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Wild Rice Sulfate Standard Sediment Incubation Experiment QAPP

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1. 7 17 Calibration Standards 7 17 1 Stock Standard 100 mg L In an acid rinsed 1 L volumetric flask dissolve 0 7491 g sodium sulfide nonahyrdate Na2S 9H20 Mallinckrodt 8044 or equivalent in approximately 900 mL of 0 025 M sodium hydroxide reagent Dilute to volume with 0 025 M sodium hydroxide reagent and invert to mix Prepare fresh daily Standardize this stock standard after preparation 7 17 1 4 In an acid rinsed 250 mL Erlenmeyer flask add 20 mL 0 0250 N iodine solution and 2 mL 1 1 HCI 7 17 1 2 Add 10 mL of 100 mg L stock standard 7 17 1 3 Titrate with 0 0250 N sodium thiosulfate until a straw yellow color appears 7 17 14 Add a few drops of 2 w v starch indicator mixture will turn blue and continue titration until blue color disappears 7 17 1 5 Calculate the concentration of stock standard using the following calculation A x B C x D x 16000 mL sample mg L sulfide Where A normality of iodine solution B mL of iodine solution used C normality of thiosulfate solution D mL of thiosulfate used Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 9 of 31 https inside mn gov sites MDH bureaus hpb phid env inorganics Gen Chem SOPs gen26 doc oo 1 QE 7 17 1 6 Two blanks should be run to verify t
2. A solution of one or more method analytes used to evaluate the performance of the instrument system with respect to a defined set of criteria LABORATORY SPIKED BLANK LSB an aliquot of reagent water or other blank matrices to which known quantities of the method analytes are added in the laboratory 10 115 01 3 E Post MUR Pagel 3 December 2010 sat 230 3 6 3 7 3 8 3 9 The LSB is analyzed exactly like a sample and its purpose is to determine whether the methodology is in control and whether the laboratory is capable of making accurate and precise measurements LABORATORY SPIKED SAMPLE MATRIX LSM An aliquot of an environmental sample to which known quantities of the method analytes are added in the laboratory The LSM is analyzed exactly like sample and its purpose is to determine whether the sample matrix contributes bias to the analytical results The background concentrations of the analytes in the sample matrix must be determined in a separate aliquot and the measured values in the LFM corrected for background concentrations LABORATORY REAGENT BLANK LRB An aliquot of reagent water or other blank matrices that is digested exactly as a sample including exposure to all glassware equipment and reagents that are used with other samples The LRB is used to determine if method analytes or other interferences are present in the laboratory environment the reagents or the apparatus LINEAR CALIBRATION
3. Barium Calcium Copper Iron Magnesium Sod um 2 Metals ICP MS 200 8 Aluminum Antimony Arsenic Barium Beryllium Cadmium Chromium Copper Lead Manganese Nickel Selenium Silver Thallium Zinc o OR OX OR OU 9 x ed 3 Mercury Cold Vapor AA 245 2 1631 4 Cyanide SM 4500 CN P 5 Alkalinity SM23208 6 O Phosphate SM4800 P E 7 Silica SM4500 SiO2 C 8 Fluoride SM4500 F C 9 Nitrate Nitrite SM4500 NO3 F 10 Nitrite SM 4500 NO2 B 11 Disinfection Byproducts 300 1 Bromate Chlorite Bromide Sulfate Chloride 12 Total Organic Carbon SM5310 C 13 Carbamates 531 1 Aldicarb Aldicarb Sulfone Aldicarb Sulfoxide Carbaryl Caxbofuran 3 Hydroxycarbofuran Methomyl Oxamyl 14 EDB and DBCP 504 1 1 2 Dibromoethane 1 2 Dibromo 3 chloropropane ENCLOSURE A May 5 7 2008 Certification Status Fully Fully Fully Fully Fully Fully Fully Fully Fully Fully Fully Fully Fully Fully Certified Certified Certified Certified Certified Certified Certified Certified Certified Certified Certified Certified Certified Certified Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory i Revision 9 Effective Date Date of last signature Page 64 of 67 http fyi health state mn us phl environmental index html
4. HC Arsenic form The program code HC is preprinted and test code 110 is highlighted but there may or may not be a preprinted X Multiple samples may be collected from one facility Code 601 lab preservation needs to be added for these samples The form and labels are e yellow Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 35 of 57 SAMPLE PROCESSING PROCEDURE SAMPLE DELIVERY SCHEDULE Samples are delivered via the following schedule Monday Friday Times are approximate and each company normally delivers only once per day U S Mail 8 00 8 30 AM United Parcel Service 9 00 10 00 AM Spee Dee Delivery 9 00 10 00 AM Federal Express Times vary may not deliver every day The U S mail is also delivered on Saturday some Holidays and occasionally on Sunday on Holiday weekends The other courier services do not deliver samples on Saturday Sunday or Holidays Individual collectors may bring in samples at any time of the day They may also bring them in after hours if necessary Samples brought in after hours should be placed in the Sample Receiving refrigerator or the after hours refrigerator in room L100 Opening Mailing Containers Open boxes and other mailing containers carefully You may need to use a retractable blade Exacto knife to open some boxes It is advisable to wear safety
5. Section No A 1 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 3 of 44 Section A 1 Approvals Continued Approval Date 11 03 2013 Edward Swain PhD Minnesota Pollution Control Agency Project Manager Research Scientist 3 651 757 2772 edward swain state mn us 11 14 2013 Patricia Engelking Minnesota Pollution Control Agency Contract Manager Planner Principal State 651 757 2340 pat engelking state mn us 11 17 2013 William Scruton Minnesota Pollution Control Agency QA Coordinator 651 757 2710 bill scruton state mn us Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 1 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 4 of 44 Approval Date E pl j wj e Je 11 07 2013 Paul Moyer Minnesota Department of Health Manager Public Health Laboratory 651 201 5669 paul moyer state mn us Amy Myrbo PhD University of Minnesota Twin Cities UMN National Lacustrine Core Facility Limnological Research Center LacCore LRC Laboratory Manager 612 626 7889 amyrbo umn edu Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 2 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 5 of 44 Section A 2 Table of Contents Contents Section A Proj
6. Time s 940 5 59 0 Precision Data for Nitrate Nitrite using a 10 0 mg N L standard RSD 0 90 Standard Deviation s 0 09 mg N L Mean x 10 01 mg N L Known Value 10 0 mg N L File Name 11 12 support HR omn Acq Date 12 Nov 2009 10 107 04 3 D Page 36 2 Dec 2010 sat Volts 0137 mr gt o 940 9 Time s Precision Data for Nitrate Nitrite using a 5 0 mg N L standard RSD 71 24 Standard Deviation s 0 062 mg N L Mean x 5 01 mg N L Known Value 5 00 mg N L File Name 11 12 support HR omn Acq Date 12 Nov 2009 7 98 amp amp 112 2t 20 gt 0 128 ae 24e 3 Time s 2 8e 3 Carryover Study Two 20 0 mg N L standards followed by three blanks Carryover Passed File Name 11 12 support HR omn Acq Date 12 Nov 2009 10 107 04 3 D l Page 37 2 Dec 2010 sat QuikChem Method 10 115 01 3 E DETERMINATION OF TOTAL PHOSPHORUS BY FLOW INJECTION ANALYSIS COLORIMETRY IN LINE PERSULFATE DIGESTION METHOD Method also includes Manifold Alterations to Analyze Ortho Phosphate Written by Lynn Egan Applications Group Revision Date 3 December 2010 LACHAT INSTRUMENTS 5600 LINDBURGH DRIVE LOVELAND CO 80539 USA 7 INSTRUMENTS A Hach Company Brand
7. Weight g of standard 2 diluted to final weight 250 g divide by factor below with DI water Weight g of standard 3 diluted to final weight 250 g divide by factor below with DI water Division Factor Divide exact weight of the standard by this factor to give final weight Stock Digestion Check Standards 1000 mg N L In a 500 mL volumetric flask dissolve x xx g test compound see table in about 400 mL DI water Dilute to the mark with DI water and invert to mix ED DoE d toluenesulfonate EE R toluenesulfonate A a c a Disodium EDTA NaOzCCH2N CH2CO2H dihydrate CH2CH2N CH2CO2Na CH CO H H 0 10 107 04 3 D Page 7 l 2 Dec 2010 sat Working Digestion Check Standards 1 5 5 mg N L By Volume In a 500 ml volumetric flask add 2 5 mL of Stock Digestion Check Standard 1 2 3 4 or 5 1000 mg N L Dilute to the mark with DI water invert to mix Prepare fresh weekly Working Standards 1 5 Concentration mg N L By Volume Volume mL of check standard 1 2 or 5 diluted to 250 mL with DI water By Weight Weight g of check standard 1 2 or 5 diluted to final weight 250 g divide by factor below with DI Water Division Factor Divide exact weight of the standard by this factor to give final weight 8 SAMPLE COLLECT ION PRESERVATION AND STORAGE 8 1 82 When samples must be stored for more than 24 hours they should be
8. i E i i i i Lab Use only Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 47 of 67 http fyi health state mn us phl environmental index html Appendix 5 Chain of Custody form for receipt of samples including those subject to criminal or civil custody MDH Chain of Custody E St Paul MN 55155 2531 Lab Use Only Potential Hazard Ve No Unkoown Circle One UL Yes phase add information to Comments below Standard CicilCrimiza Chain of Custody Circle Ono Minnesota Department of Health Public Health Laboratory Division Environmental Laboratory http fyi health state mn us phl environmental index html Appendix 6 Chain of Custody logbook page to internally track enforcement samples 000250 MOH CHEMICAL LABORATORIES CHAIN OF CUSTODY LOG Sample Number s Chain of Custory Record Site Matrix Sampler Accepted By Name Date Time Numbered By gt Name Date Time Bottles Rec d CUSTODY TRANSFER RECORD Quality Assurance Manual Filename qao001 Revision 9 Effective Date Date of last signature Page 48 of 67 Sample Number s HE 01287 02 3 87 Minnesota Department of Health Public Health Laboratory Division Environmental Laboratory http fyi health state mn us phl environmental index html
9. xl L Student s t T MDL Ls LEES DM TVMDL TV MDL between 1 and 10 ed l 1 E MOLER T IF I31 No TV E to Rit E D208H19 100 SUM D20 D31 H20 IF H2 12 H21 H18 100 T STDEV D20 D31 E VLOOKUP H20 898 C41 2 FALSE E E H19 H27 4 IF H29 1 No JF H29 10 No Yes IF H27 gt H18 No Yes RN IF Ia1z Yes JF H1g H18 Yes No aon ee E i Ea rue Value i Resultl Result2 Mean True Value Resulti2 Number of Points T z eioermi T m iommi al SR emme pja ade Cu mM EN Tee eSQRT r SUM Fesulti 2 Resut2 2 SUM Result Result 2 2 ym n 1 AM Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 57 of 67 http fyi health state mn us phl environmental index html Appendix 10 Policy and Procedure for Initial Demonstration of Capability Study for the Environmental Testing Units of the Public Health Laboratory Division Minnesota Department of Health Scope and Frequency This policy and procedure pertains to inorganic and o
