnomied up shep may snotaaad ay Sump ayqissad yt pue Judes so 3188 oui 18 H pIo 9A yu poeodiar s 3 APPEND 1038 uo POedun PEAPBS Y SPY MO ISLA JUDAS UB YANS JAYE SYOIM VAS JO Shep 10 1ISLSH ABI Mg pooy e Jo sgus Apes oq Junnp gapai A eiua sar Jqeab ui suey osoyy Append opea Jo spoadse soyo Auent 07 sa uego 218 21041 10q ppal spas wens aq 91 sofonard papuadsns UL OSBM OY SE UOTIBISOJTUEUT SNOTAGO MO Usears Y u IORA JO NTEAD peunou oy 01 SOBURYO PAYITL OSHS swour PURJIDAO yons pojoedxa oq pros sy MOYUT SSBu3as jPULLOW JO LY o quelo ip amb s npenb sy pue cotas
271. ge to allow full colonization potential e logs snags that are not new fall and not transient colonization potential adequate habitat for maintenance of populations presence of additional substrate in the form of newfall but not yet prepared for colonization may rate at high end of scale less than desirable substrate frequently disturbed or removed obvious substrate unstable or lacking SCORE 2 Embeddedness 20 19 18 17 16 Gravel cobble and boulder particles are 0 25 surrounded by fine sediment Layering of cobble provides diversity of niche space 15 14 13 12 11 Gravel cobble and boulder particles are 25 50 surrounded by fine sediment 10 9 8 7 6 Gravel cobble and boulder particles are 50 75 surrounded by fine sediment 514 3 2 1 0 Gravel cobble and boulder particles are more than 75 surrounded by fine sediment SCORE 3 Velocity Depth Regime 20 19 18 17 16 All four velocity depth regimes present slow deep slow shallow fast deep fast shallow Slow is lt 0 3 m s deep is gt 0 5 m 15 14 13 12 11 Only 3 of the 4 regimes present if fast shallow is missing score lower than if missing other regimes 10 9 8 7 6 Only 2 of the 4 habitat regimes present if fast Shallow or slow shallow are missing score low 514 3 2 1 0 Dominated by 1 velocity depth regime usually slow deep
272. ge of 0 011 mg L with a daily maximum limitation of 0 019 mg L In the event that analysis results indicate values greater then KPDES permit requirements retest If the value indicated by the retest is greater than KPDES permit requirements Immediately notify the Plant Superintendent and Laboratory Supervisor Process Ranges Expected residual chlorine results on plant effluent samples will be less than 0 010 mg L typically the results are BDL below detection limit Data Analysis and Calculations 11 1 11 2 Concentration values are read directly from the AutoCAT unit s display all calculations are preformed internally The Laboratory Supervisor will determine if the results for the standard are within the expected range Bibliography 12 1 12 2 12 3 U S EPA Method 330 3 Chlorine Total Residual Titrimetric Amperometric Issued 1978 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 Standard Methods 4500 Cl D Chlorine Residual Amperometric Titration Method APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 HACH AutoCat 9000 Chlorine Amperometric Titrator Instruction Manual HACH Company Loveland CO 16 SOP WH Fecal Coliforms
273. ging etc gt 20 past years may be present but recent channelization not present Wolf Run Watershed Page 46 of 67 Revision No 0 Based Plan Date April 11 2011 Marginal Channelization may be extensive embankments or shoring structures present on both banks and 40 80 of the stream reach channelized and disrupted Poor Banks shored with gabion or cement gt 80 of the stream disrupted in stream habitat greatly altered or removed entirely Parameter 7 Frequency of Riffles or Bends This metric measures the sequence of riffles and thus the heterogeneity occurring in a stream Estimate riffle frequency by determining the ratio of distance between riffles divided by the width of the stream An average of the riffle ratios is determined for biological monitoring stations and the upstream segment Optimal Occurrence of riffles relatively frequent ratio of distance between riffles divided by the width of the stream lt 7 1 generally 5 to 7 variety of habitat is key in streams where riffles are continuous placement of boulders or other large natural obstruction is important Suboptimal Occurrence of riffles infrequent distance between riffles divided by the width of the stream is between 7 and 15 Marginal Occasional riffle or bend bottom contours provide some habitat distance between riffles divided by the width of the stream is between 15 and 25 Poor Generally all flat water or shallow riffles poor habitat d
274. gles and lab coat ALWAYS ADD ACID TO WATER NOT WATER TO ACID Sample Handling and Preservation 4 1 None required 89 SOP Volatile Acids LFUCG Laboratory Page 90 of 219 Revision Number 3 Last Revised 09 09 Reagents 5 1 Sulfuric acid 1 1 5 2 0 1 N Sodium hydroxide 5 3 Phenolphthalein Indicator 5 4 Nanopure Water 5 5 Glacial acetic acid Equipment amp Lab Ware 6 1 Heating Mantles 6 2 Hotplate 6 3 Centrifuge tubes 6 4 Boiling flask 6 5 Condenser about 76 cm long 6 6 Distillation Assembly 6 7 Adapter tubes 6 8 Erlenmeyer flasks 6 9 Thermometers with stoppers 6 10 Titrator 6 11 Digital Buret 6 12 Plastic funnels 6 13 5 mL pipette and tips 6 14 Timer 6 15 Finger vinyl leather gloves 6 16 100 mL amp 20 mL graduated cylinders Interferences 7 1 Hydrogen sulfide and carbon dioxide are liberated during distillation and can be titrated to give a positive error Eliminate error by discarding the first 15 mL of distillate and account for this in the recovery factor Procedures 8 1 Steps 1 Turn on heating mantles 2 Make sure hot plate is on 3 Fill centrifuge tubes to obtain 125 mL of sample Centrifuge samples for 15 minutes 90 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 SOP Volatile Acids LFUCG Laboratory Page 91 of 219 Revision Number 3 Last Revised 09 09 Gently swirl tubes to mix and centrifuge for an additiona
275. gulations certifications and methods by which the laboratories operate the laboratories will perform several assessment measures To ensure that analysts are capable of performing the requested analytical methods to specifications each analyst must acceptably demonstrate this ability prior to conducting sample analyses The analyst must conduct four replicate analyses of a known standard and achieve precision and accuracy equal to or better than the acceptance ranges for laboratory duplicates and laboratory control samples respectively The laboratory QA Director or his appointee on an annual basis will perform internal audits The findings of the audits both positive and negative will be documented and the corrective response to the cited deviations will be made Corrective actions will be submitted to the auditing body for review and approval The QA Manager is responsible for the overall conformance of field personnel to the procedures protocols and methods established by this QAPP and internal project related procedures The QA Manager will conduct at least one audit of the volunteer samplers field activities and documentation including calibration and maintenance of field equipment and sample collection techniques Deviations found in such assessments will Revision No 0 Date April 11 2011 Wolf Run Watershed Based Plan Page 60 of 67 be reported to the samplers and documented using the Field Sampling Audit Checklist Appendix
276. h Volunteer Database as administered by the Watershed Management Branch The training will consist of four sessions that will cover habitat assessments grab sample collection in situ measurements and the requirements of this QAPP Powerpoint presentations to be used in this training are available at http www lrww org training The training will be organized and conducted by the FOWR and their Science Advisors The FOWR Sampling Coordinator will maintain documentation of the volunteer sampler training through the Participant Agreement Form Appendix A A9 Documentation and Records In order to provide quality data that meets the project objectives traceability and maintenance of documentation and records is essential All records relating to the collection analysis or reporting of data associated with the project shall be made available upon request by KDOW or LFUCG A summary of such documentation is included below A9 1 Field Documentation and Records Field records will include all data recorded in the field including completed field datasheets field logbooks monitoring records and chain of custody sheets All data will be recorded using black or blue indelible ink and it is recommended that waterproof paper be used where feasible Mistakes on field data sheets will be crossed out with one line so the information is still discernible with the initials and date of the person making the correction The correct information should then
277. habitat assessment hydrogeomorphic assessment water quality monitoring The sampling responsibilities frequencies and number of sites to be sampled for each monitoring activity are summarized in Table 2 The equipment necessary for each of these activities is specified in Table 3 Exhibits 1 and 2 show the study area and the selected sampling locations A discussion of each of these activities follows TABLE 2 MONITORING ACTIVITY OVERVIEW Sampling Monitoring Activity Responsibility Frequency No of Sites Karst hydrograph characterization Third Rock 6 Conductivity survey Volunteers 1 100 ft Benthic Macroinvertebrate Collection a Macroinvertebrate Collection Third Rock Once 6 Third Rock and b Habitat Assessment Once 6 Volunteers At least 1 per Segment 24 Hydrogeomorphic Assessment Third Rock Twice 9 Water Quality Monitoring Watershed Habitat Assessments Volunteers Once Third Rock and Monthly Volunteers 10 events Third Rock and 5 events in Volunteers 30 days a Water Quality Monitoring b E coli Geomean Sampling Wolf Run Watershed Page 13 of 67 Revision No 0 Based Plan Date April 11 2011 x 3 Pys 104 S4 aa W Reynolds Ra A f gt Puida ELET E z n d Ka Jus y1Sal y 499101 UslUNIO ey S 1quux SHQIYX SI DUI JOM Mapping provided by LEUCG Oct 2010 Karst mapping from KY Geological Survey Gage Location Karst Inflow Out
278. hain of Custody Chain of Custody COC forms will be completed for all samples collected in the field and will follow each sample throughout sample processing A COC form is a controlled document used to record sample information and ensure the traceability of sample handling and possession is maintained from the time of collection through analysis and final disposition A sample is considered in custody if it is e In the individual s physical possession e In the individual s sight e Secured in a tamper proof way by that individual or secured in an area restricted to authorized personnel Example COCs that will be used in the collection are attached in Appendix A All information shall be documented on the COC in black or blue waterproof permanent ink including field physical measurements and custody information The sampler shall initiate sample custody at the time the sample is collected Field custody documentation shall include Wolf Run Watershed Page 53 of 67 Revision No 0 Based Plan Date April 11 2011 Verification of sample identification Number of sample bottles collected Collection date Collection time Collector s signature The sampler shall maintain possession of the sample until custody is transferred to the laboratory or another party The COC shall accompany the sample from the time of collection until it is relinquished Field custody will be relinquished by signature with date and time of the sample in the
279. hat the GED is exceeds the KPDES permit requirements notify the Plant Superintendent and the Laboratory Supervisor 10 2 Process Ranges lt 1 to gt 120 000 CFU 100 mL Data Analysis and Calculations 11 1 See the following pages Bibliography 12 1 U S EPA Microbiological Methods for Monitoring the Environment Water and Wastes EPA 600 8 78 017 U S Environmental Protection Agency Environmental Monitoring and Support Laboratory Office of Research and Development Washington DC 1978 Page 124 122 Kentucky Department for Environmental Protection Kentucky Division of Water and the Kentucky Division of Compliance Assistance Discharge Monitoring Report Manual 2009 August 10 2009 revision 28 pp 50 SOP Fecal Coliform LFUCG Laboratory Page 51 of 219 Revision Number 3 Last Revised 09 09 FECAL COLIFORM CALCULATIONS The ways the answers are presented vary with the number of colonies on the plate A Countable plates with 20 60 Blue colonies i t Fecal Coliforms 100 mL Number of Blue colonies counted x Volume of sample filtered mL Example 40 Blue colonies are counted and 50 mL of sample was used 4 Fecal Coliforms 100 mL Z x100 80 B Countable plates with less than 20 Blue colonies e If only one plate has been set up calculate as shown but place an approximately equal to sign 2 in front of the answer 1 Fecal Coliforms 100 mL E x100 36 e If more than one plate has been set up c
280. he Determination of Total Coliforms and E coli oooonionnininnn 54 Hardness Total mg L as CaCO3 Titrimetric EDTA ooooconcccinocinonoconoconononnncnnnccon coco nocancconnnos 60 PHC EISC HOMIE EHC ii tas 63 Total Phosphorus A TAL YSIS ait riada 69 Ascorbic Acid Med ES 69 PS GETS ea FSS LTS a aires see rasta season A 78 Total Suspended Solids USS it litis 81 Total Solids spagn n a ae do Gua aes 85 EI A A 89 Volatile SOAS cad rios 94 WEST HICKMAN CREEK SO Ps ties MG secre latins alata this Maudie isso dt Ais aos 1 WH Dissolved Oxygen Field Analysis D O cccccccsssesssessseceseceeeeeeeeeseecsaeceseeneseenaeecnaeeneenses 2 WH pH Electrometric as 7 WH Total Residual Chlorine Analysis ccccscccsseceseceseceesceescecsseceecseceeeseecaeceseceeneeeaeecsaeens 12 WH Fecal Coliform Membrane Filter Procedure ooooonccinocinocononcnonnnononononoconocnnn cono conan ncnnnnns 17 WH Total Phosphorus Atialy sis vei adscesidos corel a e dal e o cal as 24 APPENDIX D LABORATORY BENCHSHEETS c ccccococcccnonononnncnnnnnnnonnnonnnnnnnnnnnnnccnnonnncnnnnnos D 1 TB Laboratory QAP September 16 2009 Revision 1 FORWARD The following Quality Assurance Plan QAP for the Town Branch Laboratory has been adapted from the Illinois Water Environment Association Laboratory Committee Model QAP This document is intended as guidance only and not a detailed explanation of the accreditation rules Periodic review of this document will be conducte
281. he comments column Page 1 of 2 Field Sampling Audit Checklist Water Quality Sample Collection Data Quality Indicator DQ ENE Comments Samples correctly labeled Storage and preservation Equipment Used Equipment Name ses Deia Conforms Comments By Date Other Comments Yes No Indicates that the task performed in conformance out of conformance with the project s DQI If the DQI is not relevant to the task write N A in the comments column Page 2 of 2 Laboratory Data Quality Checklist General Information Project No Description Laboratory Data Reviewed Evaluation For each DQI indicate whether the laboratory data met the project objectives If not document non conformances in the comments column and the action to be taken by data users Attach additional sheets if necessary for documentation Data Quality Indicator DQ aight Comments Precision Agreement among repeated measurements of the same property under identical or substantially similar conditions random error i e duplicates Splits Accuracy Overall agreement of a measurement to a known value includes a combination of precision and bias i e difference from known laboratory control standard of matrix spike Sensitivity Capability to discriminate between measurement responses representing different levels of variable interest i e
282. he sample this will be the Known Positive Remove and plate filter as indicated in Section 8 1 Log results initials time and date in the Microbiology bench sheet 21 SOP WH Fecal Coliforms West Hickman WWTP Laboratory Page 22 of 219 Revision Number 4 Last Revised 09 09 8 4 Peptone Buffer Preparation 1 2 3 4 5 6 7 Measure 1 0 g Peptone powder into 1L volumetric flask Bring to volume with Nanopure water Mix well Pour Peptone buffer into Nalgene autoclavable squeeze bottle Take a sample of the buffer and measure pH it should be 7 00 0 1 Loosely screw caps dispensers onto squeeze bottles Autoclave Peptone buffer solutions Allow to cool then transfer squeeze bottles to Micro fridge 8 5 Helpful Hints 1 2 3 4 If the bacterial density of the sample is unknown filter and plate out several volumes or dilutions in order to achieve a countable density The volumes and or dilutions should be expected to yield a countable membrane In addition select two additional quantities representing one tenth and ten times this volume respectively Separate filter holder units may be required during a set of samples These will be indicated in the bench sheet Do not use damaged or bent membrane filters Rinse the filter unit thoroughly with Peptone buffer to avoid cross contamination QA QC Requirements 9 1 Before and After Blanks must be run with each set of samples tested 9
283. horus forms when the unfiltered shaken sample is heated in the presence of sulfuric acid and ammonium peroxydisulfate Total dissolved phosphorus includes all phosphorus forms when the filtered shaken sample is heated in the presence of sulfuric acid and ammonium peroxydisulfate Phosphorus is converted to orthophosphate by digesting the water sample with ammonium persulfate and diluted sulfuric acid Ammonium molybdate and antimony potassium tartrate can then react in an acid medium with dilute solutions of orthophosphate to form an antimony phosphate molybdate complex This complex is reduced to an intensely blue colored complex by ascorbic acid The color intensity is proportional to the phosphorus concentration Sensitivity The range of determination for this method is 0 05 mg L to 1 00 mg L P Interferences Ferric iron must exceed 50 mg L copper 10 mg L or silica 10 mg L before causing an interference Higher silica concentrations cause positive interferences over the range of the test as follows results are high by 0 005 mg L of phosphorus for 20 mg L of SiO2 0 015 mg L of phosphorus for 50 mg L and 0 025 mg L of phosphorus for 100 mg L Because arsenic and phosphorus are analyzed similarly arsenic can cause an interference if its concentration is higher than that of phosphorus Sample Handling and Preparation Samples should be preserved only by refrigeration at 4 C A raw sample should be used in the analysis The holding time for
284. iation Upper Control Limit UCL Lower Control Limit LCL Upper Warning Limit UWL Lower Warning Limit LWL Date of Analysis Analyst Identification 6 8 Initial Demonstration of Method Performance Studies IDMP 6 8 1 6 8 2 Each analyst performs an IDMP study prior to initiation of sample analyses unless the IDMP is not applicable to the approved test method such as BOD CBOD total suspended solids total dissolved solids total volatile solids total solids pH temperature dissolved oxygen or turbidity The IDMP study is repeated whenever there is a change in analyst instrument type or approved test method The following steps are performed for an IDMP study A quality control QC check sample is obtained from an outside source If not available the QC check sample may be prepared by the laboratory using standards that are prepared separately from the calibration standards by someone not running the test The laboratory prepares four aliquots of the QC check samples at the required method volume to a concentration approximately 10 times the method stated or laboratory calculated MDL The three aliquots are prepared and analyzed according to the approved test method Using the three results the average recovery and standard deviation are calculated in the appropriate units for each analyte For each analyte the standard deviation and average recovery are compared to the corresponding acceptance criteria for precis
285. ic monitoring will initially be conducted in May 2011 with a second survey to assess geomorphic conditions nine 9 months after the baseline is completed February 2012 assuming sufficient flow events occur during this period Data analysis will occur subsequent to the data generation with a final report completed by April 30 2012 Wolf Run Watershed Page 20 of 67 Revision No 0 Based Plan Date April 11 2011 TABLE 4 PROJECT SCHEDULE 2011 2012 Apr May Jun Jul Aug Sep Oct Nov Dec Jan Feb_ Mar Apr May Jun Jul Aug Sep Oct Nov Dec Activity Planning and Training QAPP Approval E CS ES EA SS E E AS E O E O E E eee Volunteer Training OO A UE E PE IR A E A PE E E ee eee Council Meetings Quarterly Karst Hydrograph Characterization Installation of Data loggers Prints a rR EAaAn anh Base Flow Event La E AE A AL ES EE EA Wet Weather Event OOT O T S T TTo Data Analysis _ i ee ee E fe CO E O TS TTT Oo Report Completion A SS ae Conductivity Survey Conduct survey 0501000 lil ee STT ES Data Entry and Analysis Report Completion OC C C T PEA AAA AE Benthic Macroinvertebrate Collection So T Habitat Assessment OO HE ESO E E Oo Laboratory identification ee S E E PO S SS ee Data Entry and Analysis PAE S TS TT O LEA Report Completion CST A S S S J Sd JJ IJ Watershed Habitat Assessment Habitat Assessments by Rea
286. icon in the upper left corner of the display screen Record the indicated value remove the probe and rinse tip with Nanopure water Then proceed to the next sample or store until needed DO NOT store probe in the BOD bottle containing water Probe can be stored dry on the bench top Helpful Hints 1 2 3 4 The meter is designed to be maintenance free when needed clean the exterior with a damp cloth The probe s maintenance consist of maintaining the probe tip clean frequent rinsing with Nanopure water is sufficient DO NOT scrub the sensor cap or lens DO NOT use any organic solvents on the sensor cap or probe body QA QC Requirements 9 1 9 2 9 3 Meter must be calibrated a minimum of once per analysis day Permit sample hold times must be 15 minutes or less Probe condition must be properly maintained through routine cleaning See Section 8 3 Helpful Hints 10 11 12 SOP WH FIELD D O West Hickman WWTP Laboratory Page 6 of 219 Revision Number 3 Last Revised 09 09 Expected Results 10 1 KPDES Permit Requirements 10 2 7 0 mg L is the lowest D O value allowable in a plant effluent sample at any given time In the event of an indicated value less than 7 0 mg L assure correct calibration resample and retest If the value indicated by retest is less than 7 0 mg L Immediately notify the Plant Superintendent and the Laboratory Supervisor Process Ranges Raw influent dissolved ox
287. ification laboratory will follow laboratory protocols for benthic macroinvertebrate sample processing identification and data reporting per KDOW 2009b 2008 with the following exceptions e All samples will be logged into Third Rock s Macroinvertebrate Laboratory Information Management System MacLIMS upon receipt e Sample identification date will be maintained in MacLIMS e Taxonomic QA QC dates if applicable will be noted on individual QA QC forms and maintained electronically in the Project File e Initials of the applicable party completing each task associated with sorting identification or quality control will be noted electronically in MacLIMS or on associated QA QC forms e QA checks will be documented on applicable forms and maintained in associated project files These forms include the Macroinvertebrate Sample Sorting Efficiency Form Macroinvertebrate Sample Taxonomy Precision Form and Macroinvertebrate Sample Taxonomic and Enumeration Efficiency Form Appendix A Completed chain s of custody and sample labels will also be controlled throughout the analysis process and completed chain s of custody will be submitted in the data package The laboratory will retain all data associated with the sample analysis for the duration of the grant period Expected turn around time for the laboratory analysis is 30 days Chemical laboratory reports with data quality review by the Project QA Manager will be submitted to the project
288. igher number of particles sampled is not indicated If it is determined upon field investigation that a given hydrogeomorphic monitoring site has a wide particle size spectrum at least 400 particles may be collected for the reach wide pebble count An active bed riffle pebble count will also be collected within the permanent cross section at each of the nine hydrogeomorphic monitoring sites For the active riffle bed count particle sampling will be completed along evenly spaced transects over the active bed width and consist of at least 100 particles refer to Rosgen 2008 and Bunte and Steven 2001 for pebble count procedures For all pebble counts each transect will start on the same side of the stream and collection will move from downstream to upstream Sampling points will be spaced by at least the Dmax particle size The pebble count will end at the extent of a given transect not in an arbitrary location when a count of 100 particles is reached If fine sediments sand silt are encountered and the thickness of the sediment layer is less than 0 5 inch then it will be appropriate to select the larger particle below the fines Otherwise the observation will be counted as fines i e less than or equal to 2mm Equipment used will include a ruler mm or gravelometer gravel template with the gravelometer being preferred Data may be recorded in RiverMorph software using a Rugged Reader Pocket PC or on a Pebble Count Datasheet see Append
289. ile Acids Buret Titration Method 2 Edition HACH Company Loveland CO 1992 93 SOP Volatile Solids LFUCG Laboratory Page 94 of 219 Revision Number 3 Last Revised 09 09 Volatile Solids EPA Method 160 4 Residue Volatile Gravimetric Ignition at 550 C Issued 1971 Standard Methods Part 2540 E Fixed and Volatile Solids Ignited at 550 C Scope Significance to Process and Application 1 1 This method is applicable to drinking surface and saline waters domestic and industrial wastes Summary of Method 2 1 Executive Summary Total solids are the material residue left in a vessel after evaporation of a sample and subsequent oven drying at a defined temperature The total solids are then ignited to a constant weight at 550 C and the weight loss on ignition represents the volatile solids Volatile solids analyses are important because they offer a rough approximation of the amount of organic matter present in the solid fraction of wastewater activated sludge and industrial waste 2 2 Discussion Volatile solids are the weight lost due to ignition The remaining solids represent the fixed total Health amp Safety Precautions 3 1 Watch out for broken glass from Vycor dishes cylinders and beakers 32 Wastewater samples should be considered potentially hazardous Use proper personal protective equipment 3 3 Dishes are HOT 550 C use proper gloves when handling Watch out for hot surfaces Sample Handling and P
290. immediately and preserve sample accordingly B2 2 6 3 Field Filtration The collection of the ortho phosphorus samples requires field filtration using a hand pump Third Rock will perform this field filtration within 15 minutes of sample collection In order to collect this field filtered sample the stream sample will be collected using the grab sample methodology The funnel funnel filter base and flask will be triple rinsed with with DI water and the hand pump the inside of tubing and tweezers will be single rinsed with DI water Clean forceps will be used to place 0 45 um paper filter onto funnel filter base The filter base will be attached to flask and the tubing from the hand pump will be connected 50 mL DI water will be poured into funnel filtered rinsed and discarded 50 mL of the stream sample water will be poured into funnel filtered rinsed and discarded Then enough stream sample water will be poured into the funnel to provide enough finished sample for rinsing the storage bottle and for analysis If the stream is particularly turbid smaller amounts of the sample water will be used When 0 45 um paper filter becomes excessively clogged the filter will be removed with forceps discarded and replaced with a fresh filter Filtering will be continued until the Wolf Run Watershed Page 52 of 67 Revision No 0 Based Plan Date April 11 2011 required sample volume is achieved The sample will be poured from the filter flask into th
291. in the conductivity of a waterbody can indicate groundwater input catchment geology or pollution B1 2 3 Benthic Macroinvertebrate Collection Benthic macroinvertebrate sampling integrates months or even years of water quality impacts as well as the cumulative effects of multiple stressors and pollutants instead of particular individual stressors The KDOW uses biological indicators to determine the use attainability of a water of the Commonwealth as it relates to KDOW s narrative water quality standards Biological assessment will provide a more accurate evaluation of water quality health in the watershed The six macroinvertebrate sites are located on the tributaries of Wolf Run and in its headwaters to evaluate the macroinvertebrate communities in the headwaters for comparison to the data collected over multiple years near the mouth of the watershed B1 2 4 Watershed Habitat Assessments Habitat assessments will be used to supplement biological and physicochemical data when determining the overall health of the stream reach and stream use designation Additionally habitat assessments will serve as a baseline to document physical changes that occur over time and to identify potential areas for BMP implementation The watershed was divided into 24 stream segments in order to ensure that assessments are collected from all representative reaches B1 2 5 Hydrogeomorphic Assessment The process of development within the Wolf Run watershed has affe
292. ine the sample blank for reactive phosphorus 1 Run the Reactive Phosphorus Method 10209 test but do not add the DosiCap C in step 3 2 Cap the vial with the original DosiCap Zip but do not remove the foil Use the side of the cap without the reagent 3 Subtract the value obtained in step 7 from the value obtained on the original reactive phosphate sample to give the corrected sample concentration Alternatively reactive phosphate samples that contain only turbidity may be first filtered through a membrane filter and then analyzed Samples without color or turbidity do not require sample blanks 74 9 10 8 9 SOP TP LFUCG Laboratory Page 75 of 219 Revision Number 1 Last Revised 09 09 Helpful Hints 1 Analysis results are directly proportional to sample volumes therefore it is very important that accurate sample volume measurements are made Correct the test results for volume dilutions 2 The TNTplus test vials are cuvettes to be analyzed spectrophotometrically and must provide a clear optical path Prior to reading clean the vials by wiping with a Kim Wipe 3 When washing lab ware involved with this method use only phosphate free cleaning agents 1 1 HCL solution is recommended followed by thorough Nanopure water rinse Note Most of the lab ware used in this method is disposable Standard Preparation A 100 mg L as PO Phosphate Standard Solution is used as the stock to make standard dilutions Th
293. ined yearly in the use and safe handling of the extinguishers 10 4 2 Other Safety Equipment The Town Branch lab maintains a fully stocked first aid kit two eye wash and shower stations All safety equipment is inspected on a monthly basis The lab has a total of 8 chemical hoods which are inspected and serviced yearly Chemical neutralization and spill control kits and acid and flammable storage cabinets are located in the chemical storage room Current MSDS sheets are maintained for all chemicals used in the lab Computer Resources Including Equipment and Software The LFUCG IT department is responsible for all computers and software used in the laboratory A total of 5 PC computers are located throughout the laboratory All computers have access to the internet via the City s server Password protections restricts access to lab data to lab personnel only All data is viewable as a read only file In addition to the Excel based database all laboratory computers can access the HACH Water Information Management Solution WIMS database which houses all laboratory information Laboratory Work Areas Several sections in the laboratory have been reserved for specific analyses These sections include sample receiving microbiology BOD preparation analysis wet chemistry total residual chlorine analysis total cyanide digestion solids processing weighing spectrophotometric methods 1 e HACH TNT methods water purification Emp
294. ing back on the plunger of the syringe Make certain that all of the air bubbles are removed from the eluent line to the pumps Press OFF ON on the pump to turn it off 8 Turn the valve on the Priming Block clockwise remove the syringe and expel the air bubbles from the syringe Reinsert the syringe filled with eluent into the Priming Block 10 Open the valve on the Pressure Transducer and the valve on the Priming Block with the eluent filled syringe still attached This is accomplished by turning both counterclockwise 11 Press PRIME on the pump and push the contents of the syringe into the Priming Block After the eluent has been injected into the Priming Block press OFF ON to turn the prime pump off and to close the valves on the Pressure Transducer and Priming Block 12 Remove the syringe from the Priming Block 13 Scroll to the mL min on the screen for the pump For the GP50 type 2 mL min and press ENTER For the IP25 type 1 2 mL min and press ENTER 14 Press OFF ON to turn on the pump at the appropriate rate The pressure should soon stabilize between both pumpheads after two minutes of pumping time 15 If the pressure between pumpheads has a difference gt 20 psi then shut down the pump and repeat steps 2 14 to remove air bubbles and prime the pumps 16 Once the pump has a pumping pressure difference between pumpheads of lt 20 psi then go to the computer and enter PeakNet 17 On the computer turn on the Chrome