10. Chemistry Calibration Data l Concentration mg N L 20 0 Calibration Fit Type Weighting Method Force through zero Sampler Timing Min Probe in Wash Period Sample Period Valve Timing Load Period Inject Period 10 107 04 3 D 3 10 0 1 00 45 samples h 80 s sample 35 80 mg N L 67 6 s 28 9 s Direct Bipolar 4 SAS 2 Order Polynomial 1 x No Page 30 15s 15s 10s 70 s 2 Dec 2010 sat Nitrate manifold l orangeAvhite Inidazole buffer Carrier DI water gt Manifold Tubing 0 8 mm 0 032 in i d This is 5 2 nL cm QC8000 8500 Sample Loop 40 cm Low Range Microloop High Range Interference Filter 540 nm l Apparatus An injection valve a 10 mm path length flow cell and a colorimetric detector module is required 7 135 cm of tubing on a 7 cm coil support Note 1 This is a two state valve used to place the cadmium column in line with the manifold nitrite only nitrate nitrite 5 E Rr cadmium column l When changing the in line manifold over to run for non digested nitrate nitrite you can remove the debubbler from port 6 of the injection valve to speed up the time to valve time 10 107 04 3 D Page 31 2 Dec 2010 sat Calibration Data for Nitrate Nitrite Low Range 5 288 CalStad A lt E ue 8 4726 2 000 mg L 2 900 mg L Vols e E z i 3 S 1 0 CalSind C CalSind
11. Frequency of Detection Level Studies With regard to the frequency of Detection Level Studies the laboratory must follow any requirements cited in the reference method or applicable regulatory program for which the data is to be used If no such requirements exist the frequency of a Detection Level Study is determined as follows 1 Hnitially as part of an IDC for each combination of method environmental matrix and instrument 2 At the discretion of the Unit Supervisor as part of an IDC for each analyst performing the analysis Note MN Rules do not require an MDL Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 52 of 67 http fyi health state mn us phl environmental index html 3 Whenever significant changes affecting the sensitivity of the analysis occur in the SOP matrix or instrument as determined by the Quality Assurance Officer in consultation with the analyst and Unit supervisor 4 When any other change occurs that in the opinion of the Quality Assurance Officer could significantly affect the precision or accuracy of the analysis Documentation and other requirements The Detection Level Study option chosen including the acceptance criteria and corrective actions that the analyst must take if the acceptance criteria are not met must be described in the SOP for both t
12. If you do not know the PWS first use the PWS Table View screen to find it see previous section 1 From the main screen use select View and pull down to select Lab Review 2 Using either the PWS Number or Program PWSN Collected Date etc search options enter the PWS and execute a search This should pull up all the sample records from that specific system 3 Click on individual samples to pull up more information about the samples Find the most recent sample with the same analysis codes and use that program code It is important to find a previous sample with the same analyses because a system can have samples under different programs depending on the analysis codes 4 If you cannot find the program code by following these steps contact EH for assistance If you are unable to obtain assistance before the sample must be submitted choose the code that seems most appropriate The code can be changed when you do obtain the correct information General Information on EH Program Codes While the information below is helpful always look up the facility information in the computer to determine the correct code even for community samples HZ SDWA Phosphorus study HY SDWA Lead Copper HJ new well Well Management groundwater quality HM private well water Community PWS ID s begin with a 1 Codes used are HA HB and HC There will normally be more than one code per community as determined by sample type HA commu
13. Numerical List Analysis Test Code Bottle Type Solids total suspended Solids total dissolved Alkalinity Chloride Sulfate Phosphate dissolved Nitrogen Ammonia Nitrite total Nitrate total Nitrite dissolved Nitrate dissolved CBOD BOD Arsenic Barium Cadmium Chromium Cobalt Copper Iron 3 113 114 122 123 129 130 136 137 145 146 152 154 108 109 General 1 liter General 1 liter General 1 liter General 1 liter General 1 liter Nutrient Nutrient General 1 liter Nutrient General 125 ml Nutrient General 2 liter General 2 liter Metals Metals Metals Metals Metals Metals Metals Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory l Effective Date Date of last signature Page 53 of 57 Lead 157 158 Metals Manganese 166 168 Metals Nickel 171 172 Metals Zinc 194 195 Metals Mercury 200 202 Mercury Vanadium 248 249 Metals Potassium 255 256 Metals Sodium 257 258 Metals Calcium 694 695 Metals Magnesium 696 697 Metals Bromide rarely ordered 455 2 40 ml vials ask organics VOC s 498 3 VOC vials set Parameter List by Bottle Type General 1 liter 3 5 22 23 28 67 General 125 ml 73 General 2 liter 83 96 Metals 108 109 113 114 122 123 129 130 136 137 145 146 152 154 157 158 166 168 171 172 194 195 248 249 255 256 257 258 69
14. d S B g 2 2 D a e f oD a S 1 gt z E E orthophosphorus Phenyl Phos 3 December 2010 sat Page 19 10 115 01 3 E Post MUR Silicate interference Time 1180 15 Seconds Amp 199146 Volts arses 0 lt 1000 ppm SiO2 5 5442 ug PA 1000 ppm SiO2 8 4373 ug PAL 1500 1650 100 1150 Seconde E A 1000 ppm SiO standard was injected This resulted in an average response of about 6 ppb P as PO Conclusion Silicate is not a significant interferent in this method Selectivity 166 667 Data Filename 050102A fdt Acq Date 01 May 2002 10 115 01 3 E Post MUR Page 20 3 December 2010 sat 17 3 TOTAL PHOSPHORUS MANIFOLD DIAGRAM Apparatus 4 5 7 12 A12 Note 1 Note 2 Note 3 Note 4 Note 5 Sample prep module Note Debubbler ewe Note 8 12 Dow cell PAD 50 Note gi 3B en WASTE Carrier 0 45 M Sulfuric acid KCI solution Reagent 5 Manifold Tubing 0 5mm 0 022 in i d This is 2 5 pL em QC8000 8500 Sample Loop 200 cm 0 032 1 d Interference Filter 880 nm A sample prep module with heater and UV lamp an injection valve a 10 mm path length flow cell a heater LM and a colorimetric detector module are required 70 cm of tubing on a 4 5 cm coil support 135 cm of tubing on a 7 cm coil support 255 cm of tubing on a 12 cm alternating coil support 150 cm of tubing on a 12 cm al
15. date L Quality Assurance Manuals Training Records ralning_Checkilst 2006 02 Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 44 of 67 http fyi health state mn us phl environmental index html Appendix 3 Record of Personnel Education and Training MDH Environmental Laboratory Document Number 2006 01 Quarterly Period Se ect One Jan Mar 2006 Apr Jun 200 E n Jul Sep 2008 Record of Personnel Education and Training Oct Dec 2006 Please Print Employee Name Job Title Instructions are on the back of this sheet Type ot Training Activity Trainer s Instruction Name Trainee s Signature Date Date Supervisor s Signature Page 1 of 2 LiQuatty Assurance Manua s Training Records Training_Record 2006 01 Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 45 of 67 http fyi health state mn us phl environmental index html Appendix 4 Sample analysis request form a k a Chain of Custody form Example of a form used by MDH Environmental Health Division AO EA E PA Minnesota Department of Health Section of Drinking Water Protection Environmental Laboratory Request Form ps AA ARRA wap
16. 0 Date 12 9 2013 Effective Date Date of Last Signature Page 27 of 44 Section B 3 Sample Custody Section B 3 1 Overview Sample possession must be traceable from the time samples are collected until they are disposed of To maintain and document sample possession chain of custody COC procedures are followed Section B 3 2 Microcosm Sampling Custody Procedures The microcosm sampling personnel either have the samples in their possession in their view in a secured area that only they have access to or turn custody over to another individual who has signed the chain of custody COC form See Attachment 3 for an example COC form The COC is the record of all individuals who come in contact with the samples A copy of the chain of custody is maintained at all times to ensure the samples can be used in for enforcement A COC has the following information present Date and time of sampling Name of sampler Identification number of the samples Analytical methods requested Project name Signature of the sampler and MPCA contact name and phone number O nmMmOoOnw gt Sample custody is maintained from collection through analysis The samples are cooled on ice The chain of custody form is signed by the sampler and double zip locked and taped to the inside lid of the cooler The cooler is custody taped on two corners and shipped if laboratory analyses are to be performed at the MDH The sampler and the laboratory keep
17. Date 19 Nov 2007 Calibration Graph and Statistics T 20 0 1171872007 23832 PM D 2000 11 19 2007 24110PM 38 11 19 2007 24247 PME joo 11 18 2007 24425PMp Lj 5 011 11 19 2007 5 05 1119 2007 2 54 08 PM 1 189 2007 25546PMP 5 Conc 3 53e 4 Area 2 0 305 Area 0 0631 Correlation Coefficient 1 1 00000 Weighting 1 x ET ANI pe 10 107 04 3 D Page 21 2 Dec 2010 sat 2630 3 y 1d rd ad md Ped Method Detection Limit for Nitrogen using a 0 10 mg N L standard MDL 0 008 mg N L Standard Deviation s 0 0026 mg N L Mean x 0 106 mg N L Known Value 0 10 mg N L File Name OM 11 19 2007 02 35 50PM OMN Acq Date 19 Nov 2007 MA 0436 yu o o a N a N N 2m Ls Siin 206 mg l 208 mgA 204 Vots 0 064 2337 Timo s 12883 Precision Data for Nitrogen using a 2 0 mg N L standard RSD 0 85 Standard Deviation s 0 0174 mg N L Mean x 1 05 mg N L Known Value 2 00 mg N L File Name OM 11 20 2007 07 25 01AM OMN Acq Date 20 Nov 2007 10 107 04 3 D P ge22 2 Dec 2010 sat An 387 200 R puer 3 138 Vols amn i m 2268
18. Effective Date Date of last signature Page 12 of 67 http fyi health state mn us phl environmental index html Material Safety Data Sheet MSDS Written information provided by vendors concerning a chemical s toxicity health hazards physical properties fire hazard and reactivity including storage spill and handling precautions Matrix The predominant material of the sample to be analyzed Matrices include but are not limited to air drinking water non potable water sewage sludge solids and chemical materials Matrix Spike MS An aliquot of a field sample to which known quantities of the target analytes are added in the laboratory prior to sample preparation and analysis The spiking solution for the MS should be prepared from the same source as the calibration standards The MS is prepared and analyzed exactly like a sample The background concentrations of the analytes in the sample matrix must be determined in an unspiked aliquot of sample and subtracted from the MS concentrations The purpose of the MS is to determine whether the sample matrix contributes bias to the analytical results MS is the same as Laboratory Fortified Matrix LFM Matrix Spike Duplicate MSD A second aliquot of sample to which known quantities of the target analytes are added in the laboratory prior to sample preparation and analysis The MSD is treated exactly the same as the MS The percent recoveries for the target analytes are a measure
19. Enter Collection Date if none enter Postmarked Date The system will use this date to calculate holding time for the sample l 8 Use the mouse to move the cursor to the AN field on the right side of the screen under the Analysis Data section If a List was entered there will already be some analysis codes here Ofherwise manually enter the appropriate analysis codes as shown on the lab request form e 9 Next to the AN field is the Priority field Pri If the lab sheet requests Priority 1 Analysis for the sample change the 3 to a 1 in this field for each analysis code entered This will automatically add a surcharge for the faster service Minnesota Department of Health l Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 9 of 57 10 There are additional fields that are also sometimes used e Receiving Desk Comments field can be used to enter additional information about the sample s Comments written on the lab sheets will also be entered by the clerical unit e Field Blank and Trip Blank fields are used to enter the sample numbers for field trip blanks if they accompanied the samples These are most often used for organic samples from the PCA The data sheet will list the field trip blanks and indicate which samples they are associated with Trip blanks are filled with specially prepared water at MDH and are
20. Minnesota Statutes 43A 38 lists the required code of conduct for all state employees This statute defines policies that relate to gifts and favors use of confidential information use of state property and declared or potential conflicts of interest The full text of the Minnesota Statute is available online at http www revisor leg state mn us stats 43A 38 html Data Practices Policies Minnesota Statutes Chapter 13 Government Data Practices describe the regulations that govern the collection storage maintenance dissemination and access to government data in government entities They presume that government data are public and are accessible to the public for both inspection and copying unless there is federal law state statute or a temporary classification of data that provides that certain data are not public The full text of the Minnesota Statutes Chapter 13 and other MDH policies regarding data practices are online at http fyi health state mn us datapractices index html Computer Security Policy see Section 6 0 of this manual Corrective Action Policy see Section 15 0 of this manual SECTION 5 0 PERSONNEL A Positions and Responsibilities Public Health Laboratory Division Director sets policies for the operation and management of the Public Health Laboratory Division Environmental Laboratory Management Team authorizes training and development for Minnesota Department of Health Quality Assurance Man
21. Non Community Public Water Supply 3 Source Water Protection EH PWS IDENTIFICATION NUMBERS AND PROGRAM CODES All EH PWS samples are assigned a 7 digit Public Water Supply Identification Number PWS ID COMMUNITY PROGRAMS PWS ID numbers begin with 1 Program Codes used for Community samples are HA HB HC amp HY CORROSION CONTROL PROGRAM PWS ID numbers can begin with 1 or 5 even though this is aCommunity sub unit The only Program Code used is HZ NON COMMUNITY PROGRAMS PWS ID numbers begin with 5 The Program Codes used for Non community samples are HD HU HW and HY We rarely receive samples from this unit The Program Code is IB and they do not use PWS ID numbers because they are not public water supply samples EH PWS Unit Program Codes HA Community Water Supplies Bacteriology HB Community Water Supplies Fluoride HC Community Water Supplies Sanitarian Managed HD Non Community Licensed Transient HU Non Community Non Licensed Transient HW Non Community Non Transient HY SDWA Lead Copper Community and Non ee HZ SDWA Corrosion Control Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 32 of 57 COMMUNITY SYSTEMS These public systems usually serve a variety of clients i e one system may serve homes schools and businesses However some s
22. Note 10 The 100 cm back pressure loop is 0 5 mm 0 022 in i d tubing When changing the in line manifold over to run for non digested Ortho Phosphate you can remove the debubbler from port 6 of the injection valve to speed up the time to valve time 10 115 01 3 E Post MUR Page 25 3 December 2010 sat Calibration Data for Ortho Phosphate 05016 E i Bi ME 8 0 4089 500 0 ug 000 g l E 2 Z E 3 8 2509ugiL 2500 9 o 3 H 3 3 E w 3 TE j g g 25 00ug fL 25 09 ug l 3 4 i SIR IIN ees a AS u SI Le e ped A vat N 12758 File Name 12 3 cal support omn Acq Date 3 Dec 2010 Calibration Graph and Statistics 12 3 2010 12 3 2010 Area 0 04740 Conc 0 05556 Conc 21 10 Area 1 173 Correlation Coefficient r 1 00000 Weighting 1 x stones gga EET 10 115 01 3 E Post MUR Page 26 3 December 2010 sat AAS E 0 1517 E ne 2 5271 win OU NEN ge obi ai P 914 258 va a P oe inet aen II WM LM 3 ES N Ny DVB d p dem MAL M Were cee h H qe y pi 05 Time s 1885 0 Method Detection Limit for Ortho Phosphate using a 5 ug P L standard MDL 0 776 ug P L Standard Deviation s 0 30 ug P L Mean m 5 29 ug P L Known Value 5 0 pg P L File Name 12 3 mdl omn Acq Date 3 Dec 2010 0153 8 B 8 3 8 3 g g 251 250 25 250 8 ui 5i 2508 2504 2 1 i ms Tim
23. a inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc 1 9 3 External ver ification of lal of laboratory performance Proficiency Test PT samples are analyzed as required for Federal certification If the results are not within acceptance criteria corrective action is taken and an Unacceptable Data for Performance Evaluation Samples form is filled out by the analyst describing the probable error and any corrective action taken The Unacceptable Data form is given to the Unit Supervisor and Laboratory Quality Assurance Officer 9 4 The MDL study is repeated when changes in instrumentation or instrument response occur A minimum of 7 replicate Laboratory Fortified Blanks LFB or 7 Report Level Verification CRL checks are spiked at a value 1 to 5 times the estimated detection limit and ideally analyzed over a period of at least 3 days If necessary the study may be conducted over a shorter period of time The MDL is determined using the procedure in 40 CFR Part 136 Appendix B See Section 16 3 MDL s must be low enough for regulatory client purposes otherwise remedial action is taken and the process is repeated 9 5 Dissolved Analysis The filtration blank results must be below the Report Level If the filter blank is above the Report Level consult with a lead worker or supervisor to determine if the filter blank result should be subtracted from the sample results or if other actio
24. covering the range of sample results and within the Linear Calibration Range LCR of the analyte The curve used must be 2 order polynomial and not forced through zero Acceptable correlation coefficient for the calibration curve is 0 9990 or greater The concentration of the calibration standards must be Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 13 of 31 https inside mn gov sites MDH bureaus hpb phid env inorganics Gen Chem SOPs gen26 doc 10 of the true value and 20 of the true value for the lowest standard This corresponds to the percent residual calculation The Calibration Statistics display on the analysis report summarizes in algebraic form what is seen graphically The first equation shows the plotted calibration equation in the form of Area f Conc where the peak area is a function of Conc or determined concentration of the analyte The second equation is the same calibration equation but solved for concentration It is in the form CONC f Area This is the equation that is used to determine the concentration of unknowns The third statistic is the value of r the correlation coefficient for the calibration 9 2 2 External Verification of Calibration Analyze a second source calibration verification SCV from the external source immediately after cal
25. diazonium ion is coupled with N 1 naphthyl ethylenediamine dihydrochloride The resulting pink dye absorbs at 540 nm and is proportional to total nitrogen l Interferences l Chloride is a suspected interference Seawater when spiked at 5 mg N L as ammonia gave lt 5 recovery i Special Apparatus Please see Parts and Price list for Ordering Information 1 Lachat Sample Preparation Module A30X11 X 1 for 110V x 2 for 220V with UV 254 lamp 2 PVC PUMP TUBES MUST BE USED FOR THIS METHOD Written and copyrighted O by S Tucker on 12 November 2007 by Lachat Instruments 5600 Lindburgh Drive Loveland CO 80539 USA Phone 970 663 1377 FAX 970 962 6710 This document is the property of Lachat Instruments Unauthorized copying of this document is prohibited CONTENTS 1 SCOPE AND APPLICATION sonia ie vnd 1 2 SUMMARY OF METHOD DN EE EE IA 1 A A o tue ies M E nd name 2 a A ERREUR ed NER UR aisi 3 ESI UID NN RU E at aera Rca a AE 3 6 EQUIPMENT AND SUPPLIES MU DL O CEDE LE due RED 3 7 REAGENTS AND STANDARDS occccssscsssesscsccsvsesceccnssescecccsssecessnstsscessessnsesssnrensseesessesssssonssessas4 TAG PREPARATION OE REAGENT Si ia 4 72 PREPARATION OF STANDARDS tate 8 SAMPLE COLLECTION PRESERVATION AND STORAGE cda aed ed 8 9 QUALITY CONTROL ORC ESPERE NC eee 8 10 CALIBRATION AND STANDARDIZATION acu Unt des 11 11 PROCEDURE taa TET 12