295. ington DC 2005 Standard Methods 5210 A and 5210 B Biochemical Oxygen Demand BOD APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Standard Methods Part 5560 C Distillation Method APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 52 TB Laboratory QAP September 16 2009 Revision 1 U S EPA Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 130 2 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 150 1 pH Electrometric Issued 1971 Editorial revision 1978 and 1982 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 U S EPA Method 160 2 Residue Non Filterable amp Total Suspended Solids Issued 1971 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington
296. inity TSS VSS Total Solids Volatile Solids Total Solids Volatile Solids TSS Total Phosphorus Ortho phosphate Total Solids Total Solids Total Solids Metals Total September 16 2009 Analysis Requirements Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation TB Laboratory QAP Appendix A Revision 1 Table A3 Blue Sky WWTP Analysis List Sample Name Raw Influent Plant Effluent Raw Influent Plant Effluent Contact Zone Re Aeration Digester Analysis CBOD TSS Ammonia CBOD TSS Ammonia Hardness Fecal Coliforms Oil amp Grease Total Phenols Total Phosphorus Ammonia Metals Dissolved Metals Total Total Alkalinity Total Phosphorus Ortho phosphate Ortho phosphate TSS Total Alkalinity TSS Total Alkalinity TSS Total Alkalinity September 16 2009 Analysis Requirements Required Required Required Required Required Required Required Required Required Required Required Required Required Required Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation TB Laboratory QAP Appendix A September 16
297. ion and accuracy in the approved test method if applicable or laboratory generated acceptance criteria if a non standard method If standard deviation and average recovery for all analytes meet the acceptance criteria the analysis of actual samples may begin If any one of the analytes exceeds the acceptance range the performance is considered unacceptable for that analyte The laboratory management maintains a file to track all current IDMP studies 10 TB Laboratory QAP September 16 2009 Revision 1 6 9 6 10 Method Detection Limits MDL 6 9 1 6 9 2 6 9 3 6 9 4 6 9 5 6 9 6 MDLs for each analyte of interest are determined by the test method procedure specified in 40 CFR Part 136 Appendix B unless the test method specifies another procedure for MDL determination or the determination of an MDL is not applicable to the test method The laboratory analyzes a minimum of seven replicates to determine the MDL e If seven replicates are analyzed the laboratory uses all analytical results when calculating the MDL e Ifthe laboratory analyzes more than seven replicates the laboratory only excludes analytical results which the laboratory determines are outliers by utilizing a statistical outlier test The laboratory determines MDLs for each approved test method annually and when there is a change in instrument type The laboratory may in lieu of the annual determination of the MDL annually verify the MDL by
298. ion of B the unknown made from both for comparison 6 Quality Control A quality control sample obtained from an outside source must first be used for the initial verification of the calibration standards A fresh portion of this sample should be analyzed every week to monitor stability If the results are not within 10 of the true value listed for the control sample prepare a new calibration standard and recalibrate the instrument If this does not correct the problem prepare a new standard and repeat the calibration A quality control sample should be run at the beginning and end of each sample delivery group SDG or at the frequency of one per every ten samples The QC s value should fall between 10 of its theoretical concentration A duplicate should be run for each SDG or at the frequency of one per every twenty samples whichever is greater The RPD Relative Percent Difference should be less than 10 If this difference is exceeded the duplicate must be reanalyzed From each pair of duplicate analytes X and X2 calculate their RPD value X X X 2 where X X2 means the absolute difference between X and X 7 Method Performance The method detection limit MDL should be established by determining seven replicates that are 2 to 5 times the instrument detection limit The MDL is defined as the minimum concentration that can be measured and reported with 99 confidence that the analyte concentration
299. ion of the Dissolved Oxygen bench sheet under Barometer Reading On the Lab computer open the excel spreadsheet entitled DO Meter Calibration Sheet and enter the barometric pressure temperature and dissolved oxygen values from the dissolved oxygen calibration section of the Dissolved Oxygen bench sheet The spreadsheet will calculate the Dissolved Oxygen Calibration Point the Dissolved Oxygen 1 ATM and the Slope Transfer the three values onto the dissolved oxygen calibration section of the Dissolved Oxygen bench sheet then print a copy of the spreadsheet and file it Note the difference between the Dissolved Oxygen from HQ40d and the Dissolved Oxygen Calibration Point if it is greater than 0 2 mg L then the calibration is not acceptable and must be repeated until criteria is met 9 0 8 2 8 3 SOP WH FIELD D O West Hickman WWTP Laboratory Page 5 of 219 Revision Number 3 Last Revised 09 09 Measurements 1 2 3 4 5 6 Make sure that the meter is properly calibrated Rinse the LDO101 probe tip with Nanopure lab water Place probe into a BOD bottle filled to the base of its neck with sample assure that there are no air bubbles on the surface of the probe tip In the field the probe is lowered into the sample Press Read screen will display Stabilizing and a progress bar will scroll from 0 to 100 Reading stability is indicated by the appearance of a Padlock
300. ion procedure has a range of 0 0012 mg L to 5 0 mg L with an estimated detection limit of 0 0012 mg L Discussion Chlorine hypochlorite ion hypochlorous acid and chloramines liberate iodine from potassium iodide at pH 4 or less in stoichiometeric proportions The iodine is titrated with a reducing agent phenylarsine and an amperometer detects the endpoint Although the actual measurement is that of the samples oxidation potential it is calculated and expressed as mg L Cl because chlorine is the dominating oxidizing agent present Health amp Safety Precautions Glassware involved possible cut hazard Wastewater samples have the potential to be hazardous use appropriate caution 22 SOP Residual Chlorine LFUCG Laboratory Page 23 of 219 Revision Number 4 Last Revised 09 09 Sample Handling and Preservation 4 1 Residual chlorine is subject to dissipation by exposure to sunlight mechanical agitation exchange of gases with the atmosphere and reaction with compounds in the wastewater over time For these reasons chlorine residuals should be analyzed immediately within 15 minutes of sampling time 4 2 The sample should be taken gently into a glass 300 mL BOD bottle completely filling to above the base of the neck and installing the tapered glass stopper in a manner that precludes air bubbles in the sample 4 3 All glassware used in this method must have no chlorine demand therefore do not use plastic containers and pre treat g
301. ionally to promote the detachment of organic and inorganic contamination from the equipment 3 DI Water Rinse a Put ona new pair of gloves b Place equipment and tubing into a washbasin labeled DIW c Rinse all equipment and tubing with DI water d Place onto a clean surface to dry 4 Clean Equipment Storage a Place clean equipment in plastic storage bags b Double bag tubing B7 Data Management In order to ensure that project objectives are achieved data must be collected and managed in a manner that will protect and ensure its integrity The data collected under this project will be produced under standardized procedures and forms where practicable All field data will be recorded using black or blue indelible ink Mistakes on field data sheets will be crossed out with one line so the information is still discernible with the initials and date of the person making the correction The correct information will then be recorded legibly on another line or above or below the original info If a separate sheet is necessary for new information the original sheet will be attached to the new sheet and initialed and dated Wolf Run Watershed Page 58 of 67 Revision No 0 Based Plan Date April 11 2011 Data collected by volunteers shall be submitted to the Ken Cooke FOWR Sampling Coordinator He shall review the data for any nonconformances and enter the data into electronic databases and forward the electronic databases and elect
302. is removed from the lab manual and archived for a minimum of five years Forms Data Sheets Documentation Control Procedures All forms and data sheets prepared by the laboratory display a title version number and effective date TB Laboratory QAP September 16 2009 Revision 1 5 1 Section 5 Laboratory s Approved Signatories Approved Signatories The laboratory s approved signatures with job titles and accreditation position are shown in Appendix 3 Also the QAP title page has signed concurrence with appropriate titles of all responsible parties including the quality assurance officer and laboratory director Laboratory Supervisor Quality Assurance Officer Town Branch Superintendent West Hickman Creek Superintendent Director Division of Water Quality TB Laboratory QAP September 16 2009 Revision 1 6 1 6 2 6 3 Section 6 General Quality Control Procedures and Practices Documentation of Test Methods and Laboratory Practices 6 1 1 All test methods have written standard operating procedures SOPs The written methods describe each procedure and the equipment needed Each SOP follows a standard format which includes additional information on quality control measures and acceptance criteria for data All laboratory practices pertaining to QA QC as well as laboratory operation practices other than analytical methods have written standard operating procedures General Quality Control Guidelines
303. is treated with chlorine as enters the chlorine contact tanks allowing contact time for disinfection to transpire Final effluent is then treated with a dechlorinating agent reducing chlorine residual concentration to within acceptable limits see sec 10 1 Permit limits Complete dechlorination is necessary to prevent chlorine related adverse effects on the receiving environment Town Branch Waste Water Treatment Plant uses Chlorine Dioxide C102 for chlorination and Sulfur Dioxide SO2 as the dechlorinating agent Residual Chlorine analysis of treated plant effluent validates efficacy of dechlorinating agent dosing and permit compliance Summary of Method Executive Summary West Hickman Laboratory uses a HACH AutoCAT 9000 autotitrator to perform Residual Chlorine determinations The AutoCAT 9000 bench top system automatically completes all USEPA approved amperometric titration methods for chlorine calculates analyte concentration and provides real time graphics display The AutoCAT s forward amperometric titration procedure has a range of 0 0012 mg L to 5 0 mg L with an estimated detection limit of 0 0012 mg L Discussion Chlorine hypochlorite ion hypochlorous acid and chloramines liberate iodine from potassium iodide at pH 4 or less in stoichiometeric proportions The iodine is titrated with a reducing agent phenylarsine and an amperometer detects the endpoint Although the actual measurement is that of the samples oxidation potentia
304. istance between riffles divided by the width of the stream is gt 25 Parameter 8 Bank Stability This metric measures whether the stream banks are eroded or have the potential to erode Each bank is scored independently from 10 0 Optimal Banks stable evidence of erosion or bank failure absent or minimal little potential for future problems lt 5 of bank affected Suboptimal Moderately stable infrequent small areas of erosion mostly healed over 5 30 of the bank affected Marginal Moderately unstable 30 60 of bank in reach has areas of erosion high erosion potential during floods Poor Unstable many raw eroded areas obvious bank sloughing gt 60 of bank has erosional scars Parameter 9 Bank Vegetative Protection This metric measures the amount of vegetative protection afforded to the stream and the nearstream portion of the riparian zone Each bank is scored independently from 10 0 Determine what vegetative types trees understory shrubs herbs and non woody macrophysics are present on each bank Those stream banks with different vegetative types provide better erosion protection and provide more of a variety of allochthonous food material Native vegetation scores higher than invasive or non native vegetation Wolf Run Watershed Page 47 of 67 Revision No 0 Based Plan Date April 11 2011 Optimal gt 90 of the stream bank surfaces and immediate riparian zones covered by natural vegetation including
305. it relaxes The presence of DO in the process shortens the time it takes for the red light to be emitted By measuring the time lapse between when the blue light was transmitted and the red light is emitted a correlation is made to the concentration of DO in the effluent or other solution Between measurements a red LED is used as an internal reference The measurement range for the method is 0 02 20 0 mg L The Method Detection Limit MDL 40 CFR 136 Appendix B has been determined as 0 05 mg L and the Minimum Level ML Reference 15 4 has been set at 0 20 mg L 3 Health amp Safety Precautions 3 1 3 2 Glassware involved possible cut hazard All municipal and industrial wastewaters are potentially hazardous Gloves and safety glasses should be worn when dispensing these samples 39 SOP LAB D O LFUCG Laboratory Page 40 of 219 Revision Number 5 Last Revised 09 09 Sample Handling and Preservation 4 1 Sample must be collected in a glass bottle BOD bottle with stopper filled to top with no airspace 4 2 Sample must be analyzed immediately 15 minutes maximum on permit samples 4 3 There is no applicable preservative with this method Reagents 5 1 Nanopure Lab Water Equipment amp Lab Ware 6 1 HACH HQ40d portable multi meter 6 2 HACH Model LBOD101 01 probe with integrated stirrer 6 3 BOD bottles with 300 mL capacity and tapered ground glass stoppers 6 4 Sensor Cap replacements HACH part 5838000 6 5 LDO S
306. ive a label The label may be placed in the sample jar labels placed in the jar will be written in No 2 pencil on waterproof paper and written directly on some portion of the jar The label will include the site number if known stream name location county date sampled and the collector s initials TABLE 11 SUMMARY OF SAMPLING METHODS FOR MACROINVERTEBRATES Replicates Replicates Technique 1m kicknet seine Undercut banks roots Sticks Wood Emergent vegetation Bedrock slabrock J americana beds Leaf packs Sampling Device Kicknet seine and wash bucket D frame or triangular dip net and wash bucket Habitat Semi Quantitaive Riffle Multi Habitat Swee All applicable Composited for Wadeable Sites Composited for Headwater Sites 4 x 0 25m Riffle Run Pool Silt sand fine gravel US 10 Sieve Margins Aufwuchs sample 300 um nitrex sampler mesh Riffle Run Rock pick Wood sample Fine tipped forceps and wash bucket Pool o fef je Elo 15 total 5 each 5 small boulders 3 to 6 linear meters 2 linear meters After sampling has been completed all sampling gear will be thoroughly cleaned to remove all benthic macroinvertebrates so that specimens are not carried to the next site The equipment shall be examined prior to sampling at the next site to ensure that no benthic macroinverteb
307. ivity Thermometers 8 5 1 The laboratory has certified thermometers traceable to National Standards with 1 degree centigrade or finer subdivisions and a range which spans the various requirements of the analytical methods equipment temperature monitoring and checking for thermal preservation These traceable thermometers are recalibrated a minimum of every five years The laboratory maintains Certificates of Calibration that identify traceability of the calibration to National Standards 8 5 2 All other thermometers are calibrated against thermometers traceable to National Standards Liquid in glass and digital thermometers are calibrated annually Metal and continuously monitoring thermometers are calibrated at least quarterly Calibration factors are employed based upon the most recent calibration Refrigerators 8 6 1 Each refrigerator is uniquely identified and provided with a uniquely identified thermometer graduated in increments no larger than degree centigrade Thermometer readings are monitored and recorded each day the laboratory is in operation The monitoring logs include refrigerator and thermometer identification date time temperature initials of the responsible person and the acceptable temperature range 16 TB Laboratory QAP September 16 2009 Revision 1 8 6 2 The following table lists the refrigerators that are used in the Town Branch Laboratory Description Unique Identifier Range Roo
308. ix A Precision for pebble count readings will be such that each data point measures within 1 units of the narrative particle description or 0 5 phi units on the gravelometer Each pebble count will be performed twice once at the initial site visit and approximately nine months subsequent to first measurement For each sampling event particle size distributions and Dso values will be computed and differences between these two measurements will allow estimation of changes to channel substrate B2 2 6 Water Quality Monitoring Water quality monitoring will be conducted at ten 10 monthly sampling events at a minimum of twelve 12 sampling stations in the watershed during dry and wet conditions The sampling date within each month will be flexible such that at least two Wolf Run Watershed Page 50 of 67 Revision No 0 Based Plan Date April 11 2011 of the events will be considered wet weather and two of the events will be considered dry weather The FOWR Sampling Coordinator shall work with the Third Rock Sampling Coordinator to schedule sampling dates each month A minimum notice of 48 hours is required prior to mobilization of the volunteer samplers During the monthly sampling grab samples will be collected by volunteers and delivered within six hours of collection to the LFUCG Town Branch laboratory for analysis of E coli fecal coliform total suspended solids ammonia nitrite total dissolved solids alkalinity an
309. l Width of riparian zone gt 18 m human activities parking lots roadbeds clear cuts lawns pastures or crops have not impacted the zone Suboptimal Width of riparian zone 13 18 m human activities have impacted the zone only minimally Marginal Width of riparian zone 6 12 m human activities have impacted the zone a great deal Poor Width of riparian zone lt 6 m little or no riparian zone due to human activities All habitat assessments will be completed by October 31 2011 and submitted to the FOWR Sampling Coordinator The FOWR Sampling Coordinator will compile these results into an electronic Microsoft Excel database The database along with electronic copies of the field datasheets will be submitted to Third Rock by November 30 2011 for incorporation into the final report discussing the results of the habitat assessments and the macroinvertebrate survey B2 2 5 Hydrogeomorphic Assessment Three types of measurements will be made in the hydrogeomorphic assessment cross sections longitudinal profiles and pebble counts These measurements will be made at each of the nine hydrogeomorphic monitoring sites Permanent monuments consisting of rebar 0 75 inch rebar or similar material approximately 4 feet long concreted within a plastic pipe casing shall be installed at the permanent cross section survey sites A monument shall be installed on both the right and left stream banks at least 10 ft back Wolf Run Watershed Page 48 of
310. l it is calculated and expressed as mg L Cl because chlorine is the dominating oxidizing agent present Health amp Safety Precautions Glassware involved possible cut hazard Wastewater samples have the potential to be hazardous use appropriate caution 12 SOP WH Residual Chlorine West Hickman WWTP Laboratory Page 13 of 219 Revision Number 4 Last Revised 09 09 Sample Handling and Preservation 4 1 Residual chlorine is subject to dissipation by exposure to sunlight mechanical agitation exchange of gases with the atmosphere and reaction with compounds in the wastewater over time For these reasons chlorine residuals should be analyzed immediately within 15 minutes of sampling time 4 2 The sample should be taken gently into a glass 300 mL BOD bottle completely filling to above the base of the neck and installing the tapered glass stopper in a manner that precludes air bubbles in the sample 4 3 All glassware used in this method must have no chlorine demand therefore do not use plastic containers and pre treat glassware accordingly To remove chlorine demand from clean glassware soak in a dilute bleach solution 1 mL commercial bleach to 1 liter of Nanopure water for at least one hour After soaking rinse thoroughly with Nanopure water After analysis thoroughly rinse all glassware with Nanopure water to reduce the need for pretreatment Reagents 5 1 Reagent 1 Potassium Iodide 5 5 2 Reagent 2 pH 4 00 Buffer Certi
311. l measure sample temperature upon receipt determine if sample aliquots have been placed in appropriate bottles and properly preserved and inspect the sample for proper identification and bottle integrity any discrepancies and or bottle damage shall be documented on the COC If the hold time requirement is exceeded for any parameter the result is qualified and a re sampling must be scheduled B3 3 Sample Labeling Whenever possible during field preparation while in the office sample bottles will be labeled to prevent information omission Bottles can be labeled in the field as long as the following minimum requirements for labeling are followed All bottles must have the following information recorded either on a sample tag or label affixed to the container or written directly on the container e Sample identification unique site ID number e Date of collection Wolf Run Watershed Page 54 of 67 Revision No 0 Based Plan Date April 11 2011 Time of collection formatted in military time or indicate am or pm Type of analysis requested Type of sample grab composite semi quantitative multi habitat Media surface water biological macroinvertebrates Preservative ice acidification etc e Collector s initials For macroinvertebrate samples the stream name and location will also be documented on the label B3 4 Sample Designation Sampling technicians will be responsible for recording the unique sample identification a
312. l 15 minutes Decant 125 mL of sample and pour into the Boiling flask Add 125 mL of Nanopure water to the Boiling flask Swirl to mix Add 5 mL of 1 1 Sulfuric Acid to the Boiling flask Swirl to mix Connect flask to a condenser and adapter tube Distill at a rate of 5 mL min Make sure tap water is running and cooling the condenser Set timer for 5 20 and 20 more minutes Collect the first 15 mL of distillate in 20 mL graduated cylinder and discard This takes approximately 5 minutes Collect 150 mL of distillate in an Erlenmeyer flask This takes approximately 20 minutes While wearing leather gloves disconnect Boiling flask from distillation unit Transfer the Erlenmeyer flask to the hot plate insert thermometer and stopper Heat to 90 C 5 C This takes approximately 20 minutes While wearing finger gloves remove flask from hot plate Add 10 drops of Phenolphthalein Indicator Swirl to mix Titrate drop wise with 0 1 N Sodium hydroxide NaOH using the Brand Digital Buret II until first persistent pink color is obtained Record in bench sheet end point date sample collected date analysis performed time analysis started and initials 91 10 11 8 2 8 3 SOP Volatile Acids LFUCG Laboratory Page 92 of 219 Revision Number 3 Last Revised 09 09 Recovery Factor Determination To determine the recovery factor f 1 Dilute 1 9 mL of glacial acetic acid in 1 L Nanopure water 2000 mg L ac
313. label one bottle Blank 3 and add 4 mL of seed solution Siphon dilution water into BOD bottles until full Measure initial DO for each and record in bench sheet Replace any displaced dilution water stopper cap and incubate at 20 1 C for 5 days The 5 day BOD at 20 C should have a depletion of 0 6 to 1 2 mg L Dilution water Quality Control QC Unseeded Blank 1 2 3 4 Siphon 300 mL of dilution water into BOD bottle Take initial DO and record in bench sheet Replace any displaced dilution water stopper cap and incubate at 20 1 C for 5 days The 5 day DO should be 0 2 mg L of initial DO BOD standard preparation Quality Control QC check 1 2 3 4 5 6 7 Obtain Glucose Glutamic Acid BOD standard from the Micro Refrigerator located under the fecal incubators Allow the standard to warm up to room temperature before using Using a sterile 10 mL pipette add 6 mL BOD standard into BOD bottle labeled Standard Siphon dilution water into BOD bottle until full Take initial DO and record in bench sheet Replace any displaced dilution water stopper cap and incubate at 20 1 C for 5 days The 5 day BOD of the standard should be 198 mg L 30 5 mg L 18 8 2 SOP CBOD LFUCG Laboratory Page 19 of 219 Revision Number 5 Last Revised 09 09 8 1 10 Sample preparation 1 Place the sample volume indicated on the bench sheet into each labeled sample BO
314. lan Date April 11 2011 hand picking of rocks large cobble small boulder from riffles runs and pools aufwuchs material off rocks sticks leaves and filamentous algae and visual searches of large woody debris All samples collected with the dip net and the rock and wood samples will be processed through a 600um wash bucket Results of qualitative sampling from each microhabitat will be combined to form one composite sample for each station Samples will be preserved in 95 percent ethanol and returned to the laboratory for processing and identification All organisms will be identified to the lowest possible taxonomic level and recorded on laboratory data sheets Random 300 specimen subsamples will be removed from the riffle samples using methods described by KDOW 2009b Habitat assessments will be performed by trained volunteers accompanied by Third Rock personnel at each of these sites Visual assessments will be made to document riffle and pool substrates stream channelization riparian conditions and in stream cover Habitat assessment procedures will follow those outlined in Rapid Bioassessment Protocols for Use in Wadeable Streams and Rivers Barbour et al 1999 A6 1 4 Watershed Habitat Assessments In addition to the habitat assessments conducted at the macroinvertebrate sites habitat assessments will be performed by trained volunteers throughout the watershed on parcel sized or 100m stream reaches Using the visual based habitat a
315. lan in order to verify that sampling techniques are consistent with the intended use of the data Sampling equipment is selected and pre cleaned to preserve sample integrity and eliminate contamination Accepted samples are logged upon arrival and checked for sampling preservation and holding times Indelible ink is used for all written documentation associated with samples Corrections to sampling documents are made by a single line strikeout The corrected entry is written above the strikeout and initialed by the person making the correction Samples must be received with complete documentation in the form of a Chain of Custody COC record including sample identification location date and time of collection collector s name sample type person receiving sample and any special remarks COC Records The different COC records used at Town Branch Laboratory are 1 Town Branch 24 hour composite samples with COC record delivered to the Town Branch Lab by the night Operator at midnight the night before 2 Town Branch grab samples with COC record delivered to the Town Branch Lab each morning by the on duty Operator 3 Town Branch solids grab samples and composite samples with COC record delivered to the Town Branch Lab each morning by the Solids Operator 4 West Hickman grab and composite samples are on one COC record delivered to the Town Branch Lab each morning by the West Hickman on duty Operator 23 TB Laborato
316. lanned corrective actions e Implementation schedule for planned corrective actions Notification of Invalid Data In the event that the results of the internal audit indicate that the laboratory s test results are invalid immediate corrective action is taken All persons are notified who received the invalid data 38 TB Laboratory QAP September 16 2009 Revision 1 Section 20 Annual Review of the Quality Assurance Plan QAP 20 1 Scope The QAP is reviewed annually The Laboratory Supervisor conducts an internal review with the Quality Assurance Officer The laboratory in its review determines whether requirements of the QAP have been adequately addressed the results of the annual review must be documented 20 2 Correcting Deficiencies in the QAP If the Laboratory Supervisor and Quality Assurance Officer find deficiencies the QAP is revised as necessary The revised QAP is then issued with the appropriate version number and implemented at the agreed upon effective date All copies of the preceding version are replaced with the new version 39 TB Laboratory QAP September 16 2009 Revision 1 21 1 21 2 21 3 21 4 Section 21 Training and Personnel Requirements Scope and Training Objectives All personnel involved in laboratory analysis or quality assurance quality control shall have sufficient training to allow for the analysis and reporting of complete high quality data in compliance with the procedures of
317. lassware accordingly To remove chlorine demand from clean glassware soak in a dilute bleach solution 1 mL commercial bleach to 1 liter of Nanopure water for at least one hour After soaking rinse thoroughly with Nanopure water After analysis thoroughly rinse all glassware with Nanopure water to reduce the need for pretreatment Reagents 5 1 Reagent 1 Potassium Iodide 5 5 2 Reagent 2 pH 4 00 Buffer Certified Acetic Acid Both reagents are located adjacent to the AutoCAT unit 5 4 Phenylarsine Oxide Standard Solution 0 00564 N 5 5 Chlorine Standard Solution 25 30 mg L as Cly Equipment amp Lab Ware 6 1 HACH AutoCAT 9000 Chlorine Amperometric Titrator 6 2 Beakers 250 mL 6 3 Graduated Cylinders 250 mL 6 4 1 mL fixed volume Finnpipette and 1 mL tips 6 5 Stirring bars Interferences 7 1 Accurate determinations of free chlorine cannot be made in the presence of Nitrogen trichloride or Chlorine dioxide Td Some organic chloramines can also interfere 13 Free halogens other than chlorine also will titrate as free chlorine 7 4 Interference from copper has been noted in samples taken from copper pipe or after heavy copper sulfate treatment of reservoirs 7 5 Contamination of probe by metal ions such as copper silver iron interfere with amperometric titrations Fouled electrodes will not produce sharp endpoints 23 SOP Residual Chlorine LFUCG Laboratory Page 24 of 219 Revision Number 4 Last Revised 09 09 7 6
318. ld find on a topo map Sign the Relinquished by portion and witness the individual receiving the sample signing the Received by section e Take your sample directly to the lab at the UK Mines and Minerals Building Rose Street 3 Floor Call for an appt before you go or make arrangements with your collection coordinator listed below Important Phone Numbers 1 800 928 0045 Ext 473 Volunteer Support Lab 606 257 5500 606 846 4905 Project Headquarters Dr Francis or Alice Shelly Watershed Watch Chain of Custody Record 3 Normal 4 Bank Full 5 Flood This form must accompany your sample Make a copy for yourself then send the original on its way with your sample runner If you have questions or difficulties please contact us at 1 800 928 0045 Ext 473 SURFACE WATER STATIONS IN DOWNSTREAM ORDER FOR WHICH RECORDS ARE PUBLISHED IN THIS VOLUME Letters after station name designate type of data d discharge e stage c chemical b biological t water temperature s sediment Page STATION NUMBER OHIO RIVER BASIN Ohio River BIG SANDY RIVER BASIN Levisa Pork head af Big Sandy River Grapevine Creck near Phyllis d ooo oo ooo me Ste ce teats abn WOO TAOS A 39 Russell Fork at Haysi VA o o 03208500 oo 40 Levisa Fork at Pikeville ld o o ee eee 0320950 aaa aa 4 Johns Creek near Meta do 03210000 oo 42 Levisa Fork at Paintsville d 00 ee ee eee 03212500 o 43
319. le This reagent is composed of several acids that react with the alkaline species in the sample resulting in a change in sample pH The observed pH reading after the addition of the reagent varies directly with the total alkalinity Each pH reading corresponds to a unique value for alkalinity expressed in mg L ppm CaCO The alkalinity values are obtained in a chart that cross references with the pH values 2 2 Discussion Alkalinity of water is its acid neutralizing capacity Raw domestic wastewater has an alkalinity less than or slightly higher than in the water supply Properly operating anaerobic digesters have a supernatant alkalinity in the range of 2000 4000 mg CaCOy L Some samples are diluted No color change is noted Health amp Safety Precautions 3 1 Watch out for broken glass from beakers and cylinders 32 Wastewater samples have the potential to be hazardous use appropriate caution Sample Handling and Preservation 4 1 Samples should be run as soon as possible Reagents 5 1 Total Alkalinity Reagent Orion 700011 5 2 Alkalinity Standard Control 1000 ppm Orion 700012 5 3 Nanopure Water SOP Alkalinity LFUCG Laboratory Page 3 of 219 Revision Number 2 Last Revised 9 09 Equipment amp Lab Ware 6 1 Fisher AR50 ph Meter using a glass electrode and reads to 0 05 pH units 6 2 100 mL volumetric flask for standard 6 3 100 mL graduated cylinders 6 4 Appropriate size beakers to contain samples and reage