26. needed 2 Youcan normally don t need to select and edit the optimization procedures by clicking the edit list button at the left hand side of the window and choose the way and procedures to run for tuning But for the beginning will just run the Smart tune daily file or Smart tune full UMD file 3 On the right hand side of the window select the right number of position of the sampler at which you put your tuning solution or select the choice of Use manual sampling without autosampler no need to worry about right setting of the position of the tuning solution in auto sampler a Using auto sampler allowing automatic run of the tuning procedures no need to interfere the system during the process and you can use this time to work on your standard solution and preparation of samples But still need to click and save the results of daily performance check before the system can automatically run the rest of the procedures Some tuning procedures scheduled daily performance check at the beginning and the end be sure to check and save the results of this step since the tuning procedure will not continue until you save the daily check result b Byselecting Use manual sampling without autosampler you don t need to worry about where to put your tunning solution you can put it anywhere but it requires active interaction with the system during the tuning procedure by clicking OKs after each tunin
27. of collection to receipt in the laboratory This record generally includes a unique Chain of Custody identification number the number and types of containers the mode of collection collector time of collection preservation and requested analyses Clean Water Act CWA Federal Water Pollution Control Act The enabling legislation under 33 U S C 1251 et seq Public Law 92 50086 Stat 816 that empowers USEPA to set discharge limitations write discharge permits monitor and bring enforcement action for non compliance Continuing Calibration Blank CCB A blank that is run with each batch of samples and at the end of the analytical run The CCB may indicate contamination carryover baseline drift or other instrument or reagent changes occurring over the course of an analytical run that contributes to the value obtained for the quantity in the analytical procedure Continuing Calibration Verification CCV A standard analyzed with an analysis batch that verifies the previously established calibration curve and confirms accurate analyte quantitation for all samples The concentration of the CCV should be near the mid point of the calibration curve Also known as a Calibration Verification Standard CVS Control Charts Day by day or batch by batch plots of QC data such as precision or accuracy to visually monitor a process or analysis Control limits The limits on a control chart such that when data points fall outside them Min
28. or qualified designee performs internal audits of the laboratory areas at least once per year to verify that the guidance provided in this document and other related documents are being followed Internal audits may be performed at any time to investigate any result or procedure that is out of specification To qualify as a designee to the Quality Assurance Officer for the purpose of conducting an internal audit personnel must be independent of the activity being audited and must demonstrate knowledge of the tasks to be reviewed When performing an audit the Quality Assurance Officer or qualified designee examines the following areas recordkeeping sample handling reporting and archiving quality and tracking of standards and reagents appropriate use of sample containers glassware preparation and storage generation and use of control charts and completeness of training records Inspections of other areas or documents may be necessary to evaluate the root cause of a deviation from procedures The Quality Assurance Officer or qualified designee reviews the SOP prior to the audit to assure written protocols are being followed Checklists for conducting the audit are developed by the Quality Assurance Officer or are obtained from an external source i e other states and The NELAC Institute s quality system checklist Previous audit findings are reviewed prior to an internal audit to assure that corrective actions have been implemented After c
29. www health state mn us divs phl environmental handbook internet envhandbook html The actual analytical procedures used by the laboratory are described in its Standard Operating Procedures SOPs Copies of the analytical procedures are on file in the laboratory s Quality Assurance Office and in the pertinent units of the laboratory The internal website http fyi health state mn us phl environmental index html is used for controlled copy distribution to all staff The reference methods are on file with the laboratory s Quality Assurance Officer SECTION 11 0 EQUIPMENT AND SUPPLIES A Maintenance A current equipment inventory is maintained the inventory is updated as needed and includes itemization of spare parts stored at the laboratory Except where available online the laboratory ensures that copies of instrument manuals are accessible to the analyst either by storing near the instrument or on a bookshelf in the laboratory area Before being placed into service laboratory equipment is calibrated or checked to establish that it meets the required specifications to produce quality data Laboratory equipment is maintained according to the manufacturer s specifications and in such a way that the quality control requirements of the laboratory are met for all analyses performed The laboratory maintains a record in the LIMS of all regularly scheduled preventive maintenance for the equipment In general the laboratory maintains a preventive
30. 1 3 10 30 100 Li 20000 03 1 3 10 30 100 Ni 20000 03 1 3 10 30 100 Pb 20000 03 1 3 10 30 100 13 Sr 20000 0 3 1 3 10 30 100 Ti 20000 0 3 1 3 10 30 100 Zn 20000 0 3 1 3 10 30 100 Table 3 Example of calculation for needed volumes of stock and 2 HNO3 for preparing calibration solutions Target conc Volume ol Stock conc Volume of stock Standards b final b solution needed ul PP solution ml PP gt Std1 40 10 10000 40 std2 100 10 10000 100 Std3 300 10 10000 300 Std4 750 10 10000 750 Std5 1700 10 10000 1700 Std6 5000 10 10000 5000 Table 4 Example of calculation for needed volumes of stock and 2 HNO3 for preparing calibration solutions Standards Target conc nal F Stock conc Volume of stock ppb solution ml ppb solution needed ul Std1 0 3 10 10 300 std2 1 10 100 100 Std3 3 10 100 300 Std4 10 10 100 1000 Std5 30 10 100 3000 Std6 100 10 20000 50 14 b Samples i All samples to analyze metal concentrations are needed to preserve with 296 596 HNO3 Since we are using 2 HNO3 for washing solution and for preparing calibration standards we should be consistently using 2 HNO3 to preserve and dilute samples ii If your original samples have not been preserved with 296 HNO3 i e your solution is not containing 296 HNO3 the concentration of HNO3 in yo
31. 24 hours per day seven days per week The following chemicals have the potential to be highly toxic or hazardous consult applicable MSDS 5 7 1 Hydrochloric Acid 60 EQUIPMENT AND SUPPLIES 6 1 6 2 6 3 6 4 Balance Analytical capable of accurately weighing to the nearest 0 0001 g Glassware All glassware must be borosilicate Volumetric flasks and pipettes are Class A All non disposable glassware must be rinsed with 1 1 Hydrochloric acid HCI followed by three rinses with reagent water prior to use Fixed and adjustable pipettes Flow injection analysis equipment designed to deliver and mix samples and reagents in the required order and ratios Lachat Instrument or equivalent 6 4 1 Autosampler 6 4 2 Multichannel proportioning pump 6 4 3 Reaction unit or manifold Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 5 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc 6 5 6 6 6 7 6 8 B 6 4 4 Colorimetric detector 6 4 4 1 Flow Cell 10 nm 80 uL 6 4 4 2 Interference Filter 660 nm 6 4 5 Omnion software version 3 0 6 4 6 Printer 6 4 7 Lachat Special Apparatus 6 4 7 1 Heating Unit 6 4 7 2 PVC pump tubing must be used for this SOP Disposable 13X100
32. 48 56PM OMN Acq Date 19 Nov 2007 10 107 04 3 D Page 18 2 Dec 2010 sat 48 455 Vols i f H aone i KPSS a E aE 353 Carryover Study Two 5 0 mg N L standards followed by three blanks Carryover Passed File Name OM 11 19 2007 12 48 56PM OMN Acq Date 19 Nov 2007 DIN Blanks Average 0 00191 mg N L SD 0 00083 mg g NIL Calculated DIN Limits Detection Limit 0 0025 mg N L Decision Limit 0 005 mg N L Determination Limit 0 0075 mg N L File Name OM 11 19 2007 12 48 56PM OMN Acq Date 19 Nov 2007 z 10 107 04 3 D Page 19 2 Dec 2010 sat Digestion Efficiency for Nitrogen containing compounds in DI water at 2 5 mg N L Nitrogen Form Mean Result mg N L EDTA A Y ONUS Nicotinic acid iY Nicotinic acid gt D Urea YU ie gt E EDTA 3 P Niet 2 M N NHA pts p TEM i Vols AIL TAL TAL PAL WAG AS IA AG BL HL File Name OM 11 19 2007 12 48 56PM OMN Acq Date 19 Nov 2007 0 0653 10 107 04 3 D Page 20 2 Dec 2010 sat Calibration Data for Total Nitrogen High Range iS CabindB 3 Caid 2 mor E 2A Y lu M iem t EA i Pu 1 803 C Jp aer El E Cid H rs Time e File Name OM_11 19 2007_02 35 SOPM OMN Acq
33. 9 1 2 External Verification of Calibration A second source calibration verification standard SCV from an external source is analyzed The results of the SCV must be within the manufacturer s certified range of the established SCV value otherwise remedial action is taken and the entire Initial Demonstration of Capability is repeated 9 1 3 Method Detection Limit MDL Study A minimum of 7 replicate Laboratory Control Samples BS are spiked at a value 1 to 5 times the estimated detection limit and processed over a period of three days The MDL is determined using the procedure in 40 CFR Part 136 Appendix B MDLs must be low enough for regulatory client purposes otherwise remedial action is taken and the process is repeated Once the IDC has been established for this SOP the Unit Supervisor may waive this requirement for individual analysts if the reference method does not specifically require an MDL study for new analysts Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory Filename gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 12 of 31 https inside mn gov sites MDH bureaus hpb phid env inorganics Gen Chem SOPs gen26 doc E 9 1 4 Initial Precision and Accuracy To establish the ability to generate results with acceptable accuracy and precision analyze 4 replicates of a mid range standard Calcul
34. C 4 000 mg 0 4009 mg t a uy ui E B m w o e j 8 3 3 3 3 i P 3 i o a i E S E El 2 li 0 1090 ma 0 1020 mg L 3 a 3 E 3 8 8 0 Ed q o 05412 M L ll N UN ERA dL 0 01 112 009 me 538 Time s 12723 File Name 12 2 cal support Acq Date 2 Dec 2010 Calibration Graph and Statistics oe thn Det Conc mg L 2 003 995 104 7 1 3999 i ae 0 1994 120800 PMI 1 008944 12 10 05 PMI i 0 08834 0 08881 5 0 3 E i 0 03960 0 08799 bi 0 03931j 13 28 PMI 12 14 37 PM 12 18 45 Pelt 12 2 2018 y ER TUM 12 2 2010 0 001100 i 12 2 2010 F Correlation Coefficient r 1 00000 Weighting 1 x 10 107 04 3 D Page 32 2 Dec 2010 sat 0 5529 7 3 y E E 0 005 0 5516 Hee 45 mg L 8 E g d 3 0006356 ety Et ET P 3 3 E E 0 905360 ng L 0087790 voosees B z 5 5 E pi E 5 0 005192 p E 005287 mg L ALME j 005494 rEg L E ba dinis o 00556 0 005296 gr E 0053 d scagi san 3 0 005115 o 056 jd
35. Checks 1 per batch 1 per batch 1 per batch Duplicates Laboratory Duplicates 1 per batch 1 per batch 1 per batch Matrix Spike Duplicate MSD if conducted 1 per batch 1 per batch 1 per batch Laboratory Control Sample Duplicate LCSD if conducted 1 per batch 1 per batch 1 per batch Table 5 QC Acceptance Criteria for Target Analytes in Surface Water and Porewater Laboratory Duplicates Target Analyte Blanks LCS R MS R RPD Laboratory Appendix 3 UMD Civil Dissolved Oxygen N A N A N A N A Engineering Appendix D ae UMD Civil Conductivity N A N A N A N A Engineering Appendix D UMD Civil pH N A N A N A N A Ehgineering Appendix D UMD Civil Temperature N A N A N A N A Engineering Appendix D Ferrous Iron lt RL 85 115 85 115 25 UMD Civil Appendix D Engineering Sulfate lt RL 90 110 90 110 25 UMD Civil Appendix p Engineering Chloride lt RL 90 110 90 110 25 UMD Civil Appendix D Engineering Bromide lt RL 85 115 85 115 25 UMD Civil Appendix D Engineering Fluoride lt RL 85 115 85 115 25 UMD Civil Appendix D Engineering Sulfide lt RL 85 115 85 115 25 UMD Civil Appendix D Engineering Sulfide lt RL 85 115 85 115 25 UMD Civil Appendix D Engineering Phosphate lt RL 85 115 85 115 25 MDH Appendix C Nitrogen lt RL 85 115 85 115 25 MDH Appendix C Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Sec
36. Civil Court The collector or submitter has determined that there was no criminal intent or that it cannot be proven Analysis code 990 should be assigned in addition to the requested AN codes Criminal This is for custody samples that may go to Criminal Court The collector or submitter has determined that there may have been criminal intent Analysis code 991 should be assigned in addition to the requested AN codes C of C SAMPLE PROCESSING PROCEDURE Sometimes C of C samples are sent in via courier in sealed containers Check the seal to see if it is intact or not make note of the status on the C of C form If the seal is intact make a note of who cuts it Sample Receiving personnel Unit Supervisors and designated Management staff are authorized to handle custody samples 1 Record the sample temperature using the IR thermometer in sample receiving You can add a comment to the form such as samples on ice or samples brought in immediately after collection if the statement applies to the samples Minnesota Department of Health l Sample Receiving Procedure Manual Public Health Laboratory Division l Revision Environmental Laboratory Effective Date Date of last signature Page 19 of 57 2 Follow basic sample processing procedures to check the Program Code collection date time sample data sheet identification match and analysis code bottle type match Resolve any discrepancies while the collector is still in Sample Receivin
37. Documents 5 Defining Method files Consult EIAN6000 Software Guide P47 62 a A method file has to be pre defined before any sample can be analyzed A sample file should be defined based on the target elements of your samples There are defined quantitative method files such as quantitative analysis Johnson LowConc mth stored in the computer which include analytes of of Ag Al B Ba Bi Ca Cd Co Cr Cu Fe K Li Mg Mn Mo Na Ni PB Sr Ti Zn use quantitative analysis Johnson LowConc mth for low concentration 0 3ppb to 100 ppb and quantitative analysis Johnson for high concentration 40ppb 5000bbp analysis Switch to Method window by clicking Method tab i Time Tab 1 Make sure your target elements are included it the list of the analytes also of course they should be included in your standard solution 2 The factors of Sweeping reading time Reading Replicating and Replicate are changeable the selection of 40 1 and 3 respectively for the three parameters are reasonable and working well in past measurement Change of these selections affect the volume of the sample needed for the measurement z vi Processing Tab 1 Define how the instrument should detect and process the elements in the samples The selection in the previous method files worked well They are changeable as needed Equation Tab 1 List the same element you selected in the Time tab Here you
38. Group Revision Date 2 December 2010 LACHAT INSTRUMENTS 5600 LINDBURGH DRIVE LOVELAND CO 80539 USA LACHAT Lota INSTRUMENTS A Hach Company Brand QuikChem Method 10 107 04 3 D Total Nitrogen In line Persulfate Digestion Imidazole Buffer Method Method also includes Manifold Alterations to Analyze Nitrate Nitrite see j section 17 5 0 05 to 5 0 mg N L 0 2 to 20 0 mg N L Principle Nitrogen compounds are oxidized in line to nitrate using alkaline persulfate UV digestion Oxidation of nitrogen containing compounds to nitrate is achieved at 105 C with additional energy supplied by exposure to UV light The digestion occurs prior to the injection valve Results for wastewater influent may be up to 3096 low when compared with a rigorous TKN digestion because of sediment in the sample test tube If effluent samples are preserved and filtered in line digestion results will match the manual off line digestion If samples are not filtered in line results will be 1 15 low compared with off line digestion Surface water samples may not require altranon but this should be verified with a sample containing high levels of solids After digestion nitrate is quantitatively reduced to nitrite by passage of the sample through a copperized cadmium column The nitrite reduced nitrate plus original nitrite is then determined by diazotization with sulfanilamide under acidic conditions to form a diazonium ion The
39. MDH Minnesota Department of Health NELAC National Environmental Laboratory Accreditation Conference NELAP National Environmental Laboratory Accreditation Program OSHA Occupation Safety and Health Administration PHLD Public Health Laboratory Division RCRA Resource Conservation and Recovery Act SDWA Safe Drinking Water Act USEPA United States Environmental Protection Agency SECTION 2 0 DEFINITIONS OF QC TERMS The QC definitions and QC terms listed herein are standardized for use in this laboratory Employees in this laboratory recognize that in some cases a particular USEPA approved method and in turn a particular Standard Operating Procedure SOP may use different QC definitions and QC terms In those situations the QC in those particular SOPs supersedes the QC definitions and terms in this Quality Assurance Manual Acceptance Limits range within which specified measurement results must fall to be compliant Acceptance limits may be mandatory requiring corrective action if exceeded or advisory requiring that noncompliant data be flagged Accuracy The degree of agreement between an observed value and an accepted reference value Accuracy is a data quality indicator that includes a combination of random error precision and systematic error bias components which are due to sampling and analytical operations Refer to the Data Quality Section of Standard Methods for a more detailed explanation Aliquot A representat
40. MDL standard you used was prepared like a sample digested extracted etc describe that otherwise enter N A All values must be recorded in the same units It is recommended that a starting point for the MDL standard be either 1 a standard prepared that is at or near the report level RL or 2 a standard at a concentration between 1 and 5 times the anticipated MDL A minimum of seven replicates is required MDL data can be generated from a single analytical run However to generate the most variability the data should be generated o over a period of at least 3 days but no more than 2 months If target analytes are present in the reagent water used to prepare the MDL standards that can significantly affect the recovery of the analyte seven blanks are analyzed and the average of the seven is calculated This amount is then subtracted from the found results for each replicate The MDL is then calculated from these adjusted concentrations Prior approval from the supervisor and QA Officer is necessary All the results obtained from the replicates should be used in the MDL calculation unless the analyst knows for certain that a result is not valid Enter the report level for the analyte and the True Value TV of the MDL standard that you used to generate the data Enter the results for each replicate record raw numbers without rounding attend to significant figures Calculate the recovery for each replicate Minnesota Departm
41. Period 45 seconds Time to Valve 26 seconds Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 28 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc we e Ken be EA a A A PH Eo Date 13 29 75 renner Inorganic Unit Supervisor Approved By Approved By fol Ma Die 2 8 2013 Paul Moyer Environmental Lab Section Manager Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 29 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc o Appendix I NPDES Equivalent Methods Do NOT Require Letter From USEPA Lachat Instruments has received many questions regarding USEPA Equivalent methods for NPDES reporting Many customers have requested letters from the EPA stating these methods acceptance Lachat would like to stress that the USEPA will not be issuing letters for methods that fall within the flexibility allowed at 40 CFR Part 136 6 of the EPA s Method Update Rule MUR March 2007 and that these meth
42. Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 11 of 57 EDITING SAMPLE ENTRY INFORMATION Sample entry information may need to be edited due to initial entry error or because the collector laboratory or EH DWP employee have requested changes to the analysis codes program code etc If you are making actual changes to the sample not just correcting errors be sure and add a receiving comment to the sample so there will be a record of all changes made Using the Editing Init Entry Screen E When using this screen you may edit up to 20 sample numbers at one time You may change the Program Code Receiving Comments Analysis AN codes Collection Date Time Priority and Priority Memo Date 1 From the main screen use the mouse to select eDiting and pull down to select Init Entry 2 In the two boxes at the top of the screen type in the first and last sample numbers for the samples that need editing Up to 20 samples can be edited together as a group 3 After the numbers are entered the system will pull up the information on the samples The left side of the screen will show all the samples with the program codes The right side of the screen will show the analysis codes priority and priority memo date if any for the sample that is currently selected 4 After making the necessary changes hit the F3 key or click on commit to save To change the Program Code