320. le undisturbed 3 Add CyaniVer 4 powder pillow Shake for 10 seconds and immediately proceed to next step 4 Immediately add CyaniVer 5 powder pillow Shake the cell vigorously for 15 seconds 5 Set timer for 30 minutes 6 If there is any cyanide present the sample will turn blue 8 1 3 Using the DR4000 spectrophotometer on positive reaction 1 Fill a round sample cell with 10 mL of filtrated sample this will be used as the BLANK 2 Touch HACH Programs on keypad and select program 1750 Cyanide 28 10 11 12 SOP Free Cyanide LFUCG Laboratory Page 29 of 219 Revision Number 3 Last Revised 09 09 3 Place BLANK sample into DR4000 cell holder Close the light shield Touch Zero to zero instrument 4 Place the prepared sample into the cell holder Close the light shield Results will appear as mg L cyanide 8 2 Helpful Hints 1 Make sure that the CyaniVer 5 powder pillow is added immediately after the 10 second shaking period from the previous reagent 2 Ifinterference is present the sample will turn into a cloudy murky solution QA QC Requirements 9 1 Use free cyanide standards Expected Results Every now and then a positive reaction occurs If it is higher than the limit posted on the industrial waste laboratory report red number inform the Laboratory Supervisor immediately 10 1 KPDES Permit Requirements Depends on the particular industry being sampled Data Analysis and Calculati
321. le al evan thai as 3 SECON OTE 4 Organizational Chtt ii asa 4 3 1 Laboratory s Place in Company and Laboratory OrganizatiON oooconcconcnonnnoccncnnnncnnnos 4 3 2 Laboratory s OCIO dida 4 A E ONO 5 4 1 NR TN 5 4 2 QAP Documentation Control Procedures ooooocnooccconocccoooncnononcnonanononononnnonononanononnnonns 5 4 3 SOP Documentation Control Procede 5 4 4 Forms Data Sheets Documentation Control Procedures oooonccnincononnnoccnnnnnconnccanacnnos 5 PSC CL A ES 6 Laboratory s Approved Signatories ii 6 5 1 Approved SIM a OTIS scores oct Sev atesan vse aces ve ciessis os Neos ec ncesaues eases hates vs recone 6 NT 7 General Quality Control Procedures and Practices ui tisytans eels 7 6 1 Documentation of Test Methods and Laboratory PracticeS oooooonnccinncnnncononncncncnnnnss 7 6 2 General Quality Control Guidelines did 7 6 37 Method Bla ia A A reine Aten aang Ae eas a 7 GA IV A ios gate sacs we asec ese o a eee n as caste ge mare sa ceet 8 6 5 Laboratory Control Mm Ad 8 6 6 Matrix Spike Duplicates and Sample DuplicatesS ooonconinconinnnnnnnnncnconncconocinnacannnonnnos 9 6 7 Quality Control Charts and Tabulations oooonccnnnccninnnnocnconnconncconocono nono nono ncconocnnccnnnno 9 6 8 Initial Demonstration of Method Performance Studies IDMP ooooonnccccnonccccconncinnns 10 6 9 Method Detection Limits MDL a 11 GLO Internal AUCs slot 11 6 11 Analytical Quality Control StandardS ooooccnnccnonocioccnon
322. leon 6 8 browser then choose either System 1 Fluoride or System 2 all other anions including Bromide and TKN 18 Go to last run sequence click to highlight and go to file click save as This will load the method of interest and a template for the current sequence run 19 The sequence is edited to reflect the method and samples that are to be run a SYSTEM2 NITRATE for Fluoride b SYSTEM2 NITRATE for Bromides c SYSTEM2 TKN for TKN and Total Nitrogen Note Data is reprocessed in the section of Chromelon 6 8 called Sequence integration editor Only operators with a minimum of three months experience in Ion Chromatography should attempt to reprocess data for this analysis Once data is optimized then the nitrogen values from nitrate and nitrite analysis can be subtracted from this value for the TKN nitrogen value If only Total Nitrogen is needed then use the optimized data value without the correction for nitrite and nitrate nitrogen d SYSTEM 2 NITRATE for all other anions 20 Observe the reading on the screen of the CD20 Conductivity Detector A conductivity rate change of lt 0 03 uS over a 30 second time span is considered stable for analysis 21 If using the GP50 pump it will take about 15 30 minutes for the CD20 system to stabilize If using the IP25 it will take between 30 minutes to 2 hours for stabilization 22 Once the CD20 is stabilized the Dionex DX500 Ion Chromatography System is ready to start standardization NOTE
323. les into appropriately labeled precleaned containers 8 The digested QC and samples along with the corresponding data sheets are to be transferred to the IC for analysis OB NS E Prep Batching 1 Log on to the Labworks system 2 Click on Edit Data 3 Enter the SDG number or choose it from the list 4 Click on OK 5 Click on OK 6 In the row for TKN prep work TKN_PREP enter a 1 under the number of each sample completed and save it 7 Exit system 6 Quality Control A duplicate sample should be prepped at the frequency of one per every twenty samples sufficient sample permitting or one per SDG whichever is greater The RPD should be less than 10 If this difference is exceeded the duplicate may need to be reprepped The QC s value should fall between 10 of its theoretical concentration as well Ls 7 References Standard Methods for the Examination of Water and Wastewater 20 edition 1998 Method 4500 N C pg 4 102
324. liBlue24 broth simultaneously detects and identifies both total coliforms and Escherichia coli E coli Summary of Method 2 1 Executive Summary The sample is filtered through a 0 45 um Millipore membrane filter The filter is placed on a Pall filter pad containing media in a sterile Petri dish The samples are then incubated at 35 0 C 0 5 C for 24 hours 2 hours Colonies are counted blue colonies are enumerated as E coli and other coliforms are red total coliforms are the sum of the two 2 2 Discussion m ColiBlue24 is a single step MF procedure that incorporates specific non coliform growth inhibitors and a selective enzymatic indicator to allow for simultaneous detection and quantitation of both E coli and total coliforms Fecal coliforms are defined as The major species of gram negative non spore forming rods is Escherichia coli which indicates fecal pollution and the presence of enteric pathogens m ColiBlue24 method has been approved by the U S EPA for monitoring drinking water and wastewater using a 24 hour incubation period It can also be used to detect coliforms in other types of water i e surface ground well recreational Health amp Safety Precautions 3 1 All municipal and industrial wastewaters are potentially hazardous Gloves and safety glasses should be worn when dispensing these samples 3 2 Possible exposure to enteric pathogens Care must be taken to avoid undue exposure 3 3 A flame is used to
325. ling Solution 63 SOP pH LFUCG Laboratory Page 64 of 219 Revision Number 3 Last Revised 09 09 Equipment amp Lab Ware 6 1 Fisher Scientific AR50 pH Meter 6 2 Stirrer probe Interferences 7 1 pH measurements are affected by temperature and can cause the reading to drift 7 2 Grease and other debris on the probe can cause inaccurate readings Procedures 8 1 Calibration 1 Before calibrating ensure the hole on the side of the pH probe is open 2 Weekly Replace Reference Filling Solution a Push down on probe to release filling solution b Insert Reference Filling Solution bottle tip into hole of probe and flush with solution c Refill probe with Reference Electrode Filling Solution until inner workings of probe are covered 3 Touch the meter screen anywhere until you hear a beep 4 Touch the pH button and wait until you hear a beep 5 Touch the std button on the upper right corner of the screen 6 Place probes into a beaker of Buffer Solution pH 7 00 yellow color coded Turn on stirrer 7 Touch the clear button to remove previous standardization 8 Write down the temperature of the buffer and determine what the pH for the buffer will be at this temperature from chart Temperature C Buffer Solution pH 7 00 yellow color coded 10 7 07 15 7 05 20 7 03 25 7 00 30 6 99 64 9 10 11 12 13 14 15 16 17 18 19 SOP pH LFUCG Laborato
326. logical and physical wastewater treatment processes and for assessing compliance with regulatory agency effluent limitations The settled volume of a biological suspension is useful for routine activated sludge plant control 2 2 Discussion Settleable matter is measured volumetrically with an Imhoff Cone and a Settlometer after 1 hour A 1000 mL sample of mixed liquor is allowed to settle and readings are taken after 30 minutes and at 1 hour intervals thereafter Health amp Safety Precautions 3 1 Wastewater samples should be considered potentially hazardous Use proper personal protective equipment Sample Handling and Preservation 4 1 Samples should be collected in plastic or glass containers 4 2 No preservative is required 4 3 Mixed liquor samples should be taken at effluent end of aeration tanks 4 4 Care should be taken to minimize floc break up during Settlometer analysis 4 5 Maximum holding time is 7 days Reagents 5 1 None required 78 SOP Settleable Solids LFUCG Laboratory Page 79 of 219 Revision Number 3 Last Revised 09 09 6 Equipment amp Lab Ware 6 1 Imhoff Cone 6 2 Settlometer 6 3 Timer 7 Interferences 7 1 None 8 Procedures 8 1 Imhoff Cone 1 2 3 4 5 Thoroughly mix samples and fill Imhoff Cones to the 1 Liter mark Set timer for Imhoff Cone samples for 45 minutes and additional 15 minutes After the Imhoff samples have settled for 45 minutes stir samples gently to re
327. loyees are routinely rotated through the different procedures 21 TB Laboratory QAP September 16 2009 Revision 1 Section 11 Procedures for Reviewing New Work 11 1 Scope Laboratory management reviews all new work to ensure the laboratory is able to perform the additional task s in a timely and accurate manner Laboratory management consults if necessary with sampling personnel and end data users to ensure sample integrity and data quality 11 2 Unknown Samples On occasions the Laboratory will receive and analyze samples from industrial pretreatment sources or samples brought in from other outside sources These samples are considered unknown samples for which duplicate sub samples are processed and analyzed All QA QC requirements apply to the unknown samples 11 3 Contract Analyses The laboratory does not perform contract analyses 22 TB Laboratory QAP September 16 2009 Revision 1 12 1 12 2 Scope Section 12 Sample Acceptance and Receipt Policy Sampling is critical to producing data representative of conditions that occur at the sampling location This section of the QAP constitutes the laboratory s written sample acceptance policy It details the conditions under which the laboratory will accept samples It is readily available to all laboratory staff and sample collectors Sample Acceptance Requirements 12 21 12 2 2 1223 12 2 4 12 2 5 The Plant Operator confirms the appropriate sampling p
328. ls or on society from the use of a material in the quantity and in the manner proposed Safety The reciprocal of risk probability nothing will happen Selenium Se Selenium derivatives are extremely Hepatotoxic Shifts When 6 or more daily values of the same control distribute themselves on one side of the mean value line but are maintaining a constant level indicates contamination of standard use of a new batch of reagents changes in temperature of water bath change in spectrophotometer bulb etc Solids Material in a solid state In water and wastewater treatment any dissolved suspended or volatile substance contained in or removed from water or wastewater Solids Colloidal Finely divided solids intermediate between dissolved and suspended particles Solids Dissolved Solids that are present in solution Solids Non settleable Wastewater matter that will stay in suspension for an extended period of time For laboratory purposes 1 hour Solids Settleable Matter that will not stay in suspension for 1 hour Matter that settles to the bottom of an Imhoff Cone within 1 hour Solids Suspended Matter that is suspended in and will not settle in an hour For laboratory purposes it is that matter that can be collected on a standard filter Solids Total The sum of the dissolved and non dissolved matter in wastewater The sum of all matter in a wastewater sample Solids Volatile The quantity of solids in waste
329. lts can be verified using sample dilutions or standard additions 6 5 Samples with severe interferences require distillation Perform the distillation procedure using the HACH General Purpose Distillation Set SOP NH LFUCG Laboratory Page 10 of 219 Revision Number 1 Last Revised 09 09 Procedures 7 1 7 2 TNT 830 ULR 0 015 to 2 000 mg L NH3 N 1 2 3 4 5 6 7 8 Carefully remove the protective foil lid from the DosiCap Zip Unscrew the cap from the vial Carefully pipet 5 0 mL of sample into the vial Immediately proceed to step 3 Flip the DosiCap Zip over so that the reagent side faces the vial Screw the cap tightly onto the vial Shake the capped vial 2 3 times to dissolve the reagent in the cap Verify that the reagent has dissolved by looking down through the open end of the DosiCap Zip Wait 15 minutes After 15 minutes invert the sample an additional 2 3 times to mix The color remains constant for an additional 15 minutes after the timer expires Thoroughly clean the outside of the vial with a Kim wipe Insert the prepared vial into the DR5000 cell holder Slide the lid closed The instrument reads the barcode then selects and performs the correct test Results are in mg L NH3 N TNT 831 LR 1 to 12 mg L NH3 N 1 2 3 4 5 6 7 8 9 Carefully remove the protective foil lid from the DosiCap Zip Unscrew the cap from the vial Carefully pipet 0 5 mL 500 uL o
330. luent Biological Phosphorus Removal Influent Biological Phosphorus Removal Effluent Analysis CBOD TSS CBOD TSS Total Phosphorus Ammonia Hardness Fecal Coliforms Metals Dissolved Metals Total Ammonia Settleable Total Phosphorus Ortho phosphate Volatile Acids Total Alkalinity Metals Dissolved Metals Total CBOD TSS CBODs Total Phosphorus Ortho phosphate Volatile Acids Total Alkalinity CBOD Total Phosphorus Ortho phosphate Volatile Acids Total Alkalinity Analysis Requirements Required Required Required Required Required Required Required Required Required Required Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation Operation TB Laboratory QAP Appendix A Revision 1 Sample Name Zone 1 Effluent Formerly Zone 1 M L Zone 2 Effluent Formerly Zone 2 Mixed Liquor Plant Effluent Creek Above Plant Creek Below Plant Return Activated Sludge R A S Belt Feed and Wastewater Combined Sludge Feed Filtrate Filter Belt Press Belt 1 Cake Solids Belt 2 Cake Solids Belt 3 Cake Solids Filter Belt Cake Analysis TSS VSS Total Alkalinity MLTSS MLVSS Total Alkalinity Settleable Ortho phosphate CBOD TSS Metals Total CBOD TSS Metals Total pH Total Alkal
331. lumetric flask partially filled with water then fill to volume Quality Control Standard Pipette 0 1 mL of 1000 mg L NaF from a separate source stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Quality Control Standard Pipette 0 4 mL of 1000 mg L NaF from a separate source stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Quality Control Standard Pipette 1 0 mL of 1000 mg L NaF from a separate source stock standard into a 1000 mL volumetric flask partially filled with water then fill to volum Calibration Standards for the SYSTEM2 NITRATE Bromide method are prepared as follows 1 2 Calibration Standard 1 Pipette 2 mL of 1000 mg L NaBr stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Calibration Standard 2 Pipette 5 mL of 1000 mg L NaBr stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Calibration Standard 3 Pipette 10 mL of 1000 mg L NaBr stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Quality Control Standard Pipette 8 mL of 1000 mg L NaBr stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Outside Source Certified Quality Control Sample ERA 4 Procedure A Instrument Preparation 1 Sie Before turning on
332. ly 2 of the 4 regimes present if fast shallow or slow shallow are missing score low Poor Dominated by 1 regime usually slow deep Parameter 4 Sediment Deposition This metric measures the amount of sediment that has accumulated in pools and changes that have occurred to the stream bottom as a result of deposition This may cause the Wolf Run Watershed Page 45 of 67 Revision No 0 Based Plan Date April 11 2011 formation of islands point bars areas of increased deposition usually at the beginning of a meander that increases in size as the channel is diverted toward the outer bank or shoals or result in the filling of runs and pools Sediment is often found in areas that are obstructed and areas where the stream flow decreases such as bends Deposition is a symptom of an unstable and continually changing environment that becomes unsuitable for many organisms Examine bars shoals and pool substrates within the biological monitoring station when assessing this parameter Optimal Little or no enlargement of islands or point bars and less than 5 of the bottom affected by sediment deposition Suboptimal Some new increase in bar formation mostly from gravel sand or fine sediment 5 30 of the bottom affected slight deposition in pools Marginal Moderate deposition of new gravel sand or fine sediment on old and new bars 30 50 of the bottom affected moderate sediment deposits apparent at most obstructions and slow areas be
333. ly calculate the unknown concentration Peaks at the same or approximately the same retention times are compared The unknown concentration can be calculated from using this ratio Remember that when dilutions are being run that the correct dilution factor must be entered before you will get the correct result C When possible the unknown should be bracketed between two knowns and the calculation of the unknown made from both for comparison 6 Quality Control A quality control sample obtained from an outside source must first be used for the initial verification of the calibration standards A fresh portion of this sample should be analyzed every week to monitor stability If the results are not within 10 of the true value listed for the control sample prepare a new calibration standard and recalibrate the instrument If this does not correct the problem prepare a new standard and repeat the calibration A quality control sample should be run at the beginning and end of each sample delivery group SDG or at the frequency of one per every ten samples The QC s value should fall between 10 of its theoretical concentration A duplicate should be run for each SDG or at the frequency of one per every twenty samples whichever is greater The RPD Relative Percent Difference should be less than 10 If this difference is exceeded the duplicate must be reanalyzed From each pair of duplicate analytes X and X2 calculate their R
334. ly streamside of sample container handling collection and preservation and requires the volunteer to demonstrate competency 3 Planning a Synoptic Sampling Event a Sampling Event Coordinator For each synoptic sampling event the Basin Steering Committee identifies a Sampling Event Coordinator who communicates with the receiving laboratory concerning o Arrangements for receiving samples see Section 8 o Standards for analysis see Section 9 and o Standard reporting spreadsheet including flags for samples outside of standard receiving temperature and holding time lab report see Section 10 The Sampling Event Coordinator also e Assembles packets of containers and corresponding instructions to Supervising Samplers e Makes arrangements for Drop Off Centers and Runners as indicated b Selection of laboratory Watershed Watch uses laboratories that meet at least one of the following criteria e Listed on the KDOW Certified Drinking Water Lab List e Currently providing contract work for KDOW or e Approved by EPPC microbiological staff 4 Sampling Site Selection a Objectives The site selection process in Watershed Watch attempts to accommodate its two major purposes e The interest of the Volunteer Monitor who often desires to focus learning activities on a stream reach where she or he lives works learns or plays and e The need of the program and its stakeholders to collect information from a stream reach ne
335. lyte b the MDL of the measured concentration for that analyte in any environmental sample in the batch or c categorical limits such as found in BOD analysis TB Laboratory QAP September 16 2009 Revision 1 6 3 3 When method blank acceptance criteria are not met any non detect results in the associated batch of environmental samples are reported with qualification 6 3 4 Section 15 Corrective Action Policies and Procedures references procedures for taking corrective actions when blanks do not meet acceptance criteria 6 4 Matrix Spikes 6 4 1 For all test methods performed by the laboratory in which materials suitable for matrix spiking are available matrix spikes are performed at a rate of one per sample set of similar matrix type per sample extraction or preparation procedure 6 4 2 The laboratory utilizes the spiking analytes specified in the test method When the test method indicates that all method analytes are to be matrix spiked then the laboratory spikes all analytes of interest 6 4 3 Samples are selected on a rotating basis for matrix spike analysis from among various waste streams monitoring locations and other applicable locations 6 4 4 Procedures used to select samples and analytes for spiking are documented 6 4 5 Each analytical SOP references quality control criteria to use in determining discrepancies and accepting data when matrix spikes do not meet acceptance criteria 6 4 6 Section 15 Corrective Action Poli
336. m Temperature Storage Unit Room Temp Storage Unit 10 30 C Microbiology Station Refrigerator 1 4 0 2 0 C Pretreatment Sample Storage Refrigerator 2 4 0 2 0 C Town Branch Sample Storage Refrigerator 3 4 0 2 0 C West Hickman Sample Storage Refrigerator 4 4 0 2 0 C Chemical Storage Refrigerator 6 4 0 2 0 C 8 6 3 Samples which require thermal preservation are stored under refrigeration which is 2 C of the specified preservation temperature unless method specific criteria exist For samples with a specified storage temperature of 4 C storage temperatures of 4 0 2 0 C are acceptable 8 7 Incubators 8 7 1 Each incubator is uniquely identified and provided with a uniquely identified thermometer graduated in increments no larger than 1 C Thermometer readings are monitored and recorded each day the laboratory is in operation The monitoring logs include incubator and thermometer identification date time temperature initials of the responsible person and the acceptable temperature range 8 7 2 The following table lists the incubators that are used in the Town Branch Laboratory Description Unique Identifier Range BOD Incubator BOD Incubator 1 20 0 1 0 C BOD Incubator BOD Incubator 2 20 0210 Coliform Incubator Bath Precision 1 44 5 0 2 C Coliform Incubator Bath Precision 2 44 5 0 2 C Coliform Incubator Bath Precision 3 35 0 0 2 C 8 8 Ovens 8 8 1 Each oven
337. mediate riparian zone covered by native vegetation including trees understory shrubs or non vegetation but one class of plants is not well represented disruption evident but not affecting full vegetation disruption obvious patches of bare soil or closely cropped vegetation common less covered by vegetation disruption of streambank vegetation is very high vegetation has been woody macrophytes plant growth potential to any than one half of the removed to 5 centimeters vegetative disruption great extent more than potential plant stubble orless in average stubble through grazing or mowing one half of the potential height remaining height minimal or not evident plant stubble height almost all plants allowed to remaining grow naturally Left Bank 10 9 8 1 6 5 4 3 2 1 0 Right Bank 10 9 8 7 6 5 4 3 2 1 0 Width of riparian zone gt 18 Width of riparian zone 12 Width of riparian zone 6 Width of riparian zone lt 6 meters human activities i e parking lots roadbeds clear cuts lawns or crops have not impacted zone Left Bank 10 9 Right Bank 10 9 18 meters human activities have impacted zone only minimally 8 7 6 8 7 6 J Forms and Templates Technical Data Sheets and Checklists Streams Habitat Assessment Field Data Sheet high doc 12 meters human activities have impacted zone a great deal 5 4 3 5 4 3 meters little or no riparian vegetatio
338. method If there is a difference then once the pump control is turned over to remote control irreversible damage and destruction of suppressors columns piston seals and check valves on the GP50 Gradient Pump will occur NEVER switch from bottle C to A B or D without flushing the system lines with water to remove all traces of eluent from bottle C from the lines B Sample Preparation 1 Ifthe sample was not filtered in the field it must be done so now Transfer 50 mL of a well mixed sample to the filtering apparatus Apply the suction and collect the filtrate 2 Ifthe conductivity values for the sample are high dilution will be necessary to properly run the sample within the calibration standard range Dilutions are made in the Polyvials with the plastic Filter Caps If the dilutions are gt 20X then volumetric glassware is required 3 All dilutions are performed with reagent grade DI water Be sure to mix the dilution well 4 For the anions TKN and Total Nitrogen first pipette 0 05 mL of 100X sample spiking eluent into the Polyvials then pipette 4 95 mL of the filtered samples on top of the spiking eluent The Filter Caps are pressed into the Polyvials using the insertion tool 6 Place the Polyvials into the Sample Cassette which is placed into the Autosampler The white black dot on the Sample Cassette should be located on right hand side when loaded in the left hand side of the Automated Sampler for System 2 8 For ev
339. minutes another sample must be obtained and analyzed 9 2 A Check Standard pH 6 86 must be analyzed on Sunday Expected Results 10 1 KPDES Plant Effluent Permit Requirements 1 6 0 mg L is the lowest pH allowed 2 9 0 mg L is the highest pH allowed In the event that analysis results indicate values greater then KPDES permit requirements retest If the value indicated by the retest is greater than KPDES permit requirements Immediately notify the Plant Superintendent and the Laboratory Supervisor 10 2 Process Ranges Typical values for each plant are Town Branch Influent 7 3 7 4 Town Branch Effluent 6 7 8 9 West Hickman Influent 7 1 7 4 West Hickman Effluent 6 4 7 7 Blue Sky Influent RESTS Blue Sky Effluent 6 0 7 3 Data Analysis and Calculations 11 1 None required Bibliography 12 1 U S EPA Method 150 1 pH Electrometric Issued 1971 Editorial revision 1978 and 1982 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 12 2 AR50 Fisher Scientific User Manual Fisher Scientific 67 SOP pH LFUCG Laboratory Page 68 of 219 Revision Number 3 Last Revised 09 09 12 3 Code of Federal Regulations CFR 2003 Guidelines Establishing Test Procedures for the Analysis of Pollutants 40 CFR 136 3 Title 40 Chapter 1 U S Environmental Protection Agency U S Environmental Protection Agency
340. move suspended solids that may be on the surfaces of the Imhoff Cone After the Imhoff samples have settled for additional 15 minutes record the amount of settled solids in mL L Record date of sample date analysis completed and initial in bench sheet 8 2 Mixed Liquor 1 2 3 4 5 Thoroughly mix sample without aerating the sample and fill Settlometer to the 1 Liter mark Set timer for Settlometer sample for 30 minutes 1 hr 2 hr 3 hr and 4 hr After the Settlometer sample has settled for 30 minutes record the amount of settled solids in mL L Observe mixed liquor throughout the 4 hour time span If the blanket rises before 4 hours record the rise time in the bench sheet If after 4 hours the blanket has not risen record gt 4 hours for rise time in bench sheet Record date of sample date analysis completed and initial in bench sheet 9 QA QC Requirements 9 1 None Required 79 10 11 12 SOP Settleable Solids LFUCG Laboratory Page 80 of 219 Revision Number 3 Last Revised 09 09 Expected Results 10 1 KPDES Permit Requirements 10 2 1 No permit requirements Process Ranges Typical values mL L for each plant are Town Branch Influent 4 74 10 64 Town Branch Effluent 0 02 0 26 West Hickman Influent 8 65 20 61 West Hickman Effluent 0 02 0 25 Data Analysis and Calculations 11 1 Record as milliliters per liter 11 22 Always read the top of the solids column
341. mple into the cell holder Close the light shield Results will appear as mg L cyanide 8 2 Helpful Hints 1 Make sure that the CyaniVer 5 powder pillow is added immediately after the 10 second shaking period from the previous reagent 2 If interference is present the sample will turn into a cloudy murky solution QA QC Requirements 9 1 Use total cyanide standards Expected Results Every now and then a positive reaction occurs If it is higher than the limit posted on the industrial waste laboratory report red number inform the Laboratory Supervisor immediately 10 1 KPDES Permit Requirements Depends on the particular industry being sampled 32 11 12 SOP Total Cyanide LFUCG Laboratory Page 33 of 219 Revision Number 3 Last Revised 09 09 Data Analysis and Calculations 11 1 None required Bibliography 12 1 HACH DR 4000 Method 8027 HACH Company Loveland CO 12 22 Lachat Micro Dist User Manual Method Cyanide in Waters MICRO DIST Cyanide 1 Lachat Instruments HACH Company Loveland CO 12 3 U S EPA Method 335 4 Revision 1 0 August 1993 Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 U S Environmental Protection Agency Office of Research and Development Washington DC 1982 33 SOP Cr 6 LFUCG Laboratory Page 34 of 219 Revision Number 3 Last Revised 09 09 Chromium Total and Hexavalent Cr o TNT HACH Method 10219 Chromium Total TNT HACH Method 10
342. mpling Design Rationale O 32 B1 2 1 Karst Hydrograph Characterization merino ria ici 32 B12 2 Cond ctivity S VEy 201 aa 34 B1 2 3 Benthic Macroinvertebrate Collection oooooccinncninnoconccconnconcnonanconncconocnnos 34 B1 2 4 Watershed Habitat AssessmentS ooconoccinocinococonoconnconncconccconocnnn cono conan ccoo coins 34 B1 2 5 Hydrogeomorphic ASsessMent ccsccesccessecesseceseceseceeceesseecseeceeeeeeeeees 34 B1 2 6 Water Quality Monitor iii 35 B2 Sampling Methods AAA AR A A a id 36 B2 1 Sampling Equip ea to dal ta ad o ou els 36 B22 Sampling CUS erase ce A do Noa 36 B2 2 1 Karst Hydrograph Characterization ceseecceseceneeeeeeeeeeeceaecneeeneeeneeenees 36 B22 2 Conductivity Survey x x jiescctias sh aa enna ated 39 Wolf Run Watershed Page 6 of 67 Revision No 0 Based Plan Date April 12 2011 B2 2 3 Benthic Macroinvertebrate Collection cococcccncncnnnnnnnnnnnnnnonononononinononos 40 B2 2 4 Watershed Habitat AssessmentS ooconoccinncnoococonncoonconncconccconocnnn cono conan cconncinns 44 B2 2 5 Hydrogeomorphic Assessment jacssacsadslsisscessavsssessansestiaszsdacssetvass tees taraasdeddss 48 B2 2 6 Water Quality Monitoring iii didas 50 B3 Sample Handling and Custody Requirements oooooocccnoccccconcccconcnononcnonononicnnono 53 B31 A A O 53 B3 2 Sample Handling and Transpotrt ccccccccsseceseceeeceesceeeeceeceeeeeeeeeeecsecneenaes 54 BI Sample brea e E ae
343. n Watershed Based Plan Page 32 of 67 OD versailles Rd Alexandria Dr Streams mxd 3 30 2011 9 29 34 AM las N N ES wn N E x Ss ra E Ge 2 E ES wW a o lt ej 2 2 E x lt WwW WolfRun Mapping GIS QAPP 030_LFUCG Map Document P Project_Files Kentucky KY 10 Tates Creek Rd The six gaging locations in the watershed allow for the evaluation of the discharge at the mouth of the watershed W1 Prestons Spring W2 Vaughn s Branch tributary W4 Wolf Run upstream of Cardinal Run W6 Wolf Run at the edge of the karst basin W9 and Big Elm Tributary which flows into the sinkhole at Picadome W11 In the event that the capacity of the sinkhole downstream of W11 is exceeded and surface water flows from Big Elm Tributary into Vaughn s Branch this surface flow will be measured at W11A in order to measure the input into the karst system at this site B1 2 2 Conductivity Survey Specific conductance was recently listed as a cause of impairment in the Wolf Run watershed Although specific conductance or conductivity has been analyzed during several studies and the FOWR conducted a broad study of conductivity levels in the watershed a subsequent study under more normal flow conditions will aid in identifying inputs and problem areas Conductivity is a measure of water s ability to conduct an electric current and it indicates the concentration of dissolved ions in the water Rapid changes
344. n due to human activities 01 31 08 Conductivity Survey Field Datasheet Genral Info Stream Name Segment ID Date Sampler Name Cond Meter ID Measurements to be made at least 100 f p M ft apart in each segment starting Calibration upstream and working downstream Known Value 714 yS om Initial Calibration yS cm Final Calibration Known Value 1438 yS cm Initial Calibration Siom Final Calibration Additional Notes Pebble Count Datasheet Stream Date Station Survey Crew Ao e aa A e e e m fosos o o lp m foros 2 K E E E EEES E E A l Lozz os me sze T Logro ma ens iaia ha ff E Parras veycoarse 45 04 COBBLE Casso emm 0 128 sort tage 128 180 raro age 180 200 eee Fros 143 souner omar 269 082 T uso omar sees gt 20 40 mes ata tore CT soso ige ozu YO Temor beses TT E E AA AAA SE os9 126 coarse 226 32 OC CHAIN OF CUSTODY Page 1 of 1 Client Third Rock Consultants LLC LFUCG Analytical Report to Project Name Wolf Run Watershed Based Plan mwootonOthirdrockconsultants com Project KY10 030 Division of Water Quality Marcia L Wooton Project Contact sampling Marcia L Wooton Third Rock Consultants LLC Phone 859 977 2000 Town Branch Laboratory 2526 Regency Road Collected By 301 Lisle Industrial Avenue Lexington Suite 180 Kent