43. Quality Assurance Manual Filename qao001 Revision 9 Effective Date Date of last signature Page 49 of 67 Equipment maintenance example Appendix 7 Daily maintenance of an ICP MS instrument MDH Date HARDWARE Checklist Ar Tank Pressure psi Reaction Gas Type Pressure psi Cell gas A Reaction Gas Type Pressure psi Cell gas B Chiller Pressure psi Temp C Torch Box Temperature C inspect Cones if necessary z SERE v SIE SHER S ro R la lt SlslEl8s BIO Ss ils 2 Ss 318 als ejo dB a Inspect Sample Introduction System K Neb Flow L min Std mode Lens voltage V Autolens Y Mg Sensitivity cps Std Mode n Sensitivity cps Std Mode U Sensitivity cps Std Mode Kr Sensitivity cps Std mode Pb Sensitivity cps Std mode cor cop EN eT O ETT LL E TES ETT TT e Background ops 837228 __ ux Tt A Tf daily performance results are not acceptable perform Instrument optimization See optimization Worksheet Perkin Elmer Elan DRC tl Daily Maintenance Month M Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 50 of 67 http fyi health state mn us phi environmental index html Y Equipment maintenance example Monthly repairing and maintenance of an ICP MS instrument Piera
44. RANGE LCR The concentration range over which the instrument response is linear MATERIAL SAFETY DATA SHEET MSDS Written information provided by vendors conceming a chemical s toxicity health hazards physical properties fire and reactivity data including storage spill and handling precautions METHOD DETECTION LIMIT MDL The minimum concentration of an analyte that can be identified measured and reported with 99 confidence that the analyte concentration is greater than zero PRACTICAL QUANTITION LIMIT PQL The lower level where measurements become quantitatively useful is called the POL The PQL is defined as PQL 10 s where s the standard deviation of 21 replicates of a standard 2 5 5 times the MDL QUALITY CONTROL SAMPLE QCS A solution of method analytes of known concentrations that is used to spike an aliquot of LRB or sample matrix The QCS is obtained from a source external to the laboratory and different from the source of calibration standards It is used to check laboratory performance with externally prepared test materials STOCK STANDARD SOLUTION SSS A concentrated solution containing one or more method analytes prepared in the laboratory using assayed reference materials or purchased from a reputable commercial source 4 INTERFERENCES 4 4 2 Silicate is not a significant interference when using this method 1000 mg L SiO2 gives a response of approximately 6 ug P L Glassw
45. Sulfuric Acid H2SO4 Stir or swirl to mix Then add 213 g Ammonium Molybdate Solution Reagent 1 and 72 Antimony Potassium Tartrate Solution Reagent 2 Stir to mix Degas with helium Prepare weekly or if blue color or yellow precipitate develops Reagent 4 Ascorbic Acid Reducing Solution By Volume In a 1 L volumetric flask dissolve 70 0 g granular ascorbic acid in about 700 mL DI water Dilute to the mark and mix with a magnetic stirrer Degas this 10 115 01 3 E Post MUR Page 4 3 December 2010 sat solution with helium Add 1 0 g SDS sodium dodecyl sulfate Aldrich catalog no 86 201 0 Mix with a magnetic stirrer Prepare fresh every two days By Weight To a tared 1 L container add 70 0 g granular ascorbic acid and 970 g DI water Mix with a magnetic stirrer until dissolved Degas this solution with helium Add 1 0 g SDS sodium dodecyl sulfate Aldrich catalog no 86 201 0 Mix with a magnetic stirrer Prepare fresh every two days Reagent 5 Sulfuric Acid carrier solution 0 45M By Volume In a 1 L volumetric flask add 30 mL sulfuric acid H2504 in about 600 _ mL DI water Add 9 0 g potassium chloride KCI Dilute to the mark and stir to mix Degas this solution with helium after the solution 1s cool Prepare weekly By Weight To a tared 1 L container add 55 2 g sulfuric acid H2504 into 970 g DI water Add 9 0 g potassium chloride KCl Stir to mix Degas this solution with helium after the solution is cool Pre
46. Time s 7187 Carryover Study Two 20 0 mg N L standards followed by three blanks Carryover Passed _ File Name OM 11 26 2007 09 09 11 AM OMN Acq Date 26 Nov 2007 3 DIN Blanks Average 0 00061 mg N L SD 0 0026 mg N L Calculated DIN Limits Detection Limit 0 0078 mg N L Decision Limit 0 0157 mg N L Determination Limit 0 0235 mg N L i File Name OM_11 20 2007_07 25 01AM OMN Acq Date 20 Nov 2007 10 107 04 3 D Page 23 2 Dec 2010 sat Digestion Efficiency for Nitrogen containing compounds in DI water at 5 0 mg N L Nitrogen Formi dE Urea NPTS Ammonium p toluenesulfonate 953 1304 NH4J2504 de NH4 2504 5 3 8 3 gt i e Nicolinic acid NH4 pts a y RJ 2200 Time sj 1 2e 3 File Name OM_11 26 2007_10 41 56AM OMN Acq Date 26 Nov 2007 10 107 04 3 D Page 24 j 2 Dec 2010 sat Spike recovery of Total Nitrogen in Wastewater Initial total nitrogen concentration of wastewater was 9 35 mg N L Spiking level is 5 0 mg L of each of the nitrogen compounds listed below Spike Recovery le Nitrogen Compound Dd Doc Ue Nitrite Ammonia Ammonium p toluenesulfonate Conclusion Spike recoveries of 92 102 were obtained using this method 5M N03 5M EDTA SM Urea
47. a copy of the bill of lading as proof of custody in shipment Records of custody are maintained by the MPCA within the site files Section B 3 3 Laboratory Custody Laboratory custody procedures are usually described in the laboratory QAM if available The laboratory signs the COC when the samples are received The laboratory verifies the COC is correctly filled out and all samples are accounted for and not broken Any problems that occur upon receipt of the samples will cause the sample clerk at the laboratory to immediately contact the MPCA QA Coordinator The MPCA will decide if the samples are to be run depending on the problem The laboratory logs in the samples into the laboratory LIMS system The system assigns a unique number to each sample The log in numbers are then used to track the sample at the laboratory The laboratory stores the samples in a secure refrigerated area that maintains the samples at 4 2 C The sample holding area is secure from unauthorized personal having access to the samples The samples are removed by an analyst for extraction digestion the extraction digestion performed and any remaining sample placed back in the refrigerator The Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 3 B 4 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 28 of 44 laboratory disposes of the samples except in case of v
48. analysis Shall Denotes a mandatory requirement Shall is synonymous with must Should Denotes a recommended but not required action Spike A known quantity of target analyte s added to a blank or sample aliquot This QC standard is used to determine recovery or for other quality control purposes See MS or LCS Spiking solution A solution containing a known concentration of target analyte s used to fortify a blank or sample for quality control purposes Standard A solution or other material with a known value that is used in the laboratory to perform calibrations or QC checks Standard Curve See calibration curve Standard Reference Material SRM A certified reference material produced by the U S National Institute of Standards and Technology NIST and characterized for absolute content independent of any analytical method Standard Operating Procedure SOP A written document that details the techniques and procedures of an operation analysis and or action and is officially approved as the method for performing certain routine functions The SOP is written to ensure the generation of usable and consistent results Stock Standard A concentrate containing one or more target analytes that is purchased from a commercial source or prepared in the laboratory The stock standard is used to prepare intermediate standards and calibration standards Surrogate A non target analyte added to samples blanks and standards before
49. and the heater outlet is connect to the inlet of tee 2 Tee s 1 and 2 are mounted on the chemistry manifold board The UV 254 lamp inside of the sample prep module has 550 cm of zeus tubing wrapped around the UV lamp with about 50 cm of tubing remaining at each end for connections 650 cm total length The outlet of tee 2 is connected to the UV inlet and the UV outlet is connected to the tubular membrane debubbler Page 27 2 Dec 2010 sat 17 4 DEBUBBLER M pt s and outlet Membrane This debubbler has holes in the bottom and a circular membrane sandwiched between two round pices of tan PEEK Typically it does not require a backpressure loop on the outlet gt When a liquid other than water is passed through this debubbling unit it is very important that DI water be pumped through it for 5 10 minutes followed by pumping air for another 5 10 minutes at the end of each days run This aids in removing salts acids and bases that could reduce the lifetime of the membrane and at least partially dries the hydrophobic membrane material Membranes typically last 1 3 weeks or even longer with fastidious care 5 If the solution passing through the unit is very hot it is not unusual to see water droplets on the outside If bubbles are still entering in the fluid stream but not exiting at the outlet the unit is still properly functioning despite this condensation Membranes are replaced by removal of the Al
50. be capable of meeting such performance Individual laboratory and instrument conditions as well as laboratory technique play a major role in determining method performance The support data serves as a guide of the potential method performance Some labs may not be able to reach this level of performance for various reasons while other labs may exceed it 14 POLLUTION PREVENTION 14 1 142 143 Pollution prevention encompasses any technique that reduces or eliminates the quantity or toxicity of waste at the point of generation Numerous opportunities for pollution prevention exist in laboratory operation The USEPA has established a preferred hierarchy of environmental management techniques that places pollution prevention as the management option of first choice Whenever feasible laboratory personnel should use pollution prevention techniques to address their waste generation When wastes cannot be feasibly reduced at the source the United States Environmental Agency USEPA recommends recycling as the next best option The quantity of chemicals purchased should be based on expected usage during their shelf life and disposal cost of unused material Actual reagent preparation volumes should reflect anticipated usage and reagent stability For information about pollution prevention that may be applicable to laboratories and research institutions consult Less is Better Laboratory Chemical Management for Waste Reduction availab