345. n numerical value such as TNTC is unacceptable because you cannot average non numerical values e For samples in which subsequent dilutions do not produce a discrete value and are too numerous to count report results as 60 000 You would also use this value in the geometric mean calculation KDEP DMR Manual 2009 F To calculate the Geometric Mean G E D e Zeros shall be recorded as lt 1 e To calculate the logs of numbers with greater than less than and approximately equal to sign drop the sign Do the math and then replace the sign as shown below e Ifa column has only numbers without signs and numbers with less than signs then the total of this column will have a less than sign e Ifa column has numbers without signs numbers with less than signs and numbers with greater than sign then the total of this column will have a less than sign 52 SOP Fecal Coliform LFUCG Laboratory Page 53 of 219 Revision Number 3 Last Revised 09 09 e Ifa column has only numbers without signs and numbers with greater than signs then the total of this column will have a greater than sign e Ifa column has any numbers with approximately equal to signs then the total of this column will have an approximately equal to sign Example Fecal Coliform 100 mL Logarithm 100 2 00000 50 1 69897 lt 1 0 00000 10 1 00000 60 1 77815 80 1 90309 150 2 17609 gt 60000 4 77815 lt 83 15 33445 15 33445 8 1 91681 1 91681
346. n under pressure Watch out for broken glass from beakers and cylinders Wastewater samples should be considered potentially hazardous Use proper personal protective equipment Sample Handling and Preservation 4 1 Collect samples in plastic or glass bottles that have been acid cleaned with 1 1 Hydrochloric acid solution and rinsed with Nanopure water 4 2 Donot use commercial detergents containing phosphate for cleaning glassware used in this test 4 3 Analyze samples immediately after collection for best results 44 If prompt analysis is impossible preserve samples for Total Phosphorus up to 28 days by adjusting the pH to 2 or less with concentrated Sulfuric acid about 2 mL per liter and storing at 4 C 4 5 Samples to be analyzed for Reactive Phosphorus should not be preserved with acid store Reactive Phosphorus samples at 4 C and analyze within 48 hours 4 6 Warm stored samples to 15 25 C and neutralize with 5 0 N NaOH before analysis if acid has been added Reagents 5 1 Phosphorus Reactive and Total TNTplus LR Reagent Set HACH TNT843 5 2 Phosphorus Reactive and Total TNTplus HR Reagent Set HACH TNT844 5 3 Phosphorus Reactive and Total TNTplus UHR Reagent Set HACH TNT845 5 4 Nanopure Water 5 5 Phosphate Standard Solution 100 mg L as PO Equipment amp Lab Ware 6 1 HACH DRB200 Reactor with Test N Tube block and safety shields 6 2 TNTplus reactor adapter sleeves 16 mm to 13 mm diameter 6 3 HACH
347. n verification and maintenance are found in the analytical method SOPs or sample preparation SOPs Manufacturers operation manuals may be referenced in the method SOPs when they are the source for calibration or maintenance procedures Documentation is maintained for all maintenance calibration and instrument operation activities All defective equipment is removed from service and is not returned to operation until repaired and shown by calibration certification or test to perform satisfactorily An adequate number of standards are used to define the calibration curve The test method SOP states if the calibration curve is linear or non linear If the test method does not state the number of calibration standards to use the laboratory will use a minimum of 7 concentrations to create the calibration curve The range should be within the linear range of the curve and should correspond to values typical for the samples Unless specified by the test method the lowest calibration standard is set at 1 to 15 times the MDL whenever sample results will be used in a decision related to the determination of a non occurrence of an analyte or a non detect the MDL of an analyte All sample results for test methods utilizing a calibration curve are reported within the highest calibration standard or within the linear dynamic range where the test method requires determination of the linear dynamic range Further guidance regarding calibration may be fo
348. nation during the sampling process a Completing the Chain of Custody form The Watershed Watch Chain of Custody form Appendix F serves to document and record the transfer of the samples from the stream to the laboratory functions as a field measurement form and provides a place for field observations Listed below are data elements of the form Sample identification the following information is preprinted on the form by the Steering Committee s Data Manager e Site Number e Stream Name e Watershed Number e Sampling Location e County e Name of and contact information for Supervising Sampler The following identifying information is entered by the Supervising Sampler streamside when the sample is taken e Date and Time of sample collection e Corrections to any preprinted information Field measurements The following information is entered by the Supervising Sampler when and where the sample is taken Comments on general stream conditions Flow Flow Rate Rain in past 48 hours Dissolved oxygen pH Temperature e Conductivity Signatures The Supervising Sampler signs the form at the time she or he relinquishes it to the laboratory or to the next person who will have custody of the sample as it is transported to the laboratory Signatures are annotated by the date and time they are signed b In stream sampling location and approach Samples are taken by wading to reduce sample contamination A maximum safe wa
349. nconncnnnnconnccono cono nonn cono nccnnccnnos 12 612 IRC ACIS id 12 O AS e a da el Sed Seat e bn 12 6 14 Labotatory P te Wa a dane AAA 12 SECA os 13 Verificatio Prada N 13 7 1 Performance Evaluation PE Testing ccccesccceseceseceesceesceceseceeeeeeeenseeesaeeneenees 13 7 2 Standard Reference Materials sic i2 29s haiat sacs ncdataiiewtacticba acs eunacdouthe caunasantneia ids 13 7 3 Internal Quality Control ProgramSs s seseseesseseesseessessesseessesssesresseessesresseessessressesse 13 TB Laboratory QAP September 16 2008 Revision 1 O ed 15 Equipment Procedures for Calibration Verifications and Maintenance ooooonnccnoccnccconanoncnnnonos 15 8 1 Equipment Calibration nnie necnin eee a a a wise Naas E 15 A O 16 8 3 PMsn e ed 16 84 Conductivity MS A eae aa 16 8 5 Thermometers A da da 16 8 6 Refrigerators cies cases srl aS cise tne ect tues EE dene nad ta Eea EE 16 Ga TL0 110 eE E E A E ees setae ete sa ee ee ee 17 8 8 A ale aaa II ccd ned EE EE edld aes 17 8 9 Other Laboratory Equipment unn i 18 RG CHOON O 252g scp a uate ra ees ce aioe wc aes a deena Chace aah earns ar ac e E 19 Test Methods and SOPS tice kc tatela sri tattle ta hes datas tala tat T ote Salil tales helene te 19 9 1 A OTAN 19 9 2 Standard Operating Procedures SOPs cccccsccessseeseeessecseceeeeeeeeeeaeeceaeceteeneeeeeseees 19 Section LOren NS 20 The Laboratory s Physical Facilities Including Services and Resource
350. ndling and Preservation 4 1 Collect samples in plastic or glass containers that have been washed with a detergent and rinsed with tap water 1 1 Nitric Acid Solution and Nanopure water 4 2 Analyze immediately or perform preservation 4 3 To preserve the sample add 1 5 mL of Nitric Acid per liter of sample Check the sample to assure that the pH is 2 or less 4 4 Store samples at 4 C or below 60 SOP Hardness LFUCG Laboratory Page 61 of 219 Revision Number 2 Last Revised 09 09 Reagents 5 1 Hardness 1 Buffer Solution 5 2 ManVer 2 Hardness Indicator Powder Pillow 5 3 0 800 M EDTA Titration Cartridge Equipment amp Lab Ware 6 1 HACH Digital burette 6 2 100 mL graduated cylinder 6 3 Porcelain dish 6 4 Stirrer and magnet Interferences 7 1 Some metal ions interfere by causing fading or indistinct endpoint or by stoichiometric consumption of EDTA 7 2 Suspended or colloidal organic matter also may interfere with the endpoint Procedures 8 1 Steps 1 Attach a clean horse shoe bent delivery tube to a 0 800 M EDTA Titration Cartridge connected to the HACH digital burette 2 Flush the delivery tube by turning the delivery knob on the burette to eject a few drops of titrant Reset the counter to zero and wipe tip 3 Measure 100 mL of sample with a clean 100 mL graduated cylinder 4 Pour the sample into a clean porcelain dish 5 Add 2 mL of Buffer Solution Hardness 1 and stir 6 Add the contents of
351. ndom variation are acceptable Each lab and method may have its own The Town Branch Lab utilizes 2 Standard Deviation which includes 95 of the values in a Gaussian distribution Control A fluid or substance whose physical and chemical properties closely resembles unknown test specimen whose mean value has been assayed and is used as verification or check on a test procedure Chromium Cr Only the trivalent and hexavalent forms of chromium are of biologic significance Chromium in ambient air originates from industrial sources are refining and combustion of fossil fuels Copper Cu Wilson s disease is characterized by excessive accumulation of copper in liver brain kidneys and cornea Cyanide CN Cyanide is commonly found in certain rat and pest poisons metal polishes photographic solutions and fumigating products Density The ratio of weight mass to volume of a material DO Dissolved Oxygen EPA U S Environmental Protection Agency Iron Fe Acute iron toxicity is nearly always due to accidental ingestion of iron containing medicines and most often occurs in children Filterable Residue Dissolved solids and colloidal solids Fluoridation The addition of a chemical to increase the concentration of fluoride ions in drinking water to a pre determined optimum limit to reduce the incidence of dental caries in children Frequency distribution A graphic usually bar representation of a set of values r
352. nds and pools Poor Heavy deposits of fine material increased bar development more than 50 of the bottom changing frequently pools almost absent due to substantial sediment deposition Parameter 5 Channel Flow Status This metric measures the degree to which the channel is filled with water The score will change with the seasons Estimate the percentage of the channel that is wet using the low water mark Optimal Water reaches base of both lower banks minimal amount of channel substrate exposed Suboptimal Water fills gt 75 of the available channel or lt 25 of channel substrate exposed Marginal Water fills 25 75 of the available channel riffle substrates are mostly exposed Poor Very little water in channel mostly present in pools Parameter 6 Channel Alteration Both Sheets This metric measures the large scale direct changes in the shape of the stream channel Channel alteration is present when 1 artificial embankments rip rap and other forms of bank stabilization or structures are present 2 the stream is very straight for significant distances because of channelization 3 dams and bridges are present that obstruct flow and or 4 dredging or other substrate mining activities are occurring or have occurred Optimal Channelization or dredging absent or minimal stream with normal pattern Suboptimal Some channelization present usually in areas of bridge abutments evidence of past channelization dred
353. netic filter membrane Pour a small amount of sample 10 mL or less into the funnel and let it collect in the suction flask When the entire sample has drained through stop suction disconnect the suction hose from one flask at the plastic connector junction Remove both the magnetic funnel and the magnetic filter membrane together do not disturb the filter and carefully lower a 50 mL glass collection tube into the suction flask Reconnect the apparatus and filter the sample into the collection tube Once filtered measure out 50 mL of sample and transfer it into a 100 mL plastic beaker measure using a graduated cylinder This may require two separate filterings 2 Add 1 mL of 12 N HSO and 4 mL of ammonium molybdate antimony potassium tartrate to all standards and sample samples Swirl to mix thoroughly 3 Add 2 mL of ascorbic acid solution to all standards and samples Swirl to mix 1 thoroughly C Sample Analysis Place each standard and or sample under probe submersing probe in solution swirl gently tap probe releasing bubbles and read or pour into cuvet and read 2 The computer by comparing the concentration of each calibration standard against its absorbance can plot a calibration curve If above criteria is not met the standards may need to be remade and rerun 3 Once the spectrophotometer is standardized properly the samples may be analyzed 4 When completed print out a copy of the standard values
354. nies 100 mL mL A V x 100 Averages Date Sample Collected Time Sample Collected Time Sample Received by Laboratory Date Analysis Started 01 00 00 01 00 00 01 00 00 01 00 00 01 00 00 E 01 00 00 01 00 00 01 00 00 01 00 00 01 00 00 01 00 00 01 00 00 01 00 00 01 01 00 01 00 00 01 00 00 01 00 00 01 00 00 01 00 00 01 00 00 _ S ER SY Y Time Analysis Started Set up Analyst Date Analysis Completed Time Analysis Completed Reading Analyst 01 01 00 01 01 00 01 01 00 01 01 00 01 01 00 A EEES Note Plates should be read within 24hrs 2Hrs of set up time Total Coliforms Method TC Fecal Coliforms Method FC Fecal Strep Method FS 01 01 00 01 01 00 01 01 00 01 01 00 01 01 00 OOOO QUALITY CONTROL MANAGER IS TO RECEIVE A COPY OF ALL QC RESULTS Presevation Cool 4 C Maximum Holding Time 6 hours KPDES Permit Limits on Plant Effluent 200 100mL for Monthly GED 400 100mL for Maximum Weekly GED TOWN BRANCH amp WEST HICKMAN WASTEWATER TREATMENT PLANT Town Branch Laboratory 24 Hour Composite Samples pH Method EPA Method 150 1 pH Electrometric Issued 1971 Editorial revision 1978 and 1982 Enter Date 7 00 pH 4 00 pH 10 00 pH Second Calibration Sst Bor J econd Buiter i Baier Calibrated By pH Meter Calibration Temperature Slope
355. nomic and Enumeration Efficiency Form and included in the monitoring report Wolf Run Watershed Page 56 of 67 Revision No 0 Based Plan Date April 11 2011 B5 3 Chemical Laboratory Quality Controls Laboratory quality controls will be analyzed as specified in the SOPs listed in Quality Assurance Plan QAP and Standard Operating Procedures SOPs Price 2009 These controls include method blanks matrix spikes calibration check samples laboratory replicates and other method specified controls The frequencies of analysis for these standards are all specified by the individual methods B6 Instrument Equipment Testing Inspection Calibration and Maintenance Requirements Laboratory instrumentation will be maintained according to the SOPs listed in Table 5 Field sampling equipment will be maintained as specified in KDOW 2009b and Table 12 The record of inspection calibration and maintenance will be recorded in a instrument logbook maintained by the sampler For sampling nets and bottles inspection will ensure that the items are free from contamination in good condition and adequate for use TABLE 12 FIELD EQUIPMENT CALIBRATION AND MAINTENANCE Standard or Equipment Name Type Multimeter for Temperature pH Dissolved Oxygen and Conductivity Equipment Purpose Physicochemical Monitoring Inspection Frequency Before each collection event Type of Inspection Overall condition battery power Calib
356. nts 6 5 Repipettors 1 mL 5 mL and 10 mL and tips Interferences 7 1 Substances such as salts of weak organic and inorganic acids present in large amounts may cause interference in the electrometric pH measurements 7 2 Oil and Grease by coating the pH electrode may also interfere causing a sluggish response Procedures 8 1 Steps 1 Calibrate pH meter see SOP pH Section 8 2 Check alkalinity of Nanopure water Any alkalinity in the water used for diluting will contribute to the total alkalinity measured in the control eno re Measure 100 mL of Nanopure water into 150 mL beaker Add 1 0 mL Alkalinity Reagent and insert pH probe Turn on stirrer Read pH value when the meter displays STABLE Determine total alkalinity of the Nanopure water using the Low level chart 0 25 ppm and multiply result by 0 9 This value AH20 is the contribution to total alkalinity from Nanopure water 3 Check alkalinity of Standard gt o pes Measure 10 mL of Alkalinity Standard into 100 mL volumetric flask and dilute to mark with Nanopure water Pour standard into 150 mL beaker Add 10 mL of Total Alkalinity Reagent and insert pH probe Turn on stirrer Read pH value when the meter displays STABLE Obtain alkalinity value A from the Full chart 0 225 ppm by cross referencing with pH value Determine alkalinity of standard Asta Asta A AH20 Value should be 100 5 ppm 10 SOP Alkalinity LFUCG Labo
357. nvestigation ProcedUr Si A 36 17 4 Complaint Response Procedures iii 36 A E A A A ssh aA 37 Procedures for Protecting Confidentiality and Proprietary Rights ooooncconnccnoconicococacinanocnnonos 37 18 1 Procedure for Protecting Confidentiality 0 0 00 cece ccececeseceeeeeeseeeeseceeeeeeeeenseeenaeees 37 18 2 Examples of Confidential Data ij wcsaseasctssestiss tisteesstnstansnntiahsstacdbeadiuotandoMarsd dacsdeedansd 37 18 3 Procedure for Open Records Requests ccccecsceesseceteceeeceeeeeeseecaeeeeeeeseeeeseeesaeenes 37 LE O O E a A 38 Procedures for ADS VR Ainas 38 19 1 Annual Internal Audit sc csgacsts i tasnacvea eared 38 19 2 Corrective Actions Regarding the Annual Internal Audit 0 0 00 eeeeeeeeeeteeneeees 38 19 3 Notification of Invalid Datac accion teo de a do 38 Section 20 ia ida 39 A RN 39 20 2 Correcting Deficiencies in the DA dl e 39 A E E E E E E E E E aces alate Mea eta a area ales 40 Training and Personnel Requirements pio al 40 21 1 Scope and Training Objectives axes a is 40 21 2 Training Required for Laboratory Supervisor ocooccnnoconococoncnonnnonnnonnnonono conc connccnnncnnns 40 21 3 Training Required for Quality Assurance Officer oooooonoccnncnoccnocccononannoncnancnnccnonnnonos 40 21 4 Training Required for Technicians miii di dida dada 40 21 5 Additional Training for TechnicianS ooononcnnonononnconncconacnnnnonnncnnnccono cnn conan nonnccon cons 41 21 6 Substituting Experience or Education t
358. o Meet Training Requirements 41 21 7 Instrument Training Requirements dades 41 27 Traning Records las 41 IA AN TO 42 TB Laboratory QAP September 16 2008 Revision 1 MSIOSS A A O ee eh ta tae a T E N 42 Y ES A O A E ieee uel wt ceca Pale eek i etal oi E A 51 Bibliography msndsn iera a e E EE A A acess A sion Aiea ae 51 APPENDIX A LABORATORY ANALYSIS LIST c ccocooocnnnninnnnnnnnnonnncncnnnnnnonccnonnnncnnnonononcnnnos A 1 Table Al Town Branch Laboratory Analysis LiSt oooconnnccincnnnoconocaconnconnnnnncconnccono cono nonnnoos A 2 Table A2 West Hickman WWTP Analysis List cccccecscesssecsseceeeceeeeceeeeeeseecsaeeneeeeeeensees A 5 Table A3 Blue Sky WWTP Analysis Lista za A 7 Table A4 Data Provided to the Laboratory by Operations Staff oooooonnccninccinocicococoncconnconnnon A 8 APPENDIX B STAFF RESPONSIBILITIES ccccccccccsssscecessssceceesseeececssseesecsesseseceesses B 1 APPENDIX C CURRENT PERSONNEL AND LAB APPROVED SIGNATURES C 1 TOWN BRANCH LABORATORY STANDARD OPERATING PROCEDURES 0 064 1 a A A A a Ean 2 Biochemical Oxygen Demand BODA 15 Total Residual Chlorine Analia RA a a A AAA i 22 Eres Cyanide UN LE as 27 Total Cyanide NN a TE 30 Chromium Total and Hexavalent Cr dt 34 Dissolved Oxygen Analysis DO id A Aa 39 Fecal Coliform Membrane Filter Procedure ooooonnncnincononcconcnnoonconncconoconononn nooo nccononnnnncnn conos 44 m ColiBlue24 Method for t
359. o filter unit before dispensing sample Turn on vacuum after the sample is introduced For sample volumes 5 to 50 mL use sterile pipettes for dispensing into filter unit Do not touch the inside of the filter holder unit Do not allow the pipette tip to touch the filter For sample volumes 50 to 100 mL pour sample into cylinder and use the scale on the side of the cylinder for measurement 56 16 17 18 19 20 21 22 23 24 25 26 27 28 29 SOP Total Coliforms and E coli LFUCG Laboratory Page 57 of 219 Revision Number 1 Last Revised 09 09 Turn on vacuum Once sample has filtered through turn off vacuum Rinse top of the filter unit with peptone two times using autoclaved peptone in a Nalgene squeeze bottle Turn on vacuum to drain peptone Turn off vacuum Flame forceps Remove top of the filter unit and place on the sterile blue field Open Petri dish Use sterile flamed forceps to grab the edge of the filter and remove it from the filter holder unit Place filter grid side up onto edge of the Petri dish and gently slide it onto the surface of the media saturated pad Check for trapped air under the filter and make sure the filter touches the entire pad Replace the Petri dish lid Place Petri dishes into a 4 5 X 9 inch sterile sampling bag Make sure not contaminate the inside of the bag Seal bag Place bag with Petri dishes face down into water bath at 35
360. ods Part 4500 Cl D Chlorine Residual Amperometric Titration Method 1 1 2 1 2 2 3 1 3 2 Scope Significance to Process and Application Disinfection by chlorination is considered to be the primary mechanism for the inactivation destruction of pathogenic organisms in wastewater treatment plant effluents and to prevent the spread of waterborne diseases to downstream users and the environment Final clarifier effluent is treated with chlorine as enters the chlorine contact tanks allowing contact time for disinfection to transpire Final effluent is then treated with a dechlorinating agent reducing chlorine residual concentration to within acceptable limits see Section 10 1 Permit Limits Complete dechlorination is necessary to prevent chlorine related adverse effects on the receiving environment Town Branch Waste Water Treatment Plant uses Chlorine Dioxide C102 for chlorination and Sulfur Dioxide SO2 as the dechlorinating agent Residual Chlorine analysis of treated plant effluent validates efficacy of dechlorinating agent dosing and permit compliance Summary of Method Executive Summary Town Branch Laboratory uses a HACH AutoCAT 9000 autotitrator to perform Residual Chlorine determinations The AutoCAT 9000 bench top system automatically completes all USEPA approved amperometric titration methods for chlorine calculates analyte concentration and provides real time graphics display The AutoCAT s forward amperometric titrat
361. oduero atp vaya yojedojs aq dors Aoy qayemdoys ayy ses IUO puooas aq pue julod Surpreys oy SIJALA IFULIO ay SE Or SLI vosaad 3817 SUL od eya susan D RRIS BINA geago Bu MOLE OU ORN 193 0 awg Y aid oF prod Surpeys MoA oaoql yas Joy 9y olur aguezo ue doiq plua suj Jo pura yora Je uosiad g UOITISOg iampendais amg DDUBISIP 1SHOYS passed al A oa 4 or f eget E A se ere Oe B ASN 438 999 GJ 1940 JO B SOLIBA WANS MOA JO AZIS MI JF JO MOS AIBA SI MOLL ap J sajorisqo pe o TOWRTSISA jo a044 pue yjoours Yqwens oq pmoys DISH SERBS HOG SE JDOJSA UEIS SULINSBIJA es quod yep 1e weans equ Jo qadop aq 108 01 ojod INOA JO plua 19 DU 2INSEIMA HAY Y 110J10G wgons a soyonor R nun oSpuq ou Moy aod Z OP BA STRAIT 300 OMI Pag UAS OY SSOLOR IUS RIKAS ANA 40 BAIDU ayeudordde ue ye pasaras Sus SuLnsesul IRO PANS OF IBPWHS JO SISOH 04 sq F SIC AY SUNNE NOA PIOIIY CE yous 72 peodoy sons Suunevaur poread E nod 9313 03 syuotuainseau dap yya pire omy wnep jejuozuoy ayy gaera O 93 1 40 IPU Se Yous yieLupULy Y pur opqissad se opis BULONUOW INOA 0 ASOJ Se ONS Y puy stuRONS Sumo pusuemad 304 ASP SY PAQUIEQDS MP Wo SJUOUISINSLOWI OSOY ONE poys nod eas ap fo ped 307 de Aap yey SP9QUIRADS peus JO y sdj AfDOJSA X 1991 bS 1932M jO Bale puonjDaS 55049 SY49 MOJ WeaHS St WRAS 2 JO MOP Sy SALNSKOUL JOJ POLLO OY WRIQIIP 94001 Moy WEIS SULINSEITA
362. of the Dissolved Oxygen bench sheet under Temperature and Dissolved Oxygen from HQ40d Note the barometric pressure value from the laboratory barometer located adjacent to the D O meter and record on the dissolved oxygen calibration section of the Dissolved Oxygen Bench sheet under Barometer Reading On the Lab computer open the excel spreadsheet entitled DO Meter Calibration Sheet and enter the barometric pressure temperature and dissolved oxygen values from the dissolved oxygen calibration section of the Dissolved Oxygen Bench sheet The spreadsheet will calculate the Dissolved Oxygen Calibration Point the Dissolved Oxygen Y 1 ATM and the Slope Transfer the three values onto the dissolved oxygen calibration section of the Dissolved Oxygen bench sheet then print a copy of the spreadsheet and file it in the yellow file located adjacent to the D O meter Note the difference between the Dissolved Oxygen from HQ40d and the Dissolved Oxygen Calibration Point if it is greater than 0 2 mg L then the calibration is not acceptable and must be repeated until criteria is met If sample measurements are made in the afternoon the meter must be calibrated again due to changes in atmospheric pressure Repeat steps in Section 8 1 1 8 1 2 Measurements 1 2 3 4 Make sure that the meter is properly calibrated Rinse the LBOD probe tip with Nanopure water Place the probe into BOD bottle filled to the
363. on DC 1982 Standard Methods Part 2540 D Total Suspended Solids Dried at 103 C to 105 C APHA American Public Health Association Standard Methods for the Examination of Water and Wastewater 21 edition ed American Water Works Association and Water Pollution Control Federation Washington DC 2005 Code of Federal Regulations CFR Guidelines Establishing Test Procedures for the Analysis of Pollutants 40 CFR 136 3 Title 40 Chapter 1 U S Environmental Protection Agency U S Environmental Protection Agency pg 5 337 2003 Simplified Laboratory Procedures for Wastewater Examination Water Pollution Control Federation Third Edition pg 23 24 1985 Environmental Express Inc http www envexp com index asp 2009 84 SOP Total Solids LFUCG Laboratory Page 85 of 219 Revision Number 3 Last Revised 09 09 Total Solids EPA Method 160 3 Residue Total Gravimetric Dried at 103 105 C Standard Methods Part 2540 B Total Solids Dried at 103 105 C Scope Significance to Process and Application 1 1 This method is applicable to drinking surface and saline waters domestic and industrial wastes 1 2 The practical range of the determination is from 10 mg L to 20 000 mg L Summary of Method 2 1 Executive Summary Total solids are the material residue left in a vessel after evaporation of a sample and subsequent oven drying at a defined temperature Typically total solids include total suspended solids TSS
364. on species formate and acetate elute between fluoride and chloride The water dip or negative peak that elutes near and can interfere with the fluoride peak can usually be eliminated by the addition of the equivalent of 1 mL of concentrated eluent 100X to 100 mL of each standard and sample Alternatively 0 05 mL of 100X eluent can be added to 5 mL of each standard and sample Because bromide and nitrate elute very close together they can potentially interfere with each other It is advisable not to have Br NO3 ratios higher than 1 10 or 10 1 if both anions are to be quantified If nitrate is observed to be an interference with bromide use of an alternate detector e g electrochemical detector is recommended Method Interferences may be caused by contaminants in the reagent water reagents glassware and other sample processing apparatus that lead to discrete artifacts or elevated baseline in ion chromatograms Samples that contain particles larger than 0 45 micrometers and reagent solutions that contain particles larger than 0 20 micrometers require filtration to prevent damage to instrument columns and flow systems If a packed bed suppressor column is used it will be slowly consumed during analysis and therefore will need to be regenerated Use of either an anion fiber suppressor or an anion micro membrane suppressor eliminates the time consuming regeneration step by using a continuous flow of regenerant Because of the possibilit
365. on their route prior to sampling in order to coordinate swift collection and transfer e Having sufficient cooler space to immediately chill samples transferred from Volunteer Monitors coolers e Communicating with the destination laboratory so it is prepared to accept the samples delivered e Fully understanding the delivery times required for samples and e Confirming that the numbering of sample containers corresponds to the number on Chain of Custody forms e Signing Chain of Custody Forms when receiving and relinquishing samples e Checking bottle caps to assure they are securely tightened avoid over tightening and e Packing samples carefully in the receiving container to prevent bottle breakage shipping container leakage and sample degradation 9 Laboratory Analysis Labs selected by Watershed Watch are asked to use standard methods of analyis 10 Data Management The laboratory sends its results to the project data manager The Data Manager coordinates review of copies of the printed report by the Sampling Event Coordinator Steering Committee Chair and Science Advisor for errors omissions and suitability Draft copies are sent to supervising samplers for review and comment Once approved by the Basin Steering Committee the monitoring data is posted on the basin web site and released at the annual conference 11 Quality Control and Assurance a How Watershed Watch Assures the Quality of its Data Quality Control and Assurance
366. onal recovery of each acid increases with increasing molecular weight 1 3 Calculations and reporting are on the basis of acetic acid 1 4 The method is often applicable for control purposes Summary of Method 2 1 Executive Summary Volatile fatty acids are classified as water soluble fatty acids up to six carbon atoms that can be distilled at atmospheric pressure because of co distillation with water A sample is acidified with sulfuric acid distilled and the distillate is titrated to the phenolphthalein end point with sodium hydroxide The volume of titrant is proportional to the volatile acids concentration Results are expressed as mg L as acetic acid 2 2 Discussion Acidity of water is its quantitative capacity to react with a strong base to a designated pH Acidity is a measure of an aggregate property of water and can be interpreted in terms of specific substances only when the chemical composition of the sample is known In this case 125 mL is distilled brought to 95 C and titrated until a slight pinkish color is obtained Health amp Safety Precautions 3 1 3 2 3 3 3 4 3 5 3 6 Watch out for broken glass from cylinders and beakers Wastewater samples should be considered potentially hazardous Use proper personal protective equipment Distillation flasks can be HOT use proper gloves when handling Mercury from broken thermometers can be a safety hazard Sulfuric Acid is used during this analysis Wear gloves gog
367. onia nitrite total dissolved solids alkalinity and hardness The Kentucky Geological Survey will analyze samples for total phosphorus ortho phosphorus total kjeldahl nitrogen and nitrate FOWR volunteer samplers will perform field measurements of turbidity dissolved oxygen specific conductance temperature and pH Third Rock will accompany the volunteers during each event to conduct discharge monitoring and will field filter ortho phosphorus samples Also due to the short time period in which wet weather events can be collected on the hydrographic rise two wet weather sampling events will be collected solely by Third Rock staff If for some reason volunteers are not able to perform the sampling Third Rock will collect all sampling parameters In addition to the monthly sampling volunteers will collect an additional four events within a 30 day period during the Primary Contact Recreation period May 1 to October 31 for E coli and fecal coliform to evaluate the geometric mean for the primary contact period A Third Rock staff member will accompany the volunteers during each event to conduct discharge monitoring Only flow E coli and fecal coliform will be collected during these events The LFUCG Town Branch laboratory will analyze the samples A6 2 Project Timetable The project schedule for each of the monitoring activities as well as the data analysis report completion and watershed based plan section revisions are shown in Table 4
368. onitoring day If multiple datasheets are necessary to cover a given stream segment the order of these datasheets must be indicated in the Segment ID by a dash and number value For instance if two datasheets were used on Wolf Run segment 1A these would be labeled 1A 1 and 1A 2 in the Segment ID on the datasheet Datasheets and photos will be submitted to the FOWR Sampling Coordinator to be compiled into a Microsoft Excel database The FOWR Sampling Coordinator will submit the electronic database scanned copies of the field datasheets and an electronic photo library to Third Rock by November 30 2011 Third Rock will use the data to produce GIS images of the watershed indicating hotspots A final report Conductivity Survey of the Wolf Run Watershed discussing the methods results and conclusions based on the monitoring will be completed by December 31 2011 B2 2 3 Benthic Macroinvertebrate Collection Sampling for benthic macroinvertebrates will be conducted according to the KDOW s Methods for Sampling Benthic Macroinvertebrate Communities in Wadeable Waters KDOW 2009c All sites are headwater sites except W1 which is sampled for macroinvertebrates under the MS4 permit and not under this project A collection event consists of a composited semi quantitative sample and a composited multi habitat sample Semi quantitative samples will be collected from a known area in order to indicate the macroinvertebrate community in th