51. calibration standards but without the analyte l CALIBRATION STANDARD CAL A solution prepared from the primary dilution standard solution or stock standard solutions The CAL solutions are used to calibrate the instrument response with respect to analyte concentration FIELD BLANK FMB An aliquot of reagent water or equivalent neutral reference material treated as a sample in all aspects including exposure to a sample bottle holding time preservatives and all preanalysis treatments The purpose is to determine if the field or sample transporting procedures and environments have contaminated the sample FIELD DUPLICATE FD Two samples taken at the same time and place under identical circumstances which are treated identically throughout field and laboratory procedures Analysis of field duplicates indicates the precision associated with sample collection preservation and storage as well as with laboratory procedures LABORATORY BLANK LRB An aliquot of reagent water or equivalent neutral reference material treated as a sample in all aspects except that it is not taken to the sampling site The purpose is to determine if the if analytes or interferences are present in the laboratory environment the reagents or the apparatus LABORATORY CONTROL STANDARD LCS A solution prepared in the laboratory by dissolving a known amount of one or more pure compounds in a known amount of reagent water Its purpose is to assure that
52. connects the washing solution and peristaltic pump is working well 1 Make sure the end of the hose inserted in washing tank is submersed in the solution 2 Besure to pump that pumping washing solution is working well This pump is located at the back of the auto sampler Check the rubber tubes clamped at in the pump replace it if you see any damage This pump only operates when the autosampler is used iii Make sure the tank containing waste solution has enough space to receive waste during your sample run empty it as needed Ask Bryan for help iv Both tanks containing washing solution and waste are sitting on the floor underneath the auto sampler 3 Turning on Plasma a Submerse sampling tip in Milli Q water check it occasionally when system is warming up refill Milli Q as needed Double click to start the ELAN6000 software and enter the service mode using password Elan6000 Options Enter service Mode Click on the Devices Peristaltic pump Connect buttons to connect the system to peristaltic pump i Start the pump with rotating counterclockwise at 24 rpm by clicking the button showing right direction ii Double check the flowing direction and make sure the tubes drain Click on the Instrument button i Ensure the instrument is ready No part of the system model indicates red on the front panel ii Start the plasma ignition sequence by clicking the start plasma button or pressing the gree
53. demonstrate through calibration verification and analysis of the ongoing precision and recovery sample that the analysis system is in control 9 1 4 The laboratory should maintain records to define the quality of data that is generated INITIAL DEMONSTRATION OF PERFORMANCE 9 2 1 Method Detection Limit MDL To establish the ability to detect the analyte the analyst shall determine the MDL per the procedure in 40 CFR 136 Appendix B using the apparatus reagents and standards that will be used in the practice of this method An MDL less than or equal to the MDL in section 1 2 must be achieved prior to the practice of this method 9 22 Initial Precision and Recovery To establish the ability to generate acceptable precision results the operator shall perform 10 replicates of a mid range standard according to the procedure beginning in Section 11 9 2 2 Using the results of the replicates compute the average percent recovery X and the standard deviation s for the analyte Use the following equation for the calculation of the standard deviation Where n Number of samples x concentration in each sample 9 2 2 2 Compare s and x results with the corresponding data in Section 17 If the results meet the acceptance criteria system performance is acceptable and analysis of samples may begin If however s and x do not match the data in Section 17 system performance is unacceptable In this event correct the problem an
54. documents are accessible on the safety page of the PHLD website http fyi health state mn us phl safety index html K Records Retention Paper copies of raw data sample receipt documentation quality assurance documents and final reports are maintained at the laboratory for a minimum of one year and then stored at a records storage facility for a total of ten years from the date of creation The lead copper data germane to the Safe Drinking Water Act are retained for a total of twelve years from the date of creation OSHA reports are kept as required by its program Civil or criminal chain of custody documentation is retained at the laboratory for twelve years from the date of creation Electronic copies of laboratory reports are maintained at the agency Electronic records are backed up nightly by the information technology staff of MDH or the Office of Enterprise Technology the statewide IT personnel as appropriate SECTION 9 0 DATA QUALITY OBJECTIVES Monthly the laboratory management team including the Quality Assurance Officer meets with clients in the MDH Environmental Health Division and the Minnesota Pollution Control Agency to ensure compliance with the particular data quality objectives pertinent to the projects Report limits for each field of testing are in the Environmental Laboratory Handbook http fyi health state mn us phl environmental index html At the request of clients report limits may be modified to meet da
55. employees They also conduct safety and Right to Know training annually for all lab employees Employees are expected to be familiar with the documents posted on the PHLD Safety website http fyi health state mn us phl safety index html These include the Chemical Hygiene Plan the Hazardous Waste Manual Radioactive Waste Management First Report of Injury Form and Emergency Procedures Safety training related to the specific assignments of the employee is provided by the supervisor in consultation with the PHLD Health and Safety Officers The training meets the requirements of OSHA s Hazard Communication Program 29 CFR 1910 1200 In addition to courses required of all division employees supervisors and managers must attend core management training courses offered by the Minnesota Department of Employee Relations DOER Both MDH and DOER publish training bulletins to inform employees of a wide variety of course offerings 2 Radiation Safety Training for selected staff Initial radiation safety training and annual refresher training are required for staff who will work with or in the vicinity of radioactive materials Training for the selected staff covers radiation hazards appropriate precautions and emergency procedures For staff who will handle radioactive materials directly the training also includes special procedures related to their specific laboratory use of radioactive material Minnesota Department of Health Quality Assura
56. field sample The true value is 0 2 mg L 11 3 Prepare a CRL by using the lowest non zero standard 0 01 mg L Pour approximately 5 mL of the 0 05 mg L standard into a 10 mL borosilicate test tube 11 4 Calibration and Sample Analysis 11 4 1 Prepare standards as described in Section 7 11 42 Place calibration standards in descending order in the auto sampler standards tray Select the default Sulfide template from the Sulfide data folder and input the information required by the data system such as concentration replicates and QC scheme Verify peak timing and integration parameters as specified in Section 17 3 Import the sequence ID numbers from Element Database 11 4 3 Pour approximately 5 mL of each type of quality control and sample into a 10 mL borosilicate test tube and place in sample tray Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 20 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc a T 11 4 4 The CCV and CCB must be set up every 10 samples and at the end of each run in the template The CCV is the 0 5 mg L calibration standard The CCB is the same as the calibration blank The CCV and CCB come from the same cup as the equivalent calibration standard Input the information required for the QC sch
57. for a sample type over the current code Add or change the Receiving Comment by clicking on the field and typing Hitting shift F3 will copy the comment from the previous sample Toedit AN codes select the appropriate sample by clicking on the sample number on the left side of the screen to highlight it The analysis codes will appear in the right side box To add an analysis code click on the AN column and arrow down to the last code entered Hit F4 to add a box and type in the analysis Repeat as needed You have the option to add the codes to all sample numbers in the group If this is desired hit yes when asked to do so by the system To delete an analysis code click on the code in the AN column and hit shift F9 or click on the delete record button to remove the code You can only delete codes from one sample at a time Change the Priority on a sample by clicking on this field on the right side of the screen The priority for each analysis code has to be changed separately Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 12 of 57 e Edit the Priority Memo Date in the appropriate field on the right side of the screen This should be the date when the memo requesting the priority status was received This date is used to calculate the appropriate holding time e To edit Collec