369. ons 11 1 None required Bibliography 12 1 HACH DR 4000 Method 8027 HACH Company Loveland CO 29 SOP Total Cyanide LFUCG Laboratory Page 30 of 219 Revision Number 3 Last Revised 09 09 Total Cyanide CN T HACH Method 8027 Pyridine Pyrazalone Method with Distillation Lachat Instruments Method 10 204 00 1 X MICRO DIST Cyanide 1 Scope Significance to Process and Application 1 1 Measurement of the concentration of total cyanide in industrial waste water samples Summary of Method 2 1 Discussion The Pyridine Pyrazalone method used for measuring cyanide gives an intense blue color with free cyanide Health amp Safety Precautions 3 1 All municipal and industrial wastewaters are potentially hazardous Gloves and safety glasses should be worn when dispensing these samples 3 2 Cyanides their solutions and Hydrogen cyanide liberated by acids are very poisonous Both gas and solutions can be absorbed through the skin Latex gloves and safety glasses should be used 3 3 Industrial waste samples CyaniVer 3 CyaniVer 4 and CyaniVer 5 reagent powder pillows are used Also used during preparation for the distillation process is 0 75 mL of 7 11M sulfuric acid 0 79M magnesium chloride solution Latex gloves and safety glasses should be used 3 4 During the distillation process the use of heat resistant gloves and safety glasses are required Sample Handling and Preservation 4 1 Collect samples in glass or plastic bottl
370. onstant for an additional 15 minutes after the timer expires 8 Thoroughly clean the outside of the vial with a Kim wipe 9 Insert the prepared vial into the DR5000 cell holder Slide the lid closed The instrument reads the barcode then selects and performs the correct test Results are in mg L NH3 N Reagent blanks A reagent blank can be measured and the value subtracted from the results of each test performed in same reagent lot Use deionized water in place of sample in the Salicylate method TNTplus 830 831 or 832 test To subtract the value of the blank from a series of measurements 1 Measure the blank per step 3 2 Turn on the reagent blank option 3 The measured value of the blank should be displayed in the highlighted box Accept this value The reagent blank value will now be subtracted from all results until the function is turned off or a different method is selected Alternately the blank can be recorded and entered at any later time by pressing the highlighted box and using the keypad to enter the value Sample blanks Colored or turbid samples can cause high results To compensate for color or turbidity the procedure is repeated without the addition of the color forming reagent that is present in the DosiCap Zip 11 SOP NH LFUCG Laboratory Page 12 of 219 Revision Number 1 Last Revised 09 09 To determine the sample blank 1 Run the Salicylate method TNTplus 830 831 or 832 test but do not remove
371. or 15 seconds and place into the COD reactor Set the reactor timer to run for 30 minutes CAREFULLY vials are 150 C transfer hot vials to test tube racks and allow to cool to ambient temperature before proceeding Note Vials are under pressure until they cool See Sec 3 1 To each vial add 2 mL of sodium hydroxide solution 1 56N cap and shake to mix Turn the DR 4000 ON and allow the unit to go through its startup and self check routine Press the soft key under HACH PROGRAM type in the number 3036 and press ENTER The unit will respond by displaying HACH PROGRAM 3036 P Total TNT and request to be zeroed To the blank standards and samples add to each the contents of one PhosVer3 powder pillow cap and shake for 15 seconds to mix then allow a 2 minute reaction period before proceeding to step 11 Respiratory hazard See Sec 3 2 Note Step 11 must be completed within 6 minutes of the end of the 2 minute reaction period Place the reagent blank into the DR 4000 cell holder close the lid and press ZERO Make sure the instrument is reading concentration and FORM P One at a time place all the vials standards and samples into the unit Note and record the indicated values on the bench sheet If desired during the reading process the soft arrow keys can be use to select units of P PO or P20 although generally the P value Total Phosphorus will be recorded 26 10 8 2 S
372. or faster response stir at a slow to moderate rate When the measurement is stable store or record the pH and temperature values For the HQ40d meter data is stored automatically when Press to Read or Interval is selected in the Setup Measurement Mode When Continuous is selected data will only be stored when the key under STORE is pressed Store the pH electrode in pH storage solution when not in use See Sample collection preservation general storage and cleaning for more details Helpful Hints 1 2 3 Avoid strong acids and greasy samples Make sure that probe is thoroughly rinsed between samples so that cross contamination does not occur Storage of an electrode is based on how long the electrode will be stored how quickly the electrode needs to be used and the type of sample being measured For general storage use the HACH storage solution or a 3M Potassium chloride KCI solution SOP WH pH West Hickman WWTP Laboratory Page 10 of 219 Revision Number 3 Last Revised 09 09 4 A contaminated glass bulb or fouled electrode may cause slow response times Do not clean the bulb too often because the bulb life may shorten 5 To clean an electrode with general contamination immerse the electrode tip in 0 1N Hydrochloric acid HCl Then immerse the electrode in 0 1N Sodium hydroxide NaOH and again in 0 1N Hydrochloric acid each for a 2 minute period Rinse with Nanopure water and soak in Nanopure water for a
373. or is not found corrective actions are focused on review of the procedure and improvement of test method execution The test procedure is re validated by successful analysis of a second source standard or reference material Standard Reference Materials The laboratory uses standards that are traceable to Standard Reference Materials SRMs where available Internal Quality Control Programs 7 4 1 Statistical Process Control is generally used to establish batch acceptance criteria for analytical test results The test results for the laboratory control standard are evaluated annually to set limits for control charts Warning limits are set at 20 from the mean recovery and control limits are set at 30 13 TB Laboratory QAP September 16 2009 Revision 1 7 4 2 When a control limit is exceeded the analyst is required to respond in a manner that assumes something is wrong with the measurement system Whenever possible a response to an exceeded control limit includes the following e Inform the immediate supervisor of the control limit exceedance e Stop the analysis of samples if possible e Conduct a systematic investigation as soon as possible to locate the source of the problem e Take appropriate corrective action when a problem is located e Rerun samples to the last good laboratory control standard whenever possible e Document the control limit event including the details of the occurrence whether a problem was dete
374. orm of phosphates There are three major classes of phosphates 1 Orthophosphates fertilizer is major source 2 Polyphosphates detergents and cleaning agents are major sources and 3 Organic Phosphates biological waste is major source Organic Phosphates are also formed from orthophosphates during biological treatment of waste streams Analysis of Total Phosphorus includes all of the aforementioned forms of Phosphorus The reduction of Total Phosphorus levels throughout the wastewater treatment process is highly important as phosphorus concentrations in plant effluents must be low enough See Sec 10 1 Permit Requirements to avoid detrimental effects on the receiving environment such as algae blooms Summary of Method 2 1 Executive Summary Total phosphorus analysis at West Hickman Laboratory refers to the spectrophotometric analysis of all phosphorus forms in a water wastewater sample that has been digested 2 2 Discussion West Hickman Lab uses EPA approved HACH Method 8190 with a HACH DR 4000 spectrophotometer Method range is 0 0 to 1 1 mg L as Total P and 0 0 to 3 5 mg L as PO4 with an Estimated Detection Limit EDL of 0 06 mg L PO4 The sample is first subjected to an acid persulfate digestion at 150 C reducing all phosphorus forms to reactive form which reacts with molybdate reagent in an acid medium producing phosphomolybdate complex This complex is reduced with ascorbic acid forming a molybdenum blue color with
375. orrect to the best of my knowledge SIGNED DATE Lead Instructor Verification This is to verify that the volunteer listed above has completed the modules have initialed below Instructor Name print Date Initial Module Initial Module Grab Sample Collection Project Logistics and Quality Assurance Field Chemistry Habitat Assessment Note to lead instructor Return a copy of this form to your project registrar or to the Water Watch Office at 400 Fair Oaks Plaza Frankfort KY 40601 Att JoAnn Palmer 1 800 928 0045 Ext 473 PHYSICAL CHARACTERIZATION WATER QUALITY FIELD DATA SHEET FRONT LOCATION SO RIVERMILE_____ STREAM CLASS INVESTIGATORS FORM COMPLETED BY DATE REASON FOR SURVEY TIME Au Pa WEATHER Past 74 hours Has there been a heavy rain in the last days CONDITIONS a storm heavy O Yes a Ho rain a rain steady Air Temperature 6 rain a showers Other intemuttent a eloud cover a clear sunry SITE LOCATION MAP Draw a map of the site and indicate the areas sampled or attach a photgraph Stream Subsysiem Stream Type O Perennial O Intermittert O Tidal OColdyater O Warmwater Stream Origm Catchment Area knt Q Glacial O S pring fed QNon glacial montare QO Mixture of origins O Swamp and bog O Other PHYSICAL CHARACTERIZATION WATER QUALITY FIELD DATA SHEET WATERSHED FEATURES BACK Predommant Surrounding Landuse Q Forest O Conmercial Local Watershed NPS Pollution
376. ory and field duplicates on this project and is calculated as follows _ S D RPD y 100 2 where S first sample value original result D second sample value duplicate result The project standards for precision on in situ measurements and water quality grab samples are expressed in Table 5 The precision of in situ measurements will be assessed by one duplicate measurement during each sampling event The precision of the water quality grab samples will be measured by internal laboratory QC samples In addition to internal laboratory QC one field duplicate will be collected per sampling event A field duplicate or field replicate sample is a sample taken from the same location as the regular grab sample at the same time The sample is used to assess variability of environmental conditions at sampling sites For flow measurement replicate measurements will be made to test the accuracy of the individual making the measurements Replicate measurements are made by the same individual who made the original measurements and at the same cross section as the original but with different horizontal locations stations across that cross section For example if the original cross section had stations at even intervals 2 4 6 8 etc the replicate measurement might have stations set at odd intervals 3 5 7 9 etc For benthic macroinvertebrate identification ten percent of all sorting pans will be randomly checked by a second
377. pg 5 337 TEMPERATURE to pH CHART This chart is for color coded buffers only Temperature pH pH pH of the Buffer Buffer Buffer Buffer 0 4 00 7 00 10 00 4 06 6 97 9 78 4 09 6 98 9 70 68 SOP TP LFUCG Laboratory Page 69 of 219 Revision Number 1 Last Revised 09 09 Total Phosphorus Analysis Ascorbic Acid Method Phosphorus Reactive Orthophosphate HACH Method 10209 Total Phosphorus HACH Method 10210 TNT 843 LR 0 15 to 4 50 mg L PO or 0 05 to 1 50 mg L POP TNT 844 HR 1 5 to 15 0 mg L PO or 0 5 to 5 0 mg L POP TNT 845 UHR 6 to 60 mg L PO or 2 to 20 mg L PO P Reactive Phosphorus EPA Method 365 1 Total Phosphorus EPA Method 365 3 1 Scope Significance to Process and Application 1 1 Phosphorus in wastewater is almost always present in the form of phosphates There are three major classes of phosphates 1 Orthophosphates fertilizer is major source 2 Polyphosphates detergents and cleaning agents are major sources and 3 Organic Phosphates biological waste is major source Organic Phosphates are also formed from orthophosphates during biological treatment of waste streams Analysis of Total Phosphorus includes all of the aforementioned forms of Phosphorus The reduction of Total Phosphorus levels throughout the wastewater treatment process is highly important as phosphorus concentrations in plant effluents must be low enough See Sec 10 1 Permit Re
378. ple disposal must be retained Additional information on confidentiality is presented in Section 18 Waste Disposal Waste collection storage recycling and disposal procedures and policies are part of method SOPs Where disposal procedures and policies are included as part of a test method the test method disposal practices are strictly followed 32 TB Laboratory QAP September 16 2009 Revision 1 15 1 15 2 15 3 Section 15 Corrective Action Policies and Procedures Scope The following policies and procedures are used when any analysis or reporting discrepancies are detected or when any deviation from the policies and procedures in this manual occur Identification of Discrepancies 15 2 1 Discrepancies or deviations shall be defined as but not limited to any of the following 1 quality control sample results outside control limits 2 reporting sample results in wrong units 3 using unapproved analytical procedures 4 data which appears to be erroneous to current trends 15 2 2 Each analytical procedure SOP references quality control criteria to use in determining discrepancies and accepting data Staff Responsible for Investigation and Corrective Action 15 3 1 Any of the Laboratory staff may detect discrepancies Once a discrepancy is detected it is reported to laboratory supervisor Laboratory management or staff may investigate any discrepancies Data that has discrepancies should not be recorded and should be
379. plotted curve and the sample values Copy the relevant data onto the Orthophosphate Data Sheet D Clean Up 1 Turn off the spectrophotometer lamp 2 Pour waste in acidic waste container 3 For glassware clean up refer to the NORMAL section of the Glassware GLP 6 Calculations The value read from the spectrophotometer is in the form PO4 P This value may need to be converted to the PO form The equation for this conversion is PO4 P 0 32614 PO 7 Quality Control A calibration curve should be established using the standards described in section 3 Any point that is not within this range or that causes a low r value must be redeveloped and rerun until either above criteria are satisfied The quality control sample should be run at the beginning and end of each sample delivery group SDG or at the frequency of one per every ten samples The QC s value should fall between 10 of its theoretical concentration A duplicate should be run for of each SDG or at the frequency of one per every twenty samples whichever is greater The RPD Relative Percent Difference should be less than 10 If this difference is exceeded the sample must be reanalyzed From each pair of duplicate analytes X and X3 calculate their RPD value X X X 1 2 Where X X2 means the absolute difference between X and X gt If a sample s value exceeds 1 000 ppm the sample must be diluted The sample must be diluted
380. portant Note Undissolved chromium is not determined with the determination of chromium VI An analyte concentration greatly above 20 mg L in excess of the stated range will adversely affect color formation resulting in a false reading within the method range 7 4 Measurement results can be verified using sample dilutions or standard additions Procedures 8 1 Steps 8 1 1 Filtration 1 Pour the sample from the sample container to the plastic beaker as soon as the sample arrives 2 Fold a glass microfibre paper to fit in the funnel 3 Slowly pour sample into funnel so it does not overflow 4 Collect filtrate 35 SOP Cr 6 LFUCG Laboratory Page 36 of 219 Revision Number 3 Last Revised 09 09 8 1 2 Method 10219 for Total Chromium 1 2 3 4 5 6 7 8 9 Turn on the DRB200 Reactor Preheat to 100 C For DRB200 Reactors with 16 mm wells make sure the 16 mm to 13 mm adapter sleeve have been placed into each well before turning on the reactor Carefully remove the protective foil lid from the DosiCap Zip Unscrew the cap from the vial Pipet 2 0 mL of sample into the vial Turn the DosiCap Zip over so that the reagent side faces the vial Screw the cap tightly onto the vial Shake the capped vial 2 3 times to dissolve the reagent in the cap Make sure that the reagent has dissolved by looking down through the open end of the DosiCap Heat the vial for one hour at 100 C When the timer expires
381. ptone into filter unit before dispensing sample Turn on vacuum after the sample is introduced For sample volumes 5 to 50 mL use sterile pipettes for dispensing into filter unit Do not touch the inside of the filter holder unit Do not allow the pipette tip to touch the filter 19 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 SOP WH Fecal Coliforms West Hickman WWTP Laboratory Page 20 of 219 Revision Number 4 Last Revised 09 09 For sample volumes 50 to 100 mL pour sample into cylinder and use the scale on the side of the cylinder for measurement Turn on vacuum Once sample has filtered through turn off vacuum Rinse top of the filter unit with peptone two times using autoclaved peptone in a Nalgene squeeze bottle Turn on vacuum to drain peptone Turn off vacuum Flame forceps Remove top of the filter unit and place on the sterile blue field Open Petri dish Use sterile flamed forceps to grab the edge of the filter and remove it from the filter holder unit Place filter grid side up onto edge of the Petri dish and gently slide it onto the surface of the media saturated pad Replace Petri dish cover Place Petri dishes into a 4 5 X 9 inch sterile sampling bag Make sure not contaminate the inside of the bag Seal bag Place bag with Petri dishes face down into water bath at 44 5 C 0 2 C for 24 2 hours Log initials
382. quence click to highlight and go to file click save as This will load the method of interest and a template for the current sequence run 19 The sequence is edited to reflect the method and samples that are to be run a SYSTEM 2 TKN for TKN and Total Nitrogen Note Data is reprocessed in the section of Chromeleon 6 8 called Sequence integration editor Only operators with a minimum of three months experience in Ion Chromatography should attempt to reprocess data for this analysis Once data is optimized then the nitrogen values from nitrate and nitrite analysis can be subtracted from this value for the TKN nitrogen value If only Total Nitrogen is needed then use the optimized data value without the correction for nitrite and nitrate nitrogen 20 Observe the reading on the screen of the CD20 Conductivity Detector A conductivity rate change of lt 0 03 uS over a 30 second time span is considered stable for analysis 21 If using the GP50 pump it will take about 15 30 minutes for the CD20 system to stabilize If using the IP25 it will take between 30 minutes to 2 hours for stabilization 22 Once the CD20 is stabilized the Dionex DX500 lon Chromatography System is ready to start standardization NOTE When using the GP50 Gradient Pump all due care must be taken before one switches from local procedures to remote procedures The bottle from which the eluent is being pumped i e A B C or D must exactly match the bottle specified in the
383. quirements to avoid detrimental effects on the receiving environment such as algae blooms 2 Summary of Method 2 1 2 2 Executive Summary Total phosphorus analysis at Town Branch Laboratory refers to the spectrophotometric analysis of all phosphorus forms in a water wastewater sample that has been digested Discussion Phosphates present in organic and condensed inorganic forms meta pyro or other polyphosphates are first converted to reactive orthophosphate in the Total Phosphorus procedure Treatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms Organic phosphates are also converted to orthophosphates in the Total Phosphorus procedure by heating with acid and persulfate The Reactive Phosphorus procedure measures only the reactive ortho phosphorus present in the sample The reactive or orthophosphate ions react with molybdate and antimony ions in an acidic solution to form an antimonyl phosphomolybdate complex which is reduced by ascorbic acid to phosphomolybdenum blue Test results are measured at 890 nm with a HACH DR5000 spectrophotometer 69 SOP TP LFUCG Laboratory Page 70 of 219 Revision Number 1 Last Revised 09 09 Health amp Safety Precautions 3 1 32 3 3 During sample digestion the digester block is HOT 100 C Burn Hazard Use digester block safety shields In addition the capped glass sample vials contain hot 100 C acidic solutio
384. r Milli Q Water System conforming to the requirements in ASTM Specification D1193 Ammonium Peroxydisulfate Place 20 g of ammonium peroxydisulfate in a 50 mL volumetric flask Dilute with water to volume Add a magnetic stirrer to the flask and let the solution stir until all the crystals have dissolved minimum of 20 minutes Prepare daily enough for 30 beakers total Solution Mixture Dissolve 0 13 g of antimony potassium tartrate and 5 6 g of ammonium molybdate in approximately 700 mL of water Cautiously add 70 mL of concentrated sulfuric acid Allow the solution to cool and dilute to liter The solution must be kept in a polyethylene bottle away from heat This solution is stable for one year Combined Reagent Dissolve 0 50 g solid ascorbic acid in 100 mL of solution mixture Prepare daily Phenolphthalein indicator solution Dissolve 0 5 g of phenolphthalein in a mixture of 50 mL isopropyl alcohol and 50 mL water Sulfuric acid 31 69 Slowly add 310 mL of concentrated H SO to approximately 600 mL of water Allow solution to cool and dilute to 1 liter Sodium Hydroxide 10 N Dissolve 400 g of NaOH in approximately 800 mL of water Allow solution to cool and dilute to 1 liter Sodium Hydroxide 1 N Dissolve 40 g of NaOH in approximately 800 mL of water Allow solution to cool and dilute to 1 liter Phosphorus stock solution 50 mg L Dissolve 0 2197 g of predried 105 C for one hour KH PO in water and
385. r in place of sample and run the procedure as described 2 To subtract the value of the blank from a series of measurements measure the blank per step 12 of the total chromium procedure or step 7 of the hexavalent chromium procedure 3 Press OPTIONS gt MORE gt REAGENT BLANK Press ON The measured value of the blank should be displayed in the highlighted box Press OK to accept this value The reagent blank value will now be subtracted from all results until the function is turned off or a different method is selected 4 Alternately the blank can be recorded and entered at any later time by pressing the highlighted box and using the keypad to enter the value 8 1 5 Sample blanks 1 Colored or turbid samples can cause high results The digestion in the total chromium procedure usually destroys all color and turbidity and a sample blank is not required To compensate for color or turbidity in the determination of hexavalent chromium the procedure is repeated and the color forming reagent that is present in the DosiCap B is not added 2 To determine the sample blank for hexavalent chromium a Run the procedure as written but do not add the DosiCap B Reagent in step 2 b Cap the vial with the original DosiCap Zip do not remove the foil c The value obtained in step 7 is subtracted from the value obtained on the original hexavalent chromium sample to give the corrected sample concentration d Alternatively hexavalent chromium s
386. rated However to ensure accuracy calibrate on a regular basis Select a calibration standard appropriate for your Testr TDSTestr Low from 200 to 1990 ppm TDSTestr High from 2 00 to 10 00 ppt ECTestr Low from 200 to 1990 uS ECTestr High from 1 00 to 19 90 mS It is best to select a standard close to the test solu tion value 1 Open battery compartment lid end with lanyard loop The two white buttons are Increment INC and Decrement DEC calibration keys 2 Rinse electrode in deionized water then rinse it in calibration standard then dip it into a container of calibration standard 3 Switch unit on ON OFF key Wait several minutes for display to stabilize 4 Press the INC or DEC keys to adjust reading to match the calibration standard value 5 After 3 seconds without a key press the display flashes 3 times then shows ENT The tester accepts calibration value returns to measurement mode 6 Replace battery cap TDS or Conductivity Testing 1 Remove electrode cap Switch unit on ON OFF key 2 Dip electrode into test solution Make sure sensor is fully covered 3 Wait for reading to stabilize Automatic Temperature Compensation corrects for temperature changes Note reading 4 Press ON OFF to turn off Tester Replace electrode cap Note Tester automatically shuts off after 8 5 minutes of nonuse HOLD function Press HOLD key to freeze display Press HOLD again to rel
387. rates are present Habitat assessments will be performed at each of the macroinvertebrates sites The habitat assessment method is covered in Section B2 2 4 Revision No 0 Date April 11 2011 Wolf Run Watershed Based Plan Page 41 of 67 B2 2 3 1 Semi Quantitative In both headwater and wadeable streams semi quantitative sampling will consist of taking four 4 0 25m quadrat kick net samples from mid riffle or the thalweg This will be accomplished using a 0 25 m 600um mesh kick net dislodging benthos by vigorously disturbing the 0 25 m 20 x 20 in of substrate in front of the net Large rocks will be hand washed into the net The contents of the net will then be washed and all four samples will be composited to yield a 1m semi quantitative sample The composited sample will be partially field processed using a U S No 30 sieve 600um and wash bucket Large stones leaves and sticks will be individually rinsed and inspected for organisms and then discarded Small stones and sediment will be removed by elutriation using the wash bucket and U S No 30 sieve This sample must be kept separate from all other sub habitat collections For headwater sites two kick net samples will be allocated to each of two distinct riffles at minimum that are separated by at least one pool or run This will be done to help reduce between riffle variability However if there are several riffles located within the reach the sampling effor
388. ration Frequency Before each field sampling event Calibration Instrument Used Calibration standards user manual Person Responsible Sampler EC Conductivity PockeTesters Conductivity Measurement Before each collection event Overall condition battery power Before and after each uses Calibration standards user manual Sampler Hand pumps filter funnel tubing and flasks Field Filtration Before each collection event 3 solution wash overall condition N A N A Sampler Flow Meter Discharge Monitoring Before each collection event Overall condition battery power Annual Manufacturer Sampler TROLL Dataloggers Karst Characterization Stage Measurement Before use Cleanliness program settings N A N A Sampler Macroinvertebrate Sampling Nets Macroinvertebrate Sampling Before each use Overall condition N A N A Sampler Sample Bottles Sample Collection Before collection Good condition N A N A Sampler Volunteer samplers will calibrate the conductivity meters before and after each sampling event chain of custody or Conductivity Survey Field Datasheet Appendix A Two standards will be used to calibrate the meters with results recorded on the Third Rock calibrates flow meters annually through the manufacturer The multimeters to be used will be calibra
389. ratory Page 4 of 219 Revision Number 2 Last Revised 9 09 4 Record alkalinity value date time and initials in bench sheet 5 For samples Determine sample volume from the bench sheet generally 100 mL To make a 50 1 dilution pipette 2 mL of sample and dilute to 100 mL volume with Nanopure water Pour sample into 150 mL beaker Add 10 mL of Total Alkalinity Reagent and insert pH probe Turn on stirrer Read pH value when the meter displays STABLE Obtain alkalinity value Asmp from the Full chart 0 225 ppm by cross referencing with pH value If diluted determine alkalinity of diluted sample Ags Ads Asmp E AH20 MAPAS oes 5 6 Record alkalinity value date time and initials in bench sheet 8 2 Helpful Hints 1 Alkalinity ranges for the standard should be 100 5 ppm if not try recalibrating and use clean glassware QA QC Requirements Analysis values for the standard must have a pH range of 4 41 0 05 equivalent to 930 1070 mg L CaCO3 If this criterion is not met corrective action is indicated See Quality Assurance Program QAP Sec 15 Corrective Action Policies and Procedures Expected Results 10 1 KPDES Permit Requirements None required 10 2 Process Ranges Mean SD 1 Town Branch WWTP Mixed Liquor Influent 218 11 0 Mixed Liquor Effluent 152 16 8 Digesters 3270 2 245 8 11 12 SOP Alkalinity LFUCG Laboratory Page 5 of 219 Revision Number 2 Last Revised 9
390. reatment of the sample prior to injection dictates the definition of the carbon as it is measured The final usefulness of the carbon measurement is in assessing the potential oxygen demanding load of organic material on a receiving stream This statement applies whether the carbon measurement is made on a sewage plant effluent industrial waste or on water taken directly from the stream In this light carbonate and bicarbonate carbon are not a part of the oxygen 49 TB Laboratory QAP September 16 2009 Revision 1 demand in the stream and therefore should be discounted in the final calculation or removed prior to analysis The manner of preliminary treatment therefore defines the types of carbon which are measured Toxicant A substance that kills or injures an organism through chemical or physical or biological action Examples include cyanides pesticides and heavy metals such as zinc and chromium Toxicology Is the basic science of poisons and their effects It is the study of the physical effects of chemicals on biological systems Trace Element Any element in water or wastewater that for reasons associated with natural distribution industrial use solubility or other factors is present at very low concentrations as an essential element Trends When charting quality control values for the same control the values of the control tended to increase or decrease over a period of 6 consecutive days can indicate deterioration
391. remove the hot vial from the reactor Cool the vials to 15 35 C Do not invert the vial after digestion Screw an orange DosiCap B onto the cooled vial Invert the vial 2 3 times to mix 10 After inverting the tube allow the vial to sit undisturbed for 2 3 minutes 11 After the timer expires invert the vial again 2 3 times 12 Thoroughly clean the outside of the vial with a Kim wipe Insert the prepared vial into the DR5000 cell holder The instrument reads the barcode then selects and performs the correct test Results are in mg L Cr 13 No instrument Zero is required Method 10218 for Hexavalent Chromium 1 2 3 4 5 6 7 8 Remove cap and pipet 2 0 mL of sample into the vial Screw an orange DosiCap B on the vial Invert the vial 2 3 times to mix After inverting the tube allow the vial to sit undisturbed for 2 3 minutes After the timer expires invert the vial again 2 3 times Thoroughly clean the outside of the vial with a Kim wipe Insert the prepared vial into the DR5000 cell holder The instrument reads the barcode then selects and performs the correct test Results are in mg L Cr No instrument Zero is required 36 SOP Cr 6 LFUCG Laboratory Page 37 of 219 Revision Number 3 Last Revised 09 09 8 1 4 Reagent blanks 1 A reagent blank can be measured and the value subtracted from the results of each test performed using the same reagent lot number Use deionized wate
392. reparation of BOD seed 1 Siphon 500 mL dilution water into 500 mL graduated cylinder 2 Pour the 500 mL of dilution water into 1 L Erlenmeyer flask 3 Pull apart Polyseed capsule and pour contents into flask 4 Submerge the aerator discharge diffuser in the flask using a support stand to hold the diffuser centered at the bottom of the flask turn the aerator on 5 Aerate contents of flask for at least one hour 6 Decant the supernatant carefully into a clean 500 mL beaker so as not to allow any bran in the remaining seed solution 7 Stir using a spin bar and magnetic stir table 8 The Polyseed solution should be used within 6 hours of rehydration of the capsule s contents 17 SOP CBOD LFUCG Laboratory Page 18 of 219 Revision Number 5 Last Revised 09 09 Siphon dilution water into a labeled squirt bottle for dispensing Preparation of HACH HQ40d Meter with LBOD101 probe 1 2 3 Calibrate DO meter at the beginning of the analysis day see SOP DO Section 8 Meter must be calibrated a minimum of once per analysis day Recalibrate meter if reading are taken in the afternoon Rinse LBOD probe between samples with Nanopure water Blank Control Samples 1 2 3 4 5 Prepare four BOD bottles as follows label one bottle Unseeded Blank NO seed will be added label one bottle Blank 1 and add 2 mL of seed solution label one bottle Blank 2 and add 3 mL of seed solution
393. reservation 4 1 Do immediately after Total Solids Method See SOP Total Solids Reagents 5 1 Drierite 8 mesh 94 SOP Volatile Solids LFUCG Laboratory Page 95 of 219 Revision Number 3 Last Revised 09 09 6 Equipment amp Lab Ware 6 1 Denver Instrument Analytical Balance 6 2 ASTM Class 1 weight set 6 3 Vycor dishes or flat bottom crucibles 64 Tongs 6 5 Thermolyne 30400 Muffle Furnace 550 C 6 6 Desiccator 6 7 Hot Plate 103 C to 105 C 7 Interferences 7 1 Negative errors in the volatile solids may be produced by loss of volatile matter during drying 7 2 Determination of low concentrations of volatile solids in the presence of high fixed solids concentrations may be subject to considerable error 8 Procedures 8 1 Steps 1 After Total Solids Method is completed See SOP Total Solids place dishes in Muffle Furnace Use tongs and gloves 2 Ignite tares at 550 50 C to constant weight approximately 1 hr 3 Transfer tares to hot plate for 15 minutes 4 Transfer tares to desiccator for at least 20 minutes Note Make sure the dishes are cool enough not to melt the desiccator 5 Weigh tare and ash and record weight as Wa 8 2 Helpful Hints 1 Transfer tares to hot plate so it doesn t melt desiccator 2 Radiant heat from furnace can burn wear gloves and use tongs 9 QA QC Requirements 9 1 None required 95 10 11 12 SOP Volatile Solids LFUCG Laboratory Page 96
394. rk Appartments parking lot Upstream of Devonport Drive west of Alexandria Dr Park in Pleasant Cove Apartments lot to left of bridge take sample at rock upstream of bridge 38 048594 Park on Cross Keys Road just off of Parkers Mill Road Sample reach as 38 043212 diverges from curbside Take Roanoke Dr off of Alexandria Dr past 7 Pines Dr Park uphill of cement slab in greenway sample at path crossing creek 38 045274 Tum right onto Tazwell Drive off Mason Headly Road Travel to the end of the road Walk below the playground to sample Park at lot to right of Parkway Drive in front of Picadome Golf Course Site is north of the clubhouse midway between the bridges between holes 4 and 5 38 044927 38 037453 At terminus of Faircrest Dr south of Lynn Dr Sample upstream of confluence with Springs Branch From W9 cross Wolf Run at foot bridge and sample upstream on Spring Branch Park at end of parking lot behind the Harrodsburg Rd Fire Station Access just north of power trans former at edge of 38 029954 38 029855 38 031245 adjacent parking lot Park at lot behind the Picadome Golf Course clubhouse Measure discharge at 38 037494 38 022932 84 528581 confluence of surface runoff with Vaughn s Branch if flow is present Sample about 50 feet below bridge at Rosemont Garden NOTE X indicates permanent sampling location O indicates measurements will occur if flow is present
395. ronic copies of the original datasheets to the QA Manager He will be responsible for storing all original copies of the volunteer field data collected Chemical laboratory analytical results and internal laboratory logbook documentation will be the responsibility of David Price Laboratory Director Macroinvertebrate laboratory results and metric calculations will be the responsibility of Bert Remley Macroinvertebrate Laboratory Chief Taxonomist Upon completion of laboratory analysis results shall be forwarded electronically to Steve Evans QA Manager Data collected by Third Rock samplers and staff will be maintained by Steve Evans QA Manager He will receive the laboratory reports and review the data for conformance to the requirements of this QAPP and will subsequently send the results to the KDOW and LFUCG He will be responsible for sending all hardcopy and electronic copies of data reports to the LFUCG and KDOW as well as maintaining previously submitted data All final reports will receive a technical peer review and a grammatical formatting review prior to submission All raw data documentation and records shall be retained Correspondence and other documentation relating to interpretation and evaluation of data collected analyzed or processed shall also be retained The retention period is a minimum of three years subsequent to grant completion All data maintained on Third Rock computers will be supported by a daily backup and ar
396. rt it into the DR5000 cell holder The instrument reads the barcode then selects and performs the correct test Results are in mg L PO4 No instrument Zero is required 8 Note and record the indicated values on the bench sheet Reagent Blanks A reagent blank can be measured and the value subtracted from the results of each test performed using the same reagent lot number Use Nanopure water in place of sample and perform the Total Phosphorus Method 10210 or the Reactive Phosphorus Method 10209 test To subtract the value of the blank from a series of measurements 1 Measure the blank as in step 12 of the Total Phosphorus Method 10210 test or step 7 of the Reactive Phosphorus Method 10209 test 2 Activate the Reagent Blank feature The measured value of the blank is shown in the highlighted box 3 Accept the value shown The reagent blank value will be subtracted from all results until the function is turned off or a different method is selected Alternately the blank can be recorded and entered at any later time by pressing the highlighted box and using the keypad to enter the value Sample Blanks Color or turbidity in samples can cause high results The digestion in the total phosphate procedure usually destroys all color and turbidity and a sample blank is not required To compensate for color or turbidity in the reactive phosphate procedure the color forming reagent that is present in the DosiCap C is not added To determ
397. ry Page 65 of 219 Revision Number 3 Last Revised 09 09 Type the value for the pH 7 0 buffer at the given temperature then press enter key Turn off stirrer and rinse probes with Nanopure water Place probes into a beaker of Buffer Solution pH 4 00 red color coded Turn on stirrer Write down the temperature of the buffer and check what the pH for the buffer will be at this temperature from chart Temperature C Buffer Solution pH 4 00 red color coded 10 4 00 15 3 99 20 4 00 25 4 00 30 4 00 Touch the std button on the upper right corner of the screen Type the value for the pH 4 0 buffer at the given temperature then press the enter key Turn off stirrer and rinse probes with Nanopure water Place probes into a beaker of Buffer Solution pH 10 00 blue color coded Turn on stirrer Write down the temperature of the buffer and determine what the pH for the buffer will be at this temperature from chart Temperature C Buffer Solution pH 10 00 blue color coded 10 10 19 15 10 12 20 10 06 25 10 00 30 9 94 Touch the std button on the upper right corner of the screen Type the value for the pH 10 buffer at the given temperature then press the enter key 65 8 2 8 3 8 4 SOP pH LFUCG Laboratory Page 66 of 219 Revision Number 3 Last Revised 09 09 20 Turn off stirrer and rinse probes with Nanopure water 21 Touch the meas button on the
398. ry QAP September 16 2009 Revision 1 5 Blue Sky grab and composite samples are on one COC record delivered to Town Branch Lab every Thursday by the Blue Sky on duty Operator 6 Illicit Discharge Detection and Elimination IDDE grab samples with COC record delivered to Town Branch lab by the Environmental Inspector 7 Industrial waste 24 hour composite samples COC record delivered to the Town Branch Lab by the Environmental Inspector 12 2 6 COC Checklist 12 2 7 12 2 8 1 Operator obtains COC record 2 Operator collects samples 3 On COC record operator records e date sampling started e time sampling started e date sampling stopped time sampling stopped sampling method sample type sample size type of preservative analysis requested sampler s signature 4 Operator delivers samples to Town Branch Lab 5 Operator signs the COC sheet on the line Relinquished By Representing Operators Signature 6 Operator writes the date and time of relinquishment on the same line as noted above in 5 7 Operator leaves the COC sheet with a Laboratory Analyst who then signs the sheet on the line Received in the Laboratory By Signature e On the same line the Laboratory Analyst writes the date and time the samples were received in the lab Samples must be received in the sample container required by the test method and properly labeled Each sample container must have a unique identification
399. s ocooonccnconnccocccoconanonnos 20 DV UMM A A E EET E E EEEE E A 22 Procedures for Reviewing New Word e Aaa 22 DVS SCO EE E E RA 22 112 Unknown Sample NN ANA 22 11 3 Contract Anal ie 22 SECUN AA A AA 23 Sample Acceptance and Receipt Po santas Gears vice Pes shepeenedac tenia vi co erastealecessee ts 23 MD A CONS eth EE E AE E EEE A E E A EA E EEA 23 12 2 Sample Acceptance Requirements jis vixsducttase zastaestteotanesttaase duct baxteuatandeRarsdsdacsdatdenes 23 123 Werrtieation of Preservation cscs 0 actos e gi easiass 25 12 4 Actions for Deviations from the Lab s Sample Acceptance Requirements 25 12 5 Laboratory Log of Received ampli SA verdant das 26 Section Di A ave cade sing A Aaa AAA AAA AAA NA ea 27 Sample Tracking and Storage Procedures cssccsscssscsesnccssscssccesccesscsenscsscssscessacensasssanenses 27 l3 Ah SCOPE on A a A ira CO E a Rana as ate eee ees 27 132 Sample Tracking Record sia a a 27 13 3 Proper Storage and Avoidance of Cross contamination of Samples eeee 24 13 4 SEC OE Sampl S e to ona fuk has 27 13 5 Sample A E ona 21 Section TAn gekart sa O 28 Record Keeping Data Review and Reporting Procedures ooooonoccnococoncconccnonnconncconocnnnconnnonnnonns 28 A 28 14 2 Records Maintained by the Laboratorio a 28 14 3 Records of Standards and Analytical Reagents oooonccnincononococcnoocnconnoconocannnonncconncnns 29 14 4 Computerized Data Storage iii bis 30 14
400. s an internal reference The measurement range for the method is 0 02 mg L to 20 0 mg L The Method Detection Limit MDL 40 CFR 136 Appendix B has been determined as 0 05 mg L and the Minimum Level ML Reference 15 4 has been set at 0 20 mg L SOP WH FIELD D O West Hickman WWTP Laboratory Page 3 of 219 Revision Number 3 Last Revised 09 09 Health amp Safety Precautions 3 1 Glassware involved possible cut hazard 3 2 All municipal and industrial wastewaters are potentially hazardous Gloves and goggles should be worn when dispensing these samples Sample Handling and Preservation 4 1 Field measurements are obtained directly therefore sample handling may not apply 4 2 If samples are collected for analysis at another location i e Laboratory the following apply 4 2 1 Sample must be collected in a glass bottle preferably a BOD bottle with stopper filled to top with no airspace 4 2 2 Sample must be analyzed immediately 15 minutes maximum on permit samples 4 3 There is no applicable preservative with this method Reagents 5 1 Nanopure Lab Water Equipment amp Lab Ware 6 1 HACH HQ40d portable multi meter 6 2 HACH Model LDO101 Rugged Dissolved Oxygen Probe 6 3 BOD bottles with 300 ml capacity and tapered ground glass stoppers 6 4 Sensor Cap replacements HACH part 5838000 6 5 Calibration bottle for Water saturated Air calibration method Interferences 7 1 Salinity salinity correction available
401. s as specified in Section 6 8 40 TB Laboratory QAP September 16 2009 Revision 1 21 5 21 6 21 7 21 7 21 4 5 The laboratory shall have on file documentation indicating the analyst s acceptable performance on a blind sample at least once per year and a certification that the analyst has read understood and agreed to perform the most recent version of the standard operating procedure Additional Training for Technicians Additional training provided by the Laboratory Management involves participation in the Kentucky Laboratory Analyst KLA training testing and certification for laboratory technicians The KLA was created under the KY Water and Wastewater Operators Association KWWOA for individuals employed in the water quality field A total of 4 class certifications are available for Wastewater Laboratory Analysts Substituting Experience or Education to Meet Training Requirements A person may serve as Laboratory Supervisor Quality Assurance Officer or Technician when that person does not meet the training educational or experience requirements for the position In such cases the laboratory shall submit written justification explaining why a person should serve in a particular position This written justification shall take into account the following factors e Experience as an offset for education requirements e Education as an offset for experience requirements Instrument Training Requirements Analysts and
402. s during this period the survey will resume when water levels are consistent with the initial survey conditions The sampling will be performed during a period between May and September 2011 All hardcopy and electronic data will be submitted to Third Rock for data entry and analysis with a final report expected by December 31 2011 Third Rock will sample macroinvertebrates in May 2011 during the appropriate sampling index period For wadeable streams with a watershed gt 5 mi the index period is May 1 to September 30 for headwater streams with a watershed lt 5 mi it is February 15 to May 31 All sites are headwater sites except W1 which is sampled for macroinvertebrates under the MS4 permit and not under this project Sampling will not occur during periods of excessively high or low flow or within two weeks of a known scouring flow event Habitat assessments will be performed by trained volunteers concurrent with or within one week of the macroinvertebrate collections at each of these sites Laboratory identification metric calculation data analysis and report completion will occur prior to December 31 2011 The watershed habitat assessments performed within the 24 stream segments in the Wolf Run watershed will be performed subsequent to volunteer training and prior to October 31 All data will be compiled into an electronic database by the volunteer sampling coordinator and submitted to Third Rock by October 31 2011 Hydrogeomorph
403. s impaired for swimming use non support in the 1998 303 d list of Kentucky impaired waters This impaired status has remained since that time with additional impairments partial support of warmwater aquatic habitat use and non support of secondary contact use being identified in subsequent years KDOW 2010a The impairment of Wolf Run in addition to other Lexington streams led the US Environmental Protection Agency USEPA and the Kentucky Environmental and Public Protection Cabinet KY EPPC to file a lawsuit against Lexington in 2006 for violations of the Clean Water Act in 2006 The lawsuit was due to failure of the city to maintain the sanitary and storm sewer systems which caused raw sewage discharges into streams On March 14 2008 LFUCG entered into a Consent Decree in order to resolve this lawsuit United States 2006 Within the Consent Decree LFUCG agreed to make extensive improvements to its sewer systems and address sanitary sewer overflows and associated MS4 permit violations as well as to reduce the discharge of pollutants via stormwater With the Consent Decree in place LFUCG is furthering its efforts to improve water quality in Wolf Run Wolf Run Watershed Page 11 of 67 Revision No 0 Based Plan Date April 11 2011 The citizens of Lexington especially those in the Wolf Run watershed share the interest in water quality improvement with LFUCG The Friends of Wolf Run FOWR a community based watershed group became acti
404. s in are for LaMotte products These products are not included in this kit but can be ordered from LaMotte Company by using the specified code number oo Useal0ml graduated cylinder 0416 to add 15 mL of Deionized Water 5115 to the titration tube 0608 Add 2 drops of Sulfuric Acid 5N 8517WT 5 YY Swirl to dissolve Solution will turn yellowish brown Use a Direct Reading Titrator 0 1 Range 1 0 mL capacity 0376 to add 2 mL of Potassium Bi iodate 7346 Use the 0 1 e spoon 0699 to add 0 2 g Potassium Iodide Crystals 6809 Fill another Direct Reading Titrator 0376 with Sodium Thiosulfate Solution 0 025N 4169 EPA COMPLIANCE While gently swirling the Add3d i tube add Sodium Starch rops O Thiosulfate 0 025N until Indicator the color fades to pale Solution yellow It will be 4170WT necessary to refill the The solution Direct Reading Titrator y will turn blue Continue adding Sodium Thiosulfate 0 025N until the blue color disappears and the solution is C E Result colorless Read the test result directly from the scale 2 0 ppm where the large ring on the Titrator meets the Titrator barre i Include the value of the original amount dispensed 1 mL If the reading is 2 0 0 1 mL the Sodium Thiosulfate 0 025N 4169 is satisfactory If not discard and replace with new reagent 3 j ETE 0 O 10 DIS
405. s is provided below B1 1 Sampling Site and Reach Locations Exhibits 1 and 2 indicate the locations of the permanent sampling sites on aerial and geologic quadrangle mapping Table 8 describes the location of each sampling site and whether monitoring for the karst hydrograph characterization macroinvertebrate collections hydrogeomorphic sampling or water quality monitoring will be performed at these sites Wolf Run Watershed Page 30 of 67 Revision No 0 Based Plan Date April 11 2011 TABLE 8 SAMPLING LOCATIONS it z REESE Stream Location Directions Latitude Longitude Name Old Frankfort Pike McConnell Prestons Cave Cardinal Run wio Sees wio Ses Drive Elm Harrodsburg ae Road W1IA Eini E Lafayette W12 WolfR Faircrest Picadome Golf Course Downstream of Old Frankfort Pike northbound prior to roundabout Alexandria Dr Park to the right of the Assembly of God Church on Dunkirk Drive Access site through grass lot next to the church to spring on the left About 50 feet downstream of Cambridge Drive Bridge Park in Cambridge Park Appartments parking lot at 38 067303 84 554182 84 542169 84 550782 84 549624 84 553867 84 557131 84 550661 84 536148 84 525057 84 537196 84 526027 84 527095 38 057333 38 053742 About 30 feet upstream of confluence with WoltRin Sample upstream of the l 38 054904 sanitary sewer manhole cover Park in Cambridge Pa
406. s well as the date and time of the collection on each sample bottle The unique sampling event code will follow the following format SAMPLE ID W Y YMMDD Where W is Unique Site Identifier 0 12 or DD for Duplicate YYMMDD is the date in year YY month MM day DD format As indicated above duplicate samples will be indicated as such in the site identifier of WDD The time of collection will not be indicated on the chain of custody so that the laboratory is blind as to the sampling location it corresponds with This information shall be recorded in the field notebook during collection so that results can be compared after analysis B4 Analytical Methods Requirements USEPA methodology must be used for all analysis as applicable Detection limits for all parameters must be at a sensitivity level to compare to Kentucky water quality standards The requirements for all methods and detection limits are specified in Table 6 SOPs for the chemical laboratory methods are specified in Price 2009 Third Rock s macroinvertebrate identification laboratory will follow laboratory protocols for benthic macroinvertebrate sample processing identification and data reporting per KDOW 2009b 2008 with the following exceptions e All samples will be logged into Third Rock s Macroinvertebrate Laboratory Information Management System MacLIMS upon receipt e Sample identification date will be maintained in MacLIMS e Taxonomic QA Q
407. se to the complaint Complaint Investigation Procedures 17 3 1 Review the following items regarding the sample or analysis in question with laboratory staff Receipt of sample Internal Chain of Custody Analyses performed Analysis methods Analytical results Calibration check Quality control results Calculations Unit conversions 17 3 2 Document whether any discrepancies were revealed during the review especially discrepancies which address specific complaint Complaint Response Procedures 17 4 1 Laboratory management will contact the person with complaint and reveal findings of investigation If necessary a corrected report will be issued 17 4 2 File the documented complaint investigation for use during the annual review of the Quality Assurance Plan If any corrective actions are required reference Section 15 of this QAP manual Corrective Action Policies and Procedures 36 TB Laboratory QAP September 16 2009 Revision 1 Section 18 Procedures for Protecting Confidentiality and Proprietary Rights 18 1 Procedure for Protecting Confidentiality The Town Branch Laboratory must protect confidentiality and proprietary rights Laboratory employees are instructed not to divulge any information that may involve issues of confidentiality or proprietary without the approval of the Laboratory Supervisor 18 2 Examples of Confidential Data Some examples of confidential data include Effluent and or Permit data
408. sh eluent b Make certain the waste reservoir is empty of all waste c Turn on the helium The system pressure should be between 7 15psi The system pressure can be regulated with the knob on the back of the Eluent Organizer d Connecting a piece of tubing to the gas line going into the eluent bottle and putting the tubing into the eluent degasses the eluent reservoir s The gas knob on the Eluent Organizer that corresponds to the eluent bottle should be slowly opened until a constant bubbling stream can be seen in the eluent bottle e The eluent should be degassed with helium for a minimum of 30 minutes before operation of the instrument f After the eluent has been degassed remove the tube from the eluent and tightly seal the eluent bottle The eluent is now ready to introduce into the system Whether using the IP25 for Fluorides or the GP50 for everything else turn off the browser scroll to REMOTE on the screen select LOCAL and ENTER Scroll to mL min change to 0 mL min and hit ENTER If using the IP25 pump skip to step 5 Hit MENU and select 1 then ENTER Insert syringe into the Priming Block open the gas valve on the Eluent Organizer turn the valve on the Priming Block counterclockwise and turn on the pump that corresponds with the method to be ran by pushing the OFF ON button If the syringe does not fill freely assist by gently pulling back on the plunger of the syringe Make certain that all of the air bubbl
409. sion No 0 Based Plan Date April 11 2011 for E coli will occur four times within 30 days and is expected to begin in May but may occur at any time within the Primary Contact Recreation period May 1 to October 31 Third Rock will accompany volunteers during each event to conduct discharge monitoring A minimum notice of 48 hours will be provided to FOWR prior to scheduling the volunteer sampling The LFUCG Town Branch and Kentucky Geological Survey laboratories will analyze collected samples Collection events shall be scheduled to avoid collection on Thursday as this day is particularly busy for the Town Branch Laboratory Expected turn around time for the laboratory analysis is 30 days Chemical laboratory reports with data quality review by the Project QA Manager will be submitted to the project team within 60 days of sample delivery to the laboratory With each sampling event quality control samples including field duplicate samples will be collected along with the regular field samples The results of these studies will be used to complete the Wolf Run Watershed Based Plan according to the KDOW s Watershed Planning Guidebook for Kentucky Communities 2010 and the USEPA s Handbook for Developing Watershed Plans to Restore and Protect Our Waters 2008 The project schedule in Table 4 corresponds to the watershed plan chapters outlined in the KDOW guidance The final plan incorporating comments and recommendations is scheduled for
410. sion of Water LaMotte Dissolved Oxygen Water Quality Test Kit Instruction Manual Code 7414 5860 LaMotte Company Chestertown Maryland www lamotte com Lexington Fayette Urban County Government LFUCG 2008 Stormwater Quality Management Program SWQMP for Lexington Fayette Urban County Government Tetra Tech Inc LFUCG Department of Public Works and Department of Environmental Quality Oakton Instruments Waterproof TDSTestr and ECTestr Series Instructions http www 4oakton com Manuals ConductivityTDS TDS_ECTestrmnl pdf Price David J 2009 Quality Assurance Plan QAP and Standard Operating Procedures SOPs Lexington Fayette Urban County Government Division of Water Quality Town Branch Laboratory Recker S A and Meiman J 1990 Remedial investigations status report Shop N Go Food Mart Delta Environmental Consultants Lexington KY unpublished report 18 p Rosgen D L 2008 River Stability Field Guide Wildland Hydrology Pagosa Springs CO Wolf Run Watershed Page 64 of 67 Revision No 0 Based Plan Date April 11 2011 Spangler L E 1992 Unpublished groundwater tracing data University of Kentucky Department of Geology United States and Commonwealth of Kentucky v Lexington Fayette Urban county Government March 14 2006 Consent Decree Lodged in the United States District Court Eastern District of Kentucky Central Division at Lexington Related to Civil Action No 5 06 cv 00386 Accessed November
411. sis of the data 10 Identification of the reporting units such as mg L or mg kg 31 TB Laboratory QAP September 16 2009 Revision 1 14 10 14 11 14 12 11 Identification of any results not generated by the laboratory preparing the data report and identification of the laboratory from which such results were obtained 12 A statement that the report shall not be reproduced except in full without the written approval of the laboratory 13 A statement that samples results relate only to the analytes of interest tested or to the sample as received by the laboratory 14 Additional information may be required for sample data reports submitted to a regulatory authority The laboratory certifies that the sample results meet all the requirements of any environmental laboratory program for which it maintains accreditation Electronic Data Transfer Electronic data transfer i e fax email attachments CD flash drives are documented by hard copies Sample Disposal Records Ordinarily the laboratory does not need to maintain records for disposal of samples For a record of possible litigation samples and other samples that the laboratory supervisor wishes to retain such records will be catalogued by date of disposal and person responsible Samples may be disposed of by sample depletion sample returned to submitter sample washed down sink and sample manifested to a hazardous waste facility Any correspondence concerning sam
412. sment program of Watershed Watch is to generate data that volunteer monitors may use to assess conditions of the stream that most interests them Watershed Watch trains volunteer monitors to collect the following data streamside e Water Quality characteristics measured at the stream including dissolved oxygen pH and temperature and in places specific conductance e Physical characterization of representative stream reaches e Biological sampling and e Habitat assessment including biodiversity This document does not discuss procedures and methods for collection of this data Volunteer monitors also collect grab samples about stream parameters that cannot be measured streamside and require laboratory analysis Samples are collected for e Pesticides that threaten aquatic life sampled in the Spring e Human pathogens including bacteria sampled in the Summer and e Major cations and anions trace constituents total organic carbon and other water quality parameters sampled in the Fall Methods and procedures for training volunteers to grab and transport samples and for laboratory analysis and QA AC are the subject of this document c Data Rigor The KDOW has issued Agency Guidance for Volunteer Monitoring Data and Reports that indicates the level of procedural rigor necessary for data depending on the intended use for the data The guidance is summarized in the following matrix which indicates the data related activities th
413. solved by looking down through the open end of the DosiCap Zip Insert the vial in the DRB200 Reactor Close the protective cover Heat for 1 hour at 100 C After the timer expires carefully remove the hot vial from the reactor Insert it in a test tube rack and allow to cool to room temperature 15 25 C Pipet 0 5 mL 500 uL of Reagent B into the cooled vial Immediately close the Reagent B container Screw a grey DosiCap C onto the vial Invert the capped vial 2 3 times to dissolve the reagent in the DosiCap Wait 10 minutes When the timer expires invert the vial again 2 3 times Clean the outside of the vial with a Kim Wipe and insert it into the DR5000 cell holder The instrument reads the barcode then selects and performs the correct test Results are in mg L PO4 No instrument Zero is required Note and record the indicated values on the bench sheet TNTplus 845 Reactive Phosphorous UHR 6 60 mg L PO 1 2 3 4 5 6 Carefully pipet 0 4 mL of sample into the vial Pipet 0 5 mL 500 uL of Reagent B into the vial Immediately close the Reagent B container Screw a grey DosiCap C onto the vial Invert the capped vial 2 3 times to dissolve the reagent in the DosiCap Wait 10 minutes When the timer expires invert the vial again 2 3 times 73 8 7 8 8 SOP TP LFUCG Laboratory Page 74 of 219 Revision Number 1 Last Revised 09 09 7 Clean the outside of the vial with a Kim Wipe and inse
414. sorter to assure that samples have been picked thoroughly Five percent of all identified samples will randomly be re identified to insure QA QC by a second taxonomist Ninety percent or greater composition comparability e g abundance and richness is the target success criteria If there is less than 90 percent comparability between the taxonomists then taxonomy must be reconciled by both taxonomists and a third taxonomist if deemed necessary Wolf Run Watershed Page 24 of 67 Revision No 0 Based Plan Date April 11 2011 TABLE 6 ACCEPTANCE CRITERIA FOR WATER CHEMISTRY AND IN SITU MEASUREMENTS Parameter Dissolved Oxygen mg L Method LaMotte Accuracy R or 1 5 Precision RPD Sensitivity Reporting Limit 0 5 Specific Conductance uS cm Oakton 95 105 10 pH SU Watershed Watch 0 5 NA Water Temperature C Watershed Watch 0 5 5 to 45 Turbidity Visual Visual Observation NA NA Flow cfs DOWSOP03019 EO 05 ft sec 0 01 ft sec Total Dissolved Solids mg L EPA 160 1 95 105 10 Total Suspended Solids mg L SM 2540 D 95 105 Total Alkalinity mg L CaCO SM 2320 B 80 120 Hardness mg L CaCO SM 2340 C 80 120 Escherichia coli Fecal Coliform MPN 100mLs CFU 100mLs SM 9221 E SM 9221 F N A Ortho phosphorous as P mg L PO P EPA 365 1 Phosphorus
415. ssessment procedures in Barbour et al 1999 volunteers will survey as many segments as time permits within the 24 stream segments into which the watershed has been subdivided At least one assessment will occur in each segment Information obtained from the habitat assessment will be used to supplement biological and physicochemical data when determining the overall health of the stream reach and stream use designation Additionally habitat assessments will serve as a baseline to document physical changes that occur over time and to identify potential areas for BMP implementation A6 1 5 Hydrogeomorphic Assessment Nine hydrogeomorphic monitoring sites have been preliminarily designated to measure channel changes in representative reaches Assessment will include a series of spatially integrated high resolution cross section and longitudinal profile surveys and streambed substrate evaluation to determine the extent of the effects of hydromodification in the Wolf Run watershed Effects of hydromodification that may be revealed by the assessment include degree of bed and bank erosion sedimentation and habitat loss The relative potential for improvement will also be qualitatively assessed based on the lack of obvious physical constraints in a reach position in the landscape or position in the watershed The baseline cross section profile and bed substrate will be compared to a subsequent survey to determine the degree and type of changes in ph
416. sterilize forceps Maintain the area around the flame clear 3 4 Contaminated used Petri dishes and lab equipment must be placed in Biohazardous waste container This Biohazardous waste container is autoclaved before disposal 54 SOP Total Coliforms and E coli LFUCG Laboratory Page 55 of 219 Revision Number 1 Last Revised 09 09 Sample Handling and Preservation 4 1 Samples should be collected in clean sterile glass or plastic containers 4 2 If chlorine is in the sample containers should be treated with 4 drops of 10 Sodium thiosulfate before autoclaving 4 3 Run test immediately after sampling or preserve sample at 4 C for a maximum of 6 hours Reagents 5 1 Peptone powder 5 2 Peptone buffer solution pH 7 00 0 1 stored at 4 C 3 3 m ColiBlue24 media in plastic ampule stored at 4 C 5 4 Sodium thiosulfate 10 solution 5 5 Lysol disinfectant 20 solution Equipment amp Lab Ware 6 1 Vacuum flask 6 2 Pall Life Sciences single use 50 mm Petri dishes with pads 6 3 Millipore sterile 0 45 um 47 mm filter 6 4 Forceps 6 5 4 5 X 9 inch sterile sampling bags 6 6 Bunsen burner and striker 6 7 Pipettes and sterile tips 6 8 Sterilized filter holder plastic or glass 6 9 Gable topped water bath at 35 0 C 0 5 C 6 10 Thermometer 6 11 ASTM Thermometer 6 12 Tower Steam Indicator Strips 6 13 ODO Clave Heat Activated Deodorant Pads 6 14 Autoclavable Biohazard waste bags and deposit box 6 15 Autoclav
417. t Assessment Field Data Sheet high doc 10 91 8176 01 31 08 HABITAT ASSESSMENT FIELD DATA SHEET HIGH GRADIENT STREAMS BACK 7 Frequency of Riffles or bends SCORE 8 Bank Stability score each bank Note determine left or right side by facing downstream SCORE LB SCORE RB 9 Vegetative Protection score each bank Parameters to be evaluated in sampling reach SCORE LB SCORE RB 10 Riparian Vegetative Zone Width score each bank riparian zone SCORE LB SCORE RB TOTAL SCORE with normal pattern Occurrence of riffles relatively frequent ratio of distance between riffles divided by width of the stream lt 7 1 generally 5 to 7 variety of habitat is key In streams where riffles are continuous placement of boulders or other large natural obstruction is important bridge abutments evidence of past channelization i e dredging greater than past 20 yr may be present but recent channelization is not present 20 dae 15 a4 13 a2 fio fo ts fir fs 5sf0j3 2 3 0 Occurrence of riffles infrequent distance between rifles divided by the width of the stream is between 7 to 15 or shoring structures present on both banks and 40 to 80 of stream reach channelized and disrupted Occasional riffle or bend bottom contours provide some habitat distance between riffles divided by the width of the stream is between 15 to 25
418. t Quality Assurance Manual documenting all aspects of their quality system including control of Standard Operating Procedures SOPs and datasheets Documents issued as part of the quality system will be reviewed and approved by authorized personnel A master list identifying the current revision and distribution of documents in the quality system will be used to ensure that invalid and obsolete documents are not used Quality system documents will be uniquely identified by the date of the last revision issuing authority and the total number of pages or a mark indicating the end of the document The Lexington Fayette Urban County Government Division of Water Quality Town Branch Laboratory Quality Assurance Plan QAP and Standard Operating Procedures SOPs Price 2009 and the Kentucky Geological Survey s Standard Operating Procedures located in Appendix B will control the chemical laboratory document control Laboratories will be required to document the analysis of all quality controls associated with the analysis of the collected samples such that the entire data package along with a narrative description of the results and a list of all data qualifiers may be provided to the Wolf Run Watershed Page 28 of 67 Revision No 0 Based Plan Date April 11 2011 KDOW and LFUCG upon request Thus the laboratories will retain all data associated with the sample analysis for the duration of the grant period Third Rock s macroinvertebrate ident
419. t ayy ue QOUBDIFTUBIS pesiaa run ALOU IO IIV ALB JO SSA PONIA ON 230 AON LIO dis DNY THe NAT AVIN udV IGN 833 NWT FONVY YOOd 1 0 zZ lt a ao O y JONVY YOOd SUNA CYYONYLS JWYN INVIYLS Hd EO IERA a COTE RLL 10 O79TTZ UNVIAUVIA NMOLYALSAHO 67t xOd Od ANVdWOS SLondoud TWOUINTHD LLLOWET syugdead zuawrjd 10 gquauisamnbaa moi medpruy up ippiya unod jo yobal jo mo yusuidinbs pue squssval day Buya woy suauodwo fe yoaioid pue samypzadwal yBiy awanxa PIOAW qyguns anp OF gusuodwos 3832 je jo msodx po uojoid posy ssn Jaye a powuN des daurequo2 Jusdeal ay uay 7 asn dea Joye saqna 359 ISUN pue ysem Anp T 9 S p SO0URLUIJUTEA 29 2D Tuowudindy 459 1 i nnsa 3592 d aya uaqo ol spagpugis 10109 ata ysurede ajdures 3897 34 JO 10109 9 yoseu pue 1o0yezedujo ul aqni nasu y Pi s1U23UO 3Y KIU O SIW 213498 HAUT pug aqm aya dep bay ap Gano cl sdoip pazis AULIO Jun asuadsip 03 pana 304 APEI yodid 10 31220q 1oddo1p ap poH poppe aq OF BORNIOS 101e9 puj jo sdoip jo Jaquinu adod aya suTuteep 01 royeredwios aya jo 2uoy aya UO Jeq UON anasu ay peay aqm ap ul oydures aya 02 UOBNOS IOIWSIpYl ay ppy 7 O TO 9 au ui y 03 aqua aya ya ways pagsa eq OF 1978M aya yaa 2qna 3893 94s suny 1 JANPIDOS 159 L yd Ys O peyzaj asoy ueya 10y3 y spaas ye mq asvastp ayqqng ses AQ pajosjye ospe are sayezigayaaur ogenby anssyy dayo uo pu
420. t least 15 minutes 6 To clean an electrode contaminated with oils and fats immerse the electrode tip in a detergent solution Use a soft brush or ultrasonic bath if necessary Avoid scratching the glass bulb 9 QA QC Requirements 9 1 Ifsample is not collected properly or analyzed within 15 minutes another sample must be obtained and analyzed 9 2 Check electrode response An electrode is responding properly if its calibration slope meets the slope specifications of the electrode typically 58 3 mV at 25 C 9 3 Check calibration accuracy Return the electrode to a calibration buffer and measure the pH to test the system Rinse and recondition the electrode before measuring subsequent samples 10 Expected Results 10 1 KPDES Permit Requirements 1 6 0 mg L is the lowest pH allowed 2 9 0 mg L is the highest pH allowed In the event that analysis results indicate values greater then KPDES permit requirements retest If the value indicated by the retest is greater than KPDES permit requirements Immediately notify the Plant Superintendent and the Laboratory Supervisor 10 11 12 10 2 SOP WH pH West Hickman WWTP Laboratory Page 11 of 219 Revision Number 3 Last Revised 09 09 Process Ranges Typical values for each plant are Town Branch Influent 7 3 7 4 Town Branch Effluent 6 7 8 9 West Hickman Influent 7 1 7 4 West Hickman Effluent 6 4 7 7 Blue Sky Influent 7 1 7 5 Blue Sky Effluent
421. t method analytic standard concentrations instrument response and the calibration curve All calibrations record the equation of the calibration curve and the correlation coefficient 29 TB Laboratory QAP September 16 2009 Revision 1 14 4 14 5 14 6 Computerized Data Storage 14 4 1 The laboratory establishes and implements procedures for protecting the integrity of the data including data protection procedures during data entry and capture data storage data transmission and data processing Data is protected with lab password access only 14 4 2 The laboratory provides procedures for the maintenance of the security of the data including the prevention of unauthorized access to data and the unauthorized change of computer records 14 4 3 The laboratory maintains hard copy and or writes protected backup copies of computer generated records Administrative Records 14 5 1 Personnel qualifications The laboratory maintains records of personnel qualifications education experience and training 14 5 2 IDMP studies The laboratory maintains records of IDMP studies and any required repetitions of the IDMP for each analyst 14 5 3 Initials and signatures The laboratory maintains a log of names initials and signatures for all individuals who are responsible for signing or initialing any laboratory record Laboratory Record Entries and Change of Entries 14 6 1 Laboratory personnel sign or initial all three ini
422. t will be spread across the reach to give a comprehensive evaluation of the entire community B2 2 3 2 Multi Habitat This method involves sampling a variety of non riffle habitats with the aid of an 800 x 900um mesh triangular or D frame dip net The habitats sampled and the number or size of replicates will differ for headwater and wadeable sites as shown in Table 11 Each of these sub habitat samples will be composited into one multi habitat sample for each site Undercut Banks Root Mats These will be sampled by placing a large root wad into a triangular or D frame dip net and shaking vigorously The contents will be removed from the dip net and placed into a mesh wash bucket If undercut banks are present in both run and pool areas each will be sampled separately with three 3 replicates for both headwater and wadeable streams Marginal Emergent Vegetation exclusive of Justicia americana beds This habitat will be sampled by thrusting e jabbing the dip net into the vegetation for approximately Im and then sweeping through the area to collect dislodged organisms Material will then be rinsed in the wash bucket and any sticks leaves and vegetation will be thoroughly washed and inspected before discarding Three replicates will be conducted This sub habitat must be sampled for wadeable sites and may be sampled for headwater if present Bedrock or Slab Rock Habitats These habitats will be sampled by placing the edge of the dip
423. te Laboratory Wolf Run Watershed Based Plan Page 36 of 67 Revision No 0 Date April 11 2011 FIGURE 2 MEASUREMENT OF DISCHARGE THROUGH SUB SECTIONAL MEASUREMENTS Note Stream cross section showing intervals where water depth and velocity are measured Flow will be calculated for each box flow area for each box is d w and summed to obtain the flow for the entire stream Flow measurements will be conducted according to the KDOW s Measuring Stream Discharge Standard Operating Procedure KDOW 2010b as described below Under this procedure a tape measure of at least 100 feet is stretched across the stream so that it is taut and perpendicular to the stream flow lines The tape measure is located directly above the cross section to be measured and must not touch the water surface Identify the starting edge as either left edge of water LEW or right edge of water REW when facing downstream Determine the approximate width of the stream with active stream flow being sure not to include slack water areas Hence the edge of slack water areas will be considered the edge of the stream Discharge measurements are taken at several verticals defined as a point along the cross section where water velocity is measured at a defined depth or depths Twelve to twenty verticals will be targeted for streams lt 20 feet wide whereas twenty to thirty verticals will be targeted when stream width is gt 20 feet To calculat
424. te Analysis Completed Presevation None required Maximum Holding Time 48 hours Average Mixed Liquor Volatile Suspended Solids Sludge Volume Index SVI SSV30 x 1000 MLSS Sludge Density Index SDI 100 SVI LI d Sunday s Sheets Town Branch Laboratory Temperature C Calculated Dissolved Oxygen Value pH Meter Calibration 01 00 00 Temperature Ke First Buffer 7 00 pH Second Buffer 4 00 pH Third Buffer 10 00 pH Slope Calibrated By Log Number 23127 23128 Sample Name PTE M L STD Date Samples Collected 01 00 00 01 00 00 01 00 00 Time Analysis Started H Standard Units Analyst Date Analysis Completed 01 00 00 01 00 00 01 00 00 Presevation None required Analyze Immediately KPDES Permit Limits on Plant Effluent pH 6 0 mg L is the Lowest pH we can have on any given sample 9 0 mg L is the Highest pH we can have on any given sample pH Method EPA Method 150 1 pH Electrometric Issued 1971 Editorial revision 1978 and 1982 Charlie Begley 234 4886 Mark Stager 368 7296 04 26 63 PTE Date Samples Collected Time Analysis Started Date Analysis Completed 04 26 63 04 26 63 KPDES Permit Limits on Plant Effluent DO 7 0 mg L is the Lowest Dissolved Oxygen we can have on any given sample Dissolved Oxygen Method EPA Method 360 1 Oxygen Dissolved Membrane Electrode Issued 1971
425. team within 60 days of sample delivery to the laboratory The chemical laboratory data package will include the laboratory results completed chain s of custody lists of qualifiers associated with the data and a report of the quality control results The macroinvertebrate report data package will include a list of the identified species metric calculations habitat assessment scores photographs completed chain s of custody and a data analysis report This report will be submitted to KDOW and LFUCG prior to December 31 2011 A9 3 Quality Documentation and Final Reports The most recent version of this QAPP will be distributed to all parties listed on the distribution list after the QAPP has been reviewed and approved The QA Manager is responsible for ensuring that all applicable parties perform documented reviews of the QAPP If because of deviations in the QAPP revisions are required the QA manager shall ensure that all parties review the revised version The current revision and the date of the revision shall be documented in the upper right corner of the QAPP pages The QAPP shall be redistributed after all parties have reviewed the document Wolf Run Watershed Page 29 of 67 Revision No 0 Based Plan Date April 11 2011 As a result of this project multiple final reports will be used to document the findings of the monitoring performed under this QAPP Monitoring reports will be submitted to the KDOW and LFUCG in hardcopy upon
426. ted according to manufacturers instructions prior to each Wolf Run Watershed Based Plan Page 57 of 67 Revision No 0 Date April 11 2011 sampling event using a three point pH calibration and a one point conductivity calibration All results will be recorded in the instrument logbook The filter funnel tubing and flask used in field filtration will be cleaned prior to sampling or weekly at maximum To clean the equipment three clear HDPE washbasins will be used One washbasin will be labeled Detergent Wash one Acid Solution and the final DIW The detergent used for cleaning equipment must be certified phosphate free All washbasins used during the cleaning process must be pre cleaned following the same procedures 1 Detergent Wash and Tap Water Rinse a Put on powderless nitrile gloves b Place equipment in basin labeled Detergent Wash and soak equipment in a tap water detergent mix for 30 minutes c Fill tubing with solution and keep submerged for 30 minutes d Scrub exterior and interior surfaces of equipment e Rinse thoroughly with warm tap water to remove detergent residue 2 Acid Soak and Rinse a Put ona new pair of gloves b Place equipment and tubing into a washbasin labeled Acid Solution for pieces of equipment that contain metal parts skip to Step 3 c Fill washbasin with 5 HCl solution ACS trace element grade HCL 5 by volume in DIW d Soak for 30 minutes Stir solution occas
427. ted by changes in the established policies and procedures Use of Analytical Methods Not Approved by KYDEP or U S EPA When analytical methods are used which are not approved by KYDEP or U S EPA SOPs are used to document the actual procedures performed as well as the source s of the method The methods used to determine the criteria for IDMP are established and documented prior to use of the method Quality assurance and control procedures are included in the method Reporting of Non compliant Data Data which is produced from samples that do not meet the regulatory sampling holding or preservation requirements or which is produced using methods that deviate from EPA required analytical or QC requirements is reported only when accompanied by a statement that clearly indicates that the data may not be used for regulatory compliance purposes 35 TB Laboratory QAP September 16 2009 Revision 1 17 1 17 2 17 3 17 4 Section 17 Procedures for Dealing with Complaints Scope The Town Branch Laboratory has specific procedures for dealing with complaints from clients or other parties Complaint Receipt Procedures 17 2 1 Document the initial complaint with the following information e Name of person with complaint e Company name e Phone number e Sample Identification e Nature of complaint 17 2 2 Inform person with complaint that it will be investigated promptly Also inform him of the estimated time or date for a respon
428. terial for nickel cadmium batteries 42 TB Laboratory QAP September 16 2009 Revision 1 COD Chemical Oxygen Demand a measure of the oxygen consuming capacity of inorganic and organic matter present in water or wastewater It is expressed as the amount of oxygen consumed from a chemical oxidant in a specific test It does not differentiate between stable and unstable organic matter and thus does not necessarily correlate with biochemical oxygen demand The method can be applied to domestic and industrial waste samples having an organic carbon concentration greater than 15 mg L For lower concentrations of carbon such as in surface water samples the Low Level Modification should be used Organic substances in the sample are oxidized by Potassium Dichromate in 50 Sulfuric Acid solution at reflux temperature Silver Sulfate is used as a catalyst and Mercuric Sulfate is added to remove Chloride interference The excess Dichromate is titrated with standard Ferrous Ammonium Sulfate using Orthophenanthroline Ferrous complex as an indicator Chi Squared Test In setting up methods you may want to compare sex or age variables on value for a particular lab test It is a statistical test most generally suitable for determining whether or not an observed frequency of occurrence differs from that which is expected in accordance with some hypothesis Chlorine Cl An element ordinarily existing as a greenish yellow gas about 2 5 times as heavy as air
429. terioration including fire theft and electromagnetic deterioration in the case of electronic records 14 8 Raw Data Associated with Sample Analysis All raw data associated with sample analyses i e calibration curves strip charts tabular printouts computer data files analytical notebooks and run logs include the following 1 Laboratory sample number 2 Date of analysis 3 Type of analysis 4 Instrument identification 5 Instrument operating conditions or reference to such information 6 All calculations automated or manual to which the sample data is subjected 7 Analysts and or technician s initials or signature 14 9 Test Data Reports Laboratory sample data or sample result reports include the following 1 Report title such as laboratory results 2 A unique identification of the report such as serial number 3 Description and identification of samples 4 Date of sample receipt sample collection and sample analysis time of sample preparation and analysis if the required holding time for either activity is less than or equal to 48 hours 5 Characterization and condition of sample where appropriate 6 Reference to sampling procedure where applicable 7 Test method utilized 8 Sample results with any failures or deviations from approved test methods or QC criteria identified such as data qualifiers 9 Description of the calculations or operations performed on the data a summary and analy
430. th Test N Tube adapter 6 3 5 mL micropipetter with tips 6 4 2mL micropipetter with tips 6 5 Microfunnel Interferences 7 1 Do not use commercial detergents containing phosphate for cleaning any lab ware utilized in this method 7 2 Excess Turbidity Procedures 8 1 Steps 1 Turn the HACH DRB200 COD reactor ON and preheat to 150 C by pushing Start 2 Prepare a Reagent Blank by adding 5 mL of Nanopure lab water to a Total and Acid Hydrolyzable Test Vial and label it Reagent Blank 3 Prepare a Low Range Standard by adding 1 mL of phosphate standard solution 1 mg L as PO4 and 4 mL of Nanopure lab water to a Total and 25 4 5 6 7 8 9 10 11 SOP WH TP West Hickman WWTP Laboratory Page 26 of 219 Revision Number 5 Last Revised 09 09 Acid Hydrolyzable Test Vial and label it Low Standard to produce a standard of 0 2 mg L PO4 Prepare a High Range Standard by adding 5 mL of phosphate standard solution 1 mg L as PO4 to a Total and Acid Hydrolyzable Test Vial and label it High Standard to produce a standard of 1 0 mg L PO Put 5 mL of each sample to be analyzed in appropriately labeled Total and Acid Hydrolyzable Test Vials Make sure to save samples until samples are read in case samples need to be diluted and or reanalyzed Using a microfunnel add to each test vial the contents of one potassium persulfate powder pillow screw cap on tight shake f
431. the Dionex Ion Chromatography System a Fill the eluent reservoir s with fresh eluent b Make certain the waste reservoir is empty of all waste c Turn on the helium The system pressure should be between 7 15psi The system pressure can be regulated with the knob on the back of the Eluent Organizer d Connecting a piece of tubing to the gas line going into the eluent bottle and putting the tubing into the eluent degasses the eluent reservoir s The gas knob on the Eluent Organizer that corresponds to the eluent bottle should be slowly opened until a constant bubbling stream can be seen in the eluent bottle e The eluent should be degassed with helium for a minimum of 30 minutes before operation of the instrument f After the eluent has been degassed remove the tube from the eluent and tightly seal the eluent bottle The eluent is now ready to introduce into the system Whether using the IP25 for Fluorides or the GP50 for everything else turn off the browser scroll to REMOTE on the screen select LOCAL and ENTER Scroll to mL min change to 0 mL min and hit ENTER If using the IP25 pump skip to step 5 Hit MENU and select 1 then ENTER Insert syringe into the Priming Block open the gas valve on the Eluent Organizer turn the valve on the Priming Block counterclockwise and turn on the pump that corresponds with the method to be ran by pushing the OFF ON button If the syringe does not fill freely assist by gently pull
432. the extent of the effects of hydromodification in the Wolf Run watershed Effects of hydromodification that may be revealed by the assessment include degree of bed and bank erosion sedimentation and habitat loss The relative potential for improvement will also be qualitatively assessed based on the lack of obvious physical constraints in a reach position in the landscape or position in the watershed B1 2 6 Water Quality Monitoring The objective of the water quality monitoring is to provide sufficient temporal and geographic data to evaluate the sources and loadings of water quality pollutants The sampling period of ten months was selected in order to evaluate at least one sample from all seasons The twelve sampling stations were selected in order to evaluate the relative contributions of the stream reaches throughout the watershed Flow will be measured on the receiving streams because it is a component of the formula for calculating loading of pollutants in the watershed Dissolved oxygen temperature and pH will be assessed as basic measurements for describing the health of the stream and evaluating applicable water quality standards E coli and fecal coliform will be used to assess health risk due to waterborne pathogens Specific conductance and total dissolved solids will be used to assess dissolved ions levels present in the watershed Turbidity and TSS will be recorded to assess the suspended solid levels for impacts to stream biota due
433. the foil from the DosiCap Zip in step 1 2 Replace the cap in its original position in step 3 3 Subtract the value obtained in step 8 from the value obtained on the original sample to give the corrected sample concentration Samples without color or turbidity do not require sample blanks 7 6 Helpful Hints 1 After washing used glassware all glassware must be thoroughly rinsed with lab grade water 2 Analysis results are directly proportional to sample volumes therefore it is very important that sample volume measurements are accurate 3 Ammonia TNTplus tubes are temperature sensitive and must be stored in the refrigerator 4 C when not in use Standard Preparation 8 1 ULR Low Standard 1 01 mg L NH3 N Combine 1 00 mL of 10 1 mg L standard 9 0 mL DI water 8 2 HR High Standard 10 1 mg L NH3 N Add 20 0 mL of stock ammonia standard solution 100 ppm NH3 N to 200 mL volumetric flask Dilute to 200 mL with Nanopure water QA QC Requirements 9 1 A low standard 1 01 mg L and a high standard 10 1 mg L must be analyzed with every analytical run 92 5 of all samples must be run in duplicate Duplicate concentration values should agree within 5 9 3 Data acceptance criteria Analysis values for Standards must agree within 10 of the standard s known value and duplicate values must agree within 5 If these criteria are not met corrective action is indicated See Quality Assurance Program QAP Sec 15 Corr
434. this analysis is 28 days 2 Safety Safety glasses gloves and a lab coat should be worn while performing this analysis due to the use of and possible exposure to strong acids and bases 3 Apparatus Varion 50 Spectroscopy system Filtration Apparatus Coors 60242 Biichner funnels Suction flasks connected in series to a vacuum system Reservoir for the filtrate 500 mL Trap which prevents liquid from entering the vacuum system 1000 mL Paper filters 7 5 cm 1 um VWR Cat 28321 005 Analytical balance capable of weighing to the nearest 0 0001 g Drying oven Desiccator Thermix Stirring Hot Plate Model 610T HCl Acid washed glassware Refer to the Total P section of the Glassware GLP for further details Commercial detergents should never used Glassware should be dedicated for Total P use only 6 Y oz Disposable polystyrene specimen cups Cups should be rinsed three times with DI water 4 Reagents Purity of Reagents Reagent grade chemicals shall be used in all tests Unless otherwise indicated all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society Other grades may be used provided it is first ascertained that the reagent is sufficiently high in purity to permit its use without lessening the accuracy of the determinations Purity of Water Unless otherwise indicated references to water shall be understood to mean Type I reagent grade wate
435. tials all record entries The reason for the signature or initials is clearly indicated in the records including but not limited to sampled by prepared by and reviewed by 14 6 2 Permanent ink is used for manually recorded data 14 6 3 Corrections of manually recorded data are made by one line through the error The correction is initialed and dated Corrections are not made by erasure or White Out 14 6 4 Electronically maintained records are kept in such a fashion as to indicate any change in the record 14 6 5 After the laboratory delivers its sample data and results to client the laboratory will only correct add or delete information from the report when it supports those actions by supplementary documentation Any supplemental report clearly identifies there purpose and contains all reporting requirements 30 TB Laboratory QAP September 16 2009 Revision 1 14 6 6 Facilities with in house laboratories which provide data to regulatory agencies must include all items in Section 14 10 with their reports if so required by the regulatory agency 14 7 Record Retention 14 7 1 All records are retained for a minimum of five years They include information pertaining to environmental analyses performance testing obsolete or replaced procedures and supplies for tests support services and laboratory accreditation 14 7 2 Access to archived records is documented with an access log All records are protected against loss of de
436. time and date in the Microbiology bench sheet After 24 2 hours count blue colonies See Section 10 Log results initials time and date in the Microbiology bench sheet 20 8 2 8 3 SOP WH Fecal Coliforms West Hickman WWTP Laboratory Page 21 of 219 Revision Number 4 Last Revised 09 09 Before and After Blanks 1 Blanks must be analyzed before and after filtration of a set of samples 2 Before any sample is filtered place a sterile filter in the filter holder unit 3 Add 50 mL peptone buffer to filter unit 4 Turn on vacuum and filter the buffer this will be the Before Blank 5 Remove and plate filter as indicated in Section 8 1 6 Proceed with sample filtration and plating 7 Runa Known Positive after all samples have been filtered See Section 8 3 8 Place a sterile filter in the filter holder unit 9 Add 50 mL peptone buffer to filter unit 10 Turn on vacuum and filter the buffer this will be the After Blank 11 Remove and plate filter as indicated in Section 8 1 12 Log results initials time and date in the Microbiology bench sheet Known Positive 1 2 3 4 5 6 After all samples have been filtered a Known Positive is filtered and plated to ensure growth Place a sterile filter in the filter holder unit Add 10 20 mL peptone buffer to filter unit then pipet 1 0 mL of mixed liquor or suitable sample with known fecal coliforms into filter unit Turn on vacuum and filter t
437. ting and supervising Laboratory Technicians in a variety of chemical bacteriological tests and analyses on water released from wastewater treatment plants to determine conformance to EPA mandated standards Also conducts and supervises Laboratory Technicians in the monitoring testing and analysis of industrial waste and other discharges into the sanitary sewer systems to determine compliance with local State and EPA permits and other applicable rules regulations Essential Functions Administration Supervision Set up a laboratory budget and maintain budget records Set up and maintain laboratory personnel records Do employee evaluations Deal with employee problems Do job interviews for new employees Set up employee work schedules Set up and maintain all necessary records and reports as required by the state and EPA Prepares and submits all required records and reports to state and Environmental Protection Agency Do all ordering of supplies and specification of equipment for the laboratory and also for other departments wanting lab related equipment Supervises and trains Laboratory Technicians on laboratory and testing procedures Supervises the cleaning and sterilization of laboratory equipment utensils and facilities Supervises the storage of all chemicals insuring that all required safety and storage procedures are followed Supervises the proper collection of sewage and sludge samples during various phases of wastewater treatm
438. tion The Laboratory operates as a department of the Division of Water Quality for the Lexington Fayette Urban County Government LFUCG The laboratory performs analyses on samples from the Town Branch WWTP the West Hickman WWTP the Blue Sky WWTP several industrial pretreatment samples and samples brought in from other outside sources A list of samples and analyses performed are presented in Appendix A 2 2 Staff Responsibilities Appendix B contains job descriptions and responsibilities for all laboratory positions 2 3 Current Personnel Appendix C lists the laboratory s positions names of personnel education and approved signatures TB Laboratory QAP September 16 2009 Revision 1 Section 3 Organizational Charts 3 1 Laboratory s Place in Company and Laboratory Organization Diroctor Division of Water Quality i i TE HODE DE fi iH Public Servico Equipment Engineering Engineenng Worker Operator valor Technician Sr Technician oe Public Service Treatment Plant j Worker Sr Apprentce HE 3 2 Laboratory s Organization 3 2 1 Mrs La Vada Green QA QC Manager 3 2 2 Mr DiLinh Cao Laboratory Safety 3 2 3 Mrs Maria Lundin Microbiology 3 2 4 Mr Brian Reynolds Database administration TB Laboratory QAP September 16 2009 Revision 1 4 1 4 2 4 3 4 4 Scope Section 4 Documentation Control and Maintenance Procedures The laboratory maintains document control procedures for its
439. tion and there is evidence that the chilling process has begun such as arrival on ice Town Branch Lab refrigerated storage unit temperatures are checked and documented daily Temperature must be 4 C 2 C Samples are examined for chemical preservation upon receipt or prior to additional sample preparation or analysis Actions for Deviations from the Lab s Sample Acceptance Requirements Deviations from the sample acceptance policy is brought to the attention of the Laboratory Analyst and documented at the time of sample log in 25 TB Laboratory QAP September 16 2009 Revision 1 12 4 2 Whenever possible the laboratory proceeds to correct errors in sample documentation The person responsible for the error is contacted so that a deviation from the sample acceptance policy can be avoided 12 4 3 Ifa sample does not meet all of the sample acceptance criteria e Retain correspondence and records of information concerning the final disposition of rejected samples e Contact client from which the laboratory received samples 12 5 Laboratory Log of Received Samples Each sample received is logged with the following information date and time of laboratory receipt of sample sample collection date whether sample is composite or grab unique laboratory identification code sample collection point requested analyses signature or initials of data logger comments resulting from inspection for acceptance or rejection sampl
440. tirrer replacement kit HACH part 5850800 Interferences 7 1 Salinity salinity correction available See Section 8 4 3 of the Users Manual 7 2 Reactive gas chlorine and hydrogen sulfide 7 3 Air bubbles in sample or on surface of probe tip Procedures 8 1 Steps 8 1 1 Calibration and Start Up It is recommended that the HQ40d Users Manual be initially consulted when following these procedures The manual is located in a yellow folder labeled Lab D O Meter in the yellow bin located adjacent to the meter 1 Press the power button and allow the unit to perform its startup self check routine 2 Clean by rinsing with Nanopure lab water then gently blot dry the probes tip with a Kim Wipe Inspect the probe tip for indications contamination or damage 3 Take a 300 mL BOD bottle containing approximately one inch of lab water stopper and shake remove stopper and replace it with the probe 40 4 5 6 7 8 SOP LAB D O LFUCG Laboratory Page 41 of 219 Revision Number 5 Last Revised 09 09 Press Calibrate blue button the meter will prompt you to Dry the probe and place in water saturated air amp press Read Press the Read button the screen will scroll from 0 to 100 then indicate Calibration Complete Record from display screen both the temperature and the dissolved oxygen value indicated under the temperature Log the values on the dissolved oxygen calibration section
441. to 1 L preserve with 2 mL chloroform CHC1 Nitrate Working Standard 10 ppm Dilute 100 mL of Nitrate Stock Standard to 1000 mL in IL flask Preserve with 2 mL chloroform CHCl Store in refrigerator for no longer than 6 months Calibration Standards for the SYSTEM 2 TKN methods are prepared as follows 1 Using the 100 ppm Glutamic Acid Stock Standard prepare the following a 0 4 ppm 1 mL of 100 ppm diluted to 250 mL b 0 8 ppm 2 mL of 100 ppm diluted to 250 mL c 1 6 ppm 4 mL of 100 ppm diluted to 250 mLl 2 Using the 10 ppm Nitrate Stock Standard prepare the following 0 1 ppm 1 mL of 10 ppm diluted to 100 mL 0 2 ppm 2 mL of 10 ppm diluted to 100 mL 0 4 ppm 4 mL of 10 ppm diluted to 100 mL 0 8 ppm 8 mL of 10 ppm diluted to 100 mL 1 6 ppm 16 mL of 10 ppm diluted to 100 mL 2 9 ppm 29 mL of 10 ppm diluted to 100 mL 3 The QC is diluted from the ordered solution perform an appropriate dilution creating a QC with a value on calibration curve 1 5 ppm using the ordered standard E 4 If it is deemed necessary ICV s Initial Calibration Verification and CCV s continuing Calibration Verification can be run using a 0 8 ppm and or 1 6 ppm glutamic acid solution Outside Source Certified Quality Control Sample ERA 4 Procedure A Instrument Preparation 1 11 12 13 14 15 16 Before turning on the Dionex Ion Chromatography System a Fill the eluent reservoir s with fre
442. to a 1000 mL volumetric flask partially filled with water then fill to volume 3 Calibration Standard 3 Pipette 2 5 mL of 1000 mg mL NaNO stock standard 2 5 mL of 1000 mg L NaF stock standard 10 mL of 1000 mg L NaCl stock standard and 40 mL of 1000 mg L K SO stock standard into a 1000 mL volumetric flask partially filled with deionized water then fill to volume 4 Quality Control Sample Pipette 1 0 mL of 1000 mg L NaNO stock solution 1 0 mL of 1000 mg L NaF stock solution 8 mL of 1000 mg L NaCl stock solution and 30 mL of mg L KSO stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Calibration Standards for the SYSTEM2 NITRATE Fluoride method are prepared as follows 1 Calibration Standard 1 Pipette 0 01 mL of 1000 mg L NaF stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume 2 Calibration Standard 2 Pipette 0 05 mL of 1000 mg L NaF stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Calibration Standard 3 Pipette 0 1 mL of 1000 mg mL NaF stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Calibration Standard 4 Pipette 0 5 mL of 1000 g mL NaF stock standard into a 1000 mL volumetric flask partially filled with water then fill to volume Calibration Standard 5 Pipette 1 0 mL of 1000 mg L 1000 stock standard into a 1000 mL vo
443. treams are being effected by hydromodification including erosion rates changes in the streambed and position within the cycle of channel evolution in order to guide and prioritize remediation efforts Bunte Kristin Abt Steven R 2001 Sampling surface and subsurface particle size distributions in wadable gravel and cobble bed streams for analyses in sediment transport hydraulics and streambed monitoring Gen Tech Rep RMRS GTR 74 Fort Collins CO U S Department of Agriculture Forest Service Rocky Mountain Research Station 428 p Harrelson C C C L Rawlins and J P Potyondy 1994 Stream channel reference sites An illustrated guide to field technique General Technical Report RM 245 Fort Collins CO U S Department of Agriculture Forest Service Rocky Mountain Forest and Range Experiment Station 61p Rosgen D L 2008 River Stability Field Guide Wildland Hydrology Pagosa Springs CO Grab sampling Identify loading of water quality parameters to identify whether specific pollutants are causing impairments in the watershed KDOW Watershed Watch Water Chemistry Sampling Methods for Field Chemistry and Lab Analysis http www lrww org training chem test pdf KDOW 2009a In situ Water Quality Measurements and Meter Calibration Standard Operating Procedure Kentucky Department for Environmental Protection Division of Water Frankfort Kentucky DOWSOP03014 KDOW 2010b Measuring Stream Discharge Standard Op
444. trees understory shrubs herbs and non woody macrophytes vegetation disruption through grazing or mowing minimal or not evident almost all plants allowed to grow naturally Suboptimal 70 90 of the stream bank surfaces covered by native vegetation but one class of plants is not well represented disruption evident but not affecting full plant growth potential to any great extent more than one half of the potential plant stubble height remaining Marginal 50 70 of the stream bank surfaces covered by vegetation disruption obvious patches of bare soil or closely cropped vegetation common less than one half of the potential plant stubble height remaining Poor lt 50 of the stream bank surfaces covered by vegetation disruption is very high vegetation has been removed to 5 cm or less in average stubble height Parameter 10 Riparian Vegetative Zone Width This metric measures the width of the natural vegetation from the edge of the stream bank through the riparian zone The presence of old fields paths walkways etc in otherwise undisturbed riparian zones may be judged to be inconsequential to highly destructive to the riparian zone Each bank is scored independently from 10 0 When determining final scores the age and density of the riparian vegetation should be evaluated e g A score of 9 instead of 10 should be given to a riparian zone that is over 20 m in width but is dominated by 5 10 year old hardwood trees Optima
445. ty control or quality assurance Answers telephone inquiries and relays messages and information Responsible for knowing and complying with all UCG and division safety rules and for attending safety meetings Performs other related duties as required Knowledge Skills and Abilities Considerable knowledge of the principles practices and techniques of bacteriology and chemistry the operation and maintenance of complex chemical laboratory equipment and the safety requirements of a chemical laboratory in the performance of various tests and the storage and use of a variety of chemicals Fundamental knowledge of the design and operation of an AA or ICP to facilitate repair and or assistance in troubleshooting Knowledge in the use of micro or personal computers to sort data monitor trends generate reports modify existing and create new programs using spreadsheet applications Good knowledge of State and Environmental Protection Agency EPA quality control procedures record keeping and report requirements Good observational skills to detect problems in analytical procedures and to detect possible errors in data entry sample processing etc Ability to establish and monitor new testing procedures to meet state and EPA requirements Ability to use a variety of complex laboratory equipment and understand set up and run all standard laboratory tests on wastewater sludge and industrial waste as required by regulatory agencies Ability to tr
446. ubbles and waves the surface area is increased and more oxygen can enter the water Photosynthesis In the leaves of plants one of the most important chemical processes on Earth is constantly occurring photosynthesis During daylight plants constantly take carbon dioxide from the air and in the presence of water convert it to oxygen and carbohydrates which are used to produce additional plant material Since photosynthesis requires light plants do not photosynthesize at night so no oxygen is produced Chemically the photosynthesis reaction can be written as Light nCO nHO CHO nO Light Carbon Water gt Carbohydrate Oxygen Dioxide 11 WHERE DOES THE OXYGEN GO Once in the water oxygen is used by the aquatic life Fish and other aquatic animals need oxygen to breathe or respire Oxygen is also consumed by bacteria to decay or decompose dead plants and animals Respiration All animals whether on land or underwater need oxygen to respire grow and survive Plants and animals respire throughout the night and day consuming oxygen and producing carbon dioxide which is then used by plants during photosynthesis Decomposition All plant and animal waste eventually decomposes whether it is from living animals or dead plants and animals In the decomposition process bacteria use oxygen to oxidize or chemically alter the material to break it down to its component parts Some aquatic systems may
447. ucky 2008 Signature Job Title Laboratory Technician QA QC Manager Name La Vada M Green Employee 22849 Education B S Physics Eastern Kentucky University Signature Job Title Laboratory Technician Safety Officer Name Di Linh Cao Nguyen Employee 39494 Education B S Biology University of Kentucky 1997 Signature TB Laboratory QAP Appendix C September 16 2009 Revision 1 Job Title Laboratory Technician Microbiology Name Maria Lundin Employee 45854 Education B S Biology University of Wisconsin Green Bay 1995 Signature Job Title Laboratory Technician Name Jerry W McDaniel Employee 35894 Education Navy training Medical Technology 1974 Signature Job Title Laboratory Technician Database management Name Brian Reynolds Employee f 43385 Education B S Biology Eastern Kentucky University 2006 Signature TOWN BRANCH LABORATORY STANDARD OPERATING PROCEDURES SOP Alkalinity LFUCG Laboratory Page 2 of 219 Revision Number 2 Last Revised 9 09 Alkalinity Titrimetric Standard Methods 2320 B Scope Significance to Process and Application 1 1 This method is applicable to drinking surface and saline waters as well as domestic and industrial wastes Summary of Method 2 1 Executive Summary The principle of operation for the Orion Test Kit is the same as the conventional titration A pre measured volume of reagent is added to the samp
448. ucky 40511 Lexington KY 40503 859 425 2416 859 977 2000 Matrix Code Preservation Type _ Field Remarks Turnaround Time Required 30 Working Days pS War RAE Preservative Code Container Size Type j SA H2S04 80z 4oz 40z 320z Comments ST Na28203 P p P P Ammonia to RL of 0 05mg L sia Requested Lab Analysis On Site Field Measurements Nitrite to RL of 0 03 mg L Conductivity Calibration Methodology Required 40CFR Part 136 Known 714 uS cm Initial Calibration uS cm 2 Known 1438 uS cm Initial Calibration uS cm e lt Sample Location Matrix Date Time Analysis wo1 11 efn fili wo2 11 efn pafat 1 wos 11_ Po y pp wo4a 11_ Po tn lalo y WO5 11_ efn pif 1 wo6 11 o n Wo7 o efn pata pop e AL E ME W Slightly turbid TDS Hardness Fecal coliform turbid or indicate if other clear 2 Dissolved Oxygen mg L ololo Jo zlz z Turbidity Visual 1 3 Specific Conductance Temperature C Q zZ OJO z jz wos efn Woot o n a S AAA woni ooo c n aaa pop ff Wie ooo c n HA A TEA te EEES WDD 14 1 W121 o efn Relinquished By Date Time Received By Date Time Temp Upon Receipt C Measured By Containers Properly Preserved Yes No Headspace Yes No NA Bottles Intact Yes No COC Seals Intact Yes No NA Additional Documentation Attached Yes No 9 Zz Q zZ Q Zz
449. un Watershed Monitoring Organization Chart oooonccnnnccniccnincnnnncccnnacos 10 Figure 2 Measurement of Discharge Through Sub Sectional measurements 37 List Of Appendices Appendix A Datasheets Appendix B Standard Operating Procedures Wolf Run Watershed Page 8 of 67 Revision No 0 Based Plan Date April 12 2011 A3 Distribution List The following individuals will receive the approved Quality Assurance Project Plan QAPP and any subsequent revisions Name Address Phone Number E mail Address Steve Evans Third Rock Consultants LLC 2526 Regency Road Suite 180 Lexington KY 40503 859 977 2000 sevans thirdrockconsultants com Gerry Fister Third Rock Consultants LLC 2526 Regency Road Suite 180 Lexington KY 40503 859 977 2000 gfister thirdrockconsultants com Marcia Wooton Third Rock Consultants LLC Bert Remley Third Rock Consultants LLC 2526 Regency Road Suite 180 Lexington KY 40503 2526 Regency Road Suite 180 Lexington KY 40503 859 977 2000 859 977 2000 mwooton thirdrockconsultants com bremley thirdrockconsultants com Jennifer Shelby Third Rock Consultants LLC 2526 Regency Road Suite 180 Lexington KY 40503 859 977 2000 jshelby thirdrockconsultants com Susan Bush Lexington Fayette Urban County Government 200 East Main Street Lexington KY 40507 859 425 2800 sbush Ilfucg com David Pri
450. und in Section 186 155 of Illinois regulations Title 35 Environmental Protection Subtitle A General Provisions Chapter I Environmental Protection Agency Part 186 Accreditation of Laboratories for Drinking Water Wastewater and Hazardous Waste Analysis Copies of this document may be obtained from the laboratory supervisor or the quality assurance officer 15 TB Laboratory QAP September 16 2009 Revision 1 8 2 8 3 8 4 8 5 8 6 Balances The laboratory s analytical balance has a sensitivity of 0 1 mg All analytical balances are placed on a stabilizing slab base Each balance is checked daily with two or more ASTM type 1 weights which cover the effective range of the balance s use All balances are serviced and calibrated at least annually by a qualified service representative The service representative issues the laboratory a certificate of calibration with weights traceable to National Standards pH Meters All pH meters have an accuracy of at least 0 1 pH units and provide for temperature correction of pH measurements Daily calibrations are performed with a minimum of three standardization buffers as specified in SOP pH The pH of the standardization buffers are 4 0 7 0 and 10 0 Conductivity Meters A conductivity meter is maintained with an error not exceeding 1 or one micromhos cm whichever is greater The conductivity meter is calibrated before each use with a standard that reflects the sample conduct
451. uring that no disturbed streambed sediment contaminates the sample If additional work is planned upstream of the sample site the water samples must be taken first Care should be taken not to displace the preservative since sample bottles are pre prepared If bottles are not pre preserved triple rinse the sample bottle with stream water prior to sample collection When sampling point the mouth of sample container upstream against the flow Submerge the entire bottle and fill it with water If the stream is too shallow to fill the bottle while submerged fill as much as possible while submerged ensuring the minimal amount for analysis is obtained Also if the bottle contains a preservative angle the mouth so as not to spill the preservative while collecting Rinse the caps with sample water prior to capping the bottle Samples should be stored in containers that are free of potential contaminants Sample bottles may be placed inside sealed food grade plastic bags prior to being stored on ice in coolers to improve laboratory sorting and reduce potential cross contamination For bacterial samples fill bottles to the inscribed fill line Do not pour off excess water If the bottle is filled above the 100ml fill line the excess will be decanted during laboratory analysis If adequate volume is not obtained on first effort do not reuse the bottle Use a new un contaminated bottle and repeat the procedure Close and secure the sample bottle lid
452. us HR 1 5 15 0 mg L PO 1 2 3 4 Carefully pipet 0 5 mL of sample into the vial Pipet 0 2 mL 200 uL of Reagent B into the vial Immediately close the Reagent B container Screw a grey DosiCap C onto the vial Invert the capped vial 2 3 times to dissolve the reagent in the DosiCap Install the Light Shield if applicable 72 8 5 8 6 5 6 7 SOP TP LFUCG Laboratory Page 73 of 219 Revision Number 1 Last Revised 09 09 When the timer expires invert the vial again 2 3 times Clean the outside of the vial with a Kim Wipe and insert it into the DR5000 cell holder The instrument reads the barcode then selects and performs the correct test Results are in mg L PO4 No instrument Zero is required Note and record the indicated values on the bench sheet TNTplus 845 Total Phosphorous LR UHR 2 20 mg L PO P 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Turn on the DRB200 Reactor Heat to 100 C For DRB200 Reactors with 16 mm wells make sure the 16 to 13 mm adapter sleeve are in each well before turning on the reactor Carefully remove the protective foil lid from the DosiCap Zip Unscrew the cap from the vial Carefully pipet 0 4 mL 400 pL of sample into the vial Flip the DosiCap Zip over so the reagent side faces the vial Screw the cap tightly onto the vial Shake the capped vial 2 3 times to dissolve the reagent in the cap Verify that the reagent has dis
453. ustrial effluents or fertilizer runoff Excessive ammonia concentrations are toxic to aquatic life and can exert an undesirable oxygen demand on the receiving stream Summary of Method 2 1 2 2 Executive Summary Ammonium ions react at pH 12 6 with hypochlorite ions and salicylate ions in the presence of sodium nitroprusside as a catalyst to form indophenol The amount of color formed is directly proportional to the ammonia nitrogen present in the sample Test results are measured at 690 nm Nitrogen Ammonia analysis at Town Branch Laboratory refers to the spectrophotometric analysis of nitrogen ammonia compounds in a water wastewater sample Discussion This method covers the determination of ammonia nitrogen exclusive of total nitrogen in drinking surface and saline waters domestic and industrial wastes ULR HACH method covers the range from 0 015 to 2 000 mg L NH3 N The samples are analyzed colorimetrically with a HACH DR 5000 Health amp Safety Precautions 3 1 3 2 Watch out for broken glass from beakers and cylinders Wastewater samples have the potential to be hazardous use appropriate caution SOP NH LFUCG Laboratory Page 9 of 219 Revision Number 1 Last Revised 09 09 Sample Handling and Preservation 4 1 4 2 4 3 4 4 4 5 4 6 Collect samples in clean plastic or glass bottles Best results are obtained with immediate analysis Preserve the samples by reducing the pH to 2 or less with at least
454. valuated as a composite The evaluator will face downstream when determining left and right bank For parameters 8 to 10 each bank will be scored independently from 10 to 0 At each sampling site results will be recorded on the High Gradient Habitat Assessment Field Data Sheet Photographs will be taken to document upstream and downstream conditions The following paragraphs summarize each of the ten parameters assessed Parameter 1 Epifaunal Substrate Available Cover This metric measures the relative quantity and the variety of stable structures such as cobble boulders fallen trees logs branches root mats undercut banks aquatic Wolf Run Watershed Page 44 of 67 Revision No 0 Based Plan Date April 11 2011 vegetation etc that provide refugia feeding opportunities and sites for spawning and nursery functions Optimal gt 70 of substrate favorable for epifaunal colonization and fish cover mix of snags submerged logs undercut banks cobble or other stable habitat and at a stage to allow full colonization potential i e logs snags that are not new fall and not transient Suboptimal 40 70 mix of stable habitat well suited for full colonization potential adequate habitat for maintenance of populations presence of additional substrate in the form of new fall but not yet prepared for colonization may rate at the high end of the scale Marginal 20 40 mix of stable habitat habitat availability less than desir
455. ve in the watershed in 1997 prior to the first impaired listing of Wolf Run educating the community about stream health and making initial steps toward a cleaner watershed This group continues to be an outspoken proponent of improving the water quality in Wolf Run The FOWR sponsors the Wolf Run Watershed Council consisting of groups and individuals working to improve the watershed A watershed plan is being developed in order to provide a comprehensive assessment of the health of the watershed citizen and stakeholder concerns watershed remediation strategies and implementation plans for the future This is being developed under a Section 319 h Nonpoint Source Implementation Program Cooperative Agreement C9994861 09 awarded by the Commonwealth of Kentucky Energy and Environment Cabinet Department for Environmental Protection Division of Water KDOW to LFUCG based on an approved work plan These federal funds were awarded to KDOW by the EPA under Section 319 h of the Clean Water Act Third Rock was selected as the environmental consultant for work under this grant through a request for proposal issued by LFUCG FOWR was also issued grant funding through a memorandum of agreement with LFUCG primarily to engage educate and solicit input from the public during the development of this plan In the development of the Wolf Run Watershed Based Plan WBP all known and relevant existing information pertaining to the watershed was compiled and
456. vided location the time sampled time received and time analysis began Note If sample hold time time sampled to time analysis begins exceeds 15 minutes the analysis is void and must be rerun beginning with resampling 13 Select END if done with analysis or Continue to proceed to the next sample to be analyzed Note More detailed general information on the AutoCAT unit can be found in the operator s manual with details on the Forward Amperometric procedure starting on page 101 The manual is located on the shelf adjacent to the AutoCAT unit 14 SOP WH Residual Chlorine West Hickman WWTP Laboratory Page 15 of 219 Revision Number 4 Last Revised 09 09 8 2 Chlorine Standard Analysis 1 2 3 4 5 6 7 8 9 10 Obtain a Chlorine Standard Solution 25 30 mg L ampoule from Chemical Storage fridge Carefully break top off ampoule Pipette 1 0 mL of standard into 1000 mL volumetric flask Bring to 1000 mL with Nanopure water Measure 200 mL of standard solution into beaker with stir bar Run titration as indicated in Section 8 1 Record results in bench sheet The Laboratory Supervisor will determine if the standard is within the expected range Measure 200 mL of Nanopure water into a clean 250 mL beaker and analyze as indicated in Section 8 1 This will be a Blank to confirm no chlorine carry over Record results in bench sheet If chlorine is detected re run Blank until Belo
457. w Detection Limit BDL is obtained 8 3 Helpful Hints 1 2 3 4 Analysis results are directly proportional to sample volumes therefore it is very important that sample volume measurement is accurate Clean conditioned electrodes are required for the production of sharp well defined endpoints that are needed for precise analysis Rinse electrodes thoroughly before and after each use with Nanopure water and store in Nanopure water Routine use of the Electrode Cleaning and Conditioning procedure as described in Section 9 1 4 of the Operator s Manual will prevent problems Glassware must be clean and free of chlorine demand see section 4 3 QA QC Requirements 9 1 A diluted standard 25 30 mg L and Blank s must be run once a week See Section 8 2 92 5 of all samples must be run in duplicate 9 3 Data acceptance criteria 1 2 3 Results for the Standard must agree within 10 of the standard s known value Duplicate values must agree within 5 If these criteria are not met corrective action is indicated See Quality Assurance Program QAP Sec 15 Corrective Action Policies and Procedures 15 10 11 12 SOP WH Residual Chlorine West Hickman WWTP Laboratory Page 16 of 219 Revision Number 4 Last Revised 09 09 Expected Results 10 1 KPDES Permit Requirements 10 2 KPDES Permit Limits on plant effluent residual chlorine at West Hickman WWTP is a maximum monthly avera
458. water lost on ignition of dry solids at 550 C This is a rough approximation of the organic matter Solids Fixed All matter remaining in a tare after ignition of dry solids at 550 C Suspended Solids Insoluble solids that either float on the surface of or are in suspension in water wastewater or other liquids Solid organic or inorganic particles colloidal dispersed 48 TB Laboratory QAP September 16 2009 Revision 1 coagulated flocculated physically held in suspension by agitation or flow The quantity of material removed from wastewater in a laboratory test expressed as milligrams per liter and referred to as nonfilterable residue This method is applicable to surface waters domestic industrial wastes and saline waters The practical range of the determination is 20 mg L to 20 000 mg L A well mixed sample is filtered through a standard glass fiber filter and the residue retained on the filter is dried to a constant weight at 103 to 105 C Non homogenous particulates such as leaves sticks fish and lumps of fecal matter should be excluded from the sample Preservation of the sample is 4 C for a maximum of 7 days Standard A highly purified material having a known weighed fixed value or concentration of the substance being analyzed Standard Deviation A measure of the scatter of individual values in a Gaussian distribution the square root of the arithmetic mean of the square of the deviation from the arithmetic
459. were collected will be documented In addition to the duplicate grab sample collection duplicate in situ measurements and flow measurements will also be made at this site Duplicate habitat assessments will be performed by all volunteer samplers as well as by Third Rock biologists at the six macroinvertebrate sampling sites These duplicate measurements will be used to evaluate precision amongst volunteers conducting habitat assessments During the karst characterization a minimum of five percent of measurements will be duplicated B5 2 Macroinvertebrate Taxonomic Quality Controls Ten percent of all sorting pans will be checked by a second sorter to assure that samples have been picked thoroughly These samples will be selected randomly using the MacLIMS database programming This check is documented on the Taxonomic amp Enumeration Efficiency Form Five percent of all identified samples will be re identified to insure QA QC by a second taxonomist These samples will be selected randomly using the MacLIMS database programming Ninety percent or greater composition comparability e g abundance and richness is the target success criteria If there is less than 90 percent comparability between the taxonomists then taxonomy must be reconciled by both taxonomists and a third taxonomist if deemed necessary This quality control process shall be documented on the Macroinvertebrate Sample Taxonomy Precision Form and Macroinvertebrate Sample Taxo
460. with nitric acid approximately 2 mL L of the acid Store preserved samples at 4 C for up to 6 months Bring the sample temperature to 15 35 C adjust the pH to about 4 with 5 0 N NaOH before analysis 4 3 To preserve samples for hexavalent chromium analysis adjust the pH to 8 with IN NaOH Store at 4 C for up to 24 hours Bring sample to 15 35 C No pH neutralization is required 34 SOP Cr 6 LFUCG Laboratory Page 35 of 219 Revision Number 3 Last Revised 09 09 Reagents 5 1 Chromium Total and Hexavalent TNTplus Reagent Set HACH TNT854 5 2 Chromium Trivalent Standard Solution 50 mg L Cr 5 3 Chromium Hexavalent Standard Solution 50 mg L Cr 5 4 Sodium Hydroxide 1 0 N and 5 0 N Equipment amp Lab Ware 6 1 HACH DRB200 Reactor 9x13 mm 6 2 Test Tube Rack 6 3 Variable volume pipette 1 5 mL and tips 6 4 Plastic beakers or medicine cups 6 5 TNTplus Reactor Adapter Sleeves 16 mm to 13 mm diameter 6 6 Funnel plastic or glass 6 7 Glass Microfibre Filter paper 125mm diameter 6 8 HACH DR5000 spectrophotometer Interferences 7 1 The ions listed in Interfering substances See HACH method have been individually checked up to the given concentrations and do not cause interference Cumulative effects and the influence of other ions have not been determined 7 2 Larger amounts of iron copper and reducing and oxidizing agents give low bias results Lead mercury and tin give high bias results 7 3 Im
461. with a reference potential or a combination electrode 2 2 Discussion There is no color change during analysis pH stands for power of hydrogen a measure of hydrogen ion concentration in solution Health amp Safety Precautions 3 1 3 2 Watch out for broken glass from beakers and cylinders Wastewater samples should be considered potentially hazardous Use proper personal protective equipment Sample Handling and Preservation 4 1 Samples should be analyzed as soon as possible within a 15 minute time window preferably in the field 4 2 Collect samples in clean plastic or glass bottles Sample containers should be filled completely and kept sealed prior to analysis Reagents 5 1 Buffer Solution pH 4 00 color coded red 5 2 Buffer Solution pH 7 00 color coded yellow 5 3 Buffer Solution pH 10 00 color coded blue 5 4 Nanopure Grade Laboratory Water 5 5 pH Electrode Storage Solution SOP WH pH West Hickman WWTP Laboratory Page 8 of 219 Revision Number 3 Last Revised 09 09 Equipment amp Lab Ware 6 1 HQ40d Dual Input Multi Parameter Digital Meter 6 2 PHC101 IntelliCAL Rugged Gel Filled pH Electrode Interferences 7 1 pH measurements are affected by temperature and can cause the reading to drift 7 2 Grease and other debris on the probe can cause inaccurate readings Procedures 8 1 Calibration 1 Refer to the operation section of the electrode or meter manual to prepare the PHC101 pH electrode
462. y of Samples The laboratory stores all samples within the confines of the laboratory and limits access to authorized laboratory personnel only Sample Disposal If possible samples and aliquots are kept to the end of the maximum permitted holding time in the event that re analysis of the sample is required Proper temperature and holding times must be observed for re analysis Analyzed samples or samples with expired holding times are disposed of properly 27 TB Laboratory QAP September 16 2009 Revision 1 Section 14 Record Keeping Data Review and Reporting Procedures 14 1 Scope The record keeping system allows historical reconstruction of all laboratory activities that produce the resultant sample analytical data The laboratory maintains complete sample tracking records Documentation of laboratory activities includes inter laboratory transfers of samples and sample extracts The laboratory issues sample data or sample result reports accurately and in a manner that is understandable to the recipient 14 2 Records Maintained by the Laboratory 14 2 1 The laboratory retains records related to all procedures and activities to which a sample is subjected These records include 1 Identity of personnel involved in sampling preparation and testing 2 Sample preservation including sample container and compliance with holding times 3 Sample identification number receipt log in acceptance or rejection 4 Sample storage
463. y of contamination do not allow the nitrogen cylinder to run until it is empty Once the regulator gauge reads 100 kPa switch the cylinder out for a full one The old cylinder should them be returned to room 19 for storage until the gas company can pick it up Make sure that the status tag marks the cylinder as EMPTY Sample Handling and Preservation Samples should be collected in glass or plastic bottles that have been thoroughly cleaned and rinsed with reagent water The volume collected should be sufficient to ensure a representative sample and allow for replicate analysis if required Most analytes have a 28 day holding time with no preservative and cooled to 4 C Nitrite nitrate and orthophosphate have a holding time of 48 hours Combined nitrate nitrite samples preserved with H2SO0 to a pH lt 2 can be held for 28 days however pH lt 2 and pH gt 12 can be harmful to the columns It is recommended that the pH be adjusted to pH gt 2 and pH lt 12 just prior to analysis Preserved samples should not be used for TKN and Total Nitrogen analysis Note Prior to analysis the refrigerated samples should be allowed to equilibrate to room temperature for a stable analysis 2 Apparatus Dionex DX500 Dionex CD20 Conductivity Detector Dionex GP50 Gradient Pump Dionex Eluent Organizer Dionex AS40 Automated Sampler Dionex ASRS Ultra Self Regenerating Suppressor Dionex Ionpac Guard Column AG4A Dionex Ionpac Analytical Column AS4
464. ygen values are typically less than 1 mg L Target values for mixed liquor dissolved oxygen concentration in the aeration basins is 2 0 mg L Plant effluent dissolved oxygen values must be maintained at or above 7 0 mg L Data Analysis and Calculations 11 1 None required values are taken directly when measurement stability is indicated Bibliography 12 1 Report on the Validation of Proposed EPA Method 360 3 Luminescence for the Measurement of Dissolved Oxygen in Water and Wastewater August 2004 HACH Company Loveland CO 2004 122 Memorandum EPA Recommendation for the use of HACH method 10360 Revision 1 1 January 2006 ATP Case N04 0013 12 3 HACH HQ Series Portable Meter Users Manual September 2006 Edition 5 HACH Company Loveland CO 2006 SOP WH pH West Hickman WWTP Laboratory Page 7 of 219 Revision Number 3 Last Revised 09 09 WH pH Electrometric EPA Method 150 1 pH Issued 1971 Editorial revision 1978 and 1982 HACH USEPA Electrode Method 8156 Scope Significance to Process and Application 1 1 At a given temperature the intensity of the acidic or basic character of a solution is indicated by a pH or hydrogen ion activity 12 ApH meter is accurate and reproducible to 0 1 pH unit with a range of 0 to 14 and equipped with a temperature compensation adjustment Summary of Method 2 1 Executive Summary The pH of a sample is determined electrometrically using either a glass electrode in combination
465. ysical structure and stream function that has occurred Information obtained from the hydrogeomorphic assessment will be used to supplement biological physicochemical and habitat data when Wolf Run Watershed Page 18 of 67 Revision No 0 Based Plan Date April 11 2011 determining the overall health of the stream reach and stream use designation This will also allow for the development of an understanding of the nature and location of the problems associated with channel modification Hydrogeomorphic assessments will quantify physical stream changes that occur over time help identify potential BMPs implementation solutions and prioritize reaches for implementation of those solutions A6 1 6 Water Quality Monitoring Water quality monitoring will be conducted at ten 10 monthly sampling events at a minimum of twelve 12 sampling stations in the watershed during dry and wet conditions The sampling date within each month will be flexible such that at least two of the events are considered wet weather and two of the events are considered dry weather Sampling parameters will include discharge E coli fecal coliform total suspended solids total phosphorus ortho phosphorus ammonia total kjeldahl nitrogen nitrate nitrite total dissolved solids turbidity dissolved oxygen specific conductance temperature and pH The LFUCG Town Branch laboratory will analyze samples for E coli fecal coliform total suspended solids amm
466. zero and is determined from analysis of a sample in a given matrix containing the analyte MDL a lua 99 S where t the t statistic for n number of replicates used for n 7 t 3 143 n number of replicates S standard deviation of replicates 8 References ASTM vol 11 01 1996 D 515 Standard Test Methods for Phosphorus in Water pg 24 ASTM vol 11 01 1996 D 1193 Specification for Water pg 116 EPA 365 2 Phosphorous All Forms Colorimetric Ascorbic Acid 01 2009 KGS 9056 Ion Chromatography of Water 1 Discussion Principle This method addresses the sequential determination of the following inorganic anions bromide chloride fluoride nitrate Kjeldahl nitrogen total nitrogen and sulfate A small volume of water sample is injected into an ion chromatograph to flush and fill a constant volume sample loop The sample is then injected into a stream of carbonate bicarbonate eluent The sample is pumped through three different ion exchange columns and into a conductivity detector The first two columns a precolumn or guard column and a separator column are packed with low capacity strongly basic anion exchanger Ions are separated into discrete bands based on their affinity for the exchange sites of the resin The last column is a suppressor column that reduces the background conductivity of the eluent to a low or negligible level and converts the anions in the sample to their corresponding acids The

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