58. glasses while using a knife Do not discard a box until you make sure a data sheet has been included with the sample and that it contains all of the necessary information If we receive a set of several boxes from one facility open th m at the same time The data sheets for all of the grouped boxes may be sent in just one box If there is no data sheet see Step 4 for directions CHECKING BOTTLES FOR IDENTIFICATION MAKE SURE THERE IS SOME TYPE OF IDENTIFICATION ON THE BOTTLES such as facility name PWS ID or field number If this information is missing follow the directions below For samples collected by agencies other than MDH EH try to contact the collector directly This includes MPCA MN DOT OSHA etc For unmarked EH samples from a single sampling point Write the PWS ID or facility name on the bottle s for the following types of samples HA Bacteriology samples HB Fluorides HC nitrates sent singly or any EH sample set data sheet received in its own box so we know it is from that facility only Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 36 of 57 For unmarked EH samples from multiple sampling points Occasionally groups of samples will be sent in from one facility with multiple sample points but the sample points or field numbers are not marked on the bottles If the samples wer
59. in the QA office An IDC for each analyst must also be on file for each analysis they perform where an IDC is required Note The effective date of this document is the date of the last signature on this document On the effective date this document becomes an appendix to the Quality Assurance Manual for the Environmental Testing Units of the Public Health Laboratory Division Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 59 of 67 http fyi health state mn us phl environmentalVindex htm Appendix 11 Policy and Procedure for Report Level Verification for the Environmental Testing Units of the Public Health Laboratory Division Minnesota Department of Health This policy and procedure pertains to inorganic and organic chemical analyses it is not applicable to microbiological and radiological analyses The Quality Assurance Officer QAO may waive this requirement when it is not feasible to conduct a Report Level Verification RLV The QAO may also modify the RLV procedure example modifications for a multi analyte analysis or accept other QC procedures in lieu of an RLV The analyst must follow requirements for the performance of a Report Level Verification cited in the reference method or applicable regulatory program for which the data are to be used A project or client may also specify
60. in the laboratory QAM if available and SOPs The basic procedure for the analyses is to calibrate the analytical instruments at five levels One of the levels must be at or below the report level for the individual target analyte The initial curve must have a coefficient of 20 99 or a RSD of 2096 The five point initial calibration curves are verified with an external source calibration standard and then routinely as specified in the MDH Certification Rule or in a specific laboratory s SOP with a calibration verification check standard All calibration standards must have a percent difference 96D of 1596 Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 8 and B 9 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 33 of 44 Section B 8 Inspection Acceptance of Supplies and Consumables A Project staff person inspects all supplies and consumables for integrity and suitability for use Any supply or consumable judged to be of inferior quality or not suitable for the intended use is rejected Sample containers are pre certified as clean by the laboratory All chemicals and solvents used in the laboratory are inspected to verify that they are of the appropriate grade for their intended use All consumables found to be contaminated are removed from use The laboratory has a tracking system that incorporates the date of receipt the date the c
61. kept with the sample vials throughout the collection process Field blanks are filled by the collectors and then are kept with the samples during collection The lab compares the results of the trip field blank with the sample results 11 When all initial entry information has been entered commit the record by hitting F3 or clicking Save yellow disk icon with the mouse The system will then determine if the analysis codes entered have short hold times 12 If there is a short hold time you will be asked if you want to enter collection time If this information is available on the sheet hit yes and it will take you to a Time Entry Screen After entering the collection time s the system will check if samples have passed their hold times If so you will need to fill out the rejection email form to notify the collector client the e samples are past hold time On this screen the important information to enter is PWS or Location and Collector ID or Collector Name Once they receive the email they will have the opportunity to respond whether they want the samples rejected or run anyways 13 After all information entry is completed a prompt screen will appear asking if you want to print labels now Click on the appropriate box Yes or No or press the enter key to default to No It is often easier to print all labels together when you have finished entering a whole batch of samples Minnesota Department of Health Sample Receivin
62. la SM NH4 pts lo e Z SM N03 M x 5M INH4 2504 E 3 E E SM NHASDA to 3 2 5 SM EDTA E SM Nicotinic acid at 5M Nicotinic acid SM Urea 14 4 ma L a FI 5 F3 A 11m m FS is ener E 5M efi o 5M effl E vU so 2 E 20705 T M gt y mj 2128 Time s File Name OM 11 26 2007 02 09 45PM OMN Acq Date 26 Nov 2007 10 107 04 3 D Page 25 2 Dec 2010 sat 17 3 TOTAL NITROGEN MANIFOLD DIAGRAM Semple Prep Module Persulfate 50 cm Borate z Sul NED Orange wiute Imidazole buffer Carrier DI water Manifold Tubing 0 8 mm 0 032 in i d This is 5 2 uL em QC8000 8500 Sample Loop 50 cm Low Range 13 cm High Range 0 5 mm 0 022 in i d Interference Filter 540 nm Apparatus An injection valve a 10 mm path length flow cell and a colorimetric detector module is required The T shows 1200 cm of tubing wrapped around the heater block at the specified temperature 7 135 cm of tubing on a7 cm coil support Note 1 This is a two state valve used to place the cadmium column in line with the manifold nitrate nitrite PA E cadmium column Note 2 Tee s Land 2 are mounted on left side of manifold board Note 3 From sampl
63. listed in the second column 12 Sampling Point This is the site the collector obtained the sample from Examples are Women s bathroom tap Kitchen tap Well 1 Well 2 etc 13 Test Codes the collector will check the requested test codes in the appropriate columns 14 Lab Comments Collectors sometimes write sampling comments in this space We can also use it to write brief comments about problems with the samples EH SAMPLES FROM NON MDH COLLECTORS There are specialized versions of the MDH 1 data sheet that are sent out to systems to collect their own samples The Sheets are color coded and edited to make it easier for them HA Bacteriology form The program code HA and sample type O are preprinted on this form The 327 test code is highlighted and an X is preprinted in column one by the code Other test codes are blacked out Only one sample is collected from each aci per sampling cycle The form and label are pink HB Fluoride form The program code HB is preprinted on the form The 29 test code is highlighted and an X is preprinted in column one by the code Other test codes are blacked out Only one sample is collected from each facility per sampling cycle The form and label are blue HC Nitrate form The program code HC is preprinted and test code 69 is highlighted but there may or may not be a preprinted X Multiple samples may be collected from one facility The form and labels are green
64. m onoc The laboratory report is given a final review by the laboratory project manager then signed and sent to the MPCA Specific procedures used by the laboratory will be found in the QAM if available Section C 2 4 Reports to Management Reports to management will summarize the Project s sampling and analytical activities for the previous time period the findings of the audits any required corrective actions the results of PE studies any data quality problems along with purposed solutions any major changes in personnel and an overall evaluation of the laboratory s quality assurance The report is sent to all individuals identified in Section A 4 Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No D 1 D 2 and D 3 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 38 of 44 Section D Data Validation and Usability Section D 1 Data Reduction Verification and Validation Section D 1 1 Data Reduction In general instrument response for the quantitative analytical procedures described in the laboratory SOPs is converted to concentrations or absolute amounts of analyte by use of a multipoint calibration curve which relates instrument response to the quantity of the analyte introduced to the instrument The analyst reduces the raw data produced by the instrument using equations found in the laboratory SOP or QAM if available Te
65. meets defined standards of quality with a stated level of confidence Quality Assurance Manual QAM A document stating the management policies objectives principles organizational structure and authority responsibilities accountability and implementation of a laboratory or other organization to ensure the quality and the utility of its product to its users Quality Assurance Plan QAP A comprehensive plan detailing the specific quality assurance Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 f Effective Date Date of last signature Page 15 of 67 http fyi health state mn us phl environmental index html required of the Laboratory to adequately fulfill the data requirements of a program Quality Assurance Project Plan QAPP A formal document describing the detailed quality control procedures by which the quality requirements defined for the data and decisions pertaining to a specific project are to be achieved Quality Control QC The routine technical activities that give insight into the precision and accuracy of analysis results Quality Control Sample QCS A standard containing target analytes of known concentrations which is used to verify the initial calibration The QCS is obtained from a source different from the source of the calibration standards or from a different lot if a second source is not available Qua
66. obtain the correct information Make sure the station numbers field numbers sampling points and site ID s on the forms correspond with the information on the samples Compare the collection time on the bottle with the time listed on the data sheet If there is a discrepancy make note of it on the data sheet Compare the analysis codes requested with the bottles submitted See step 6 for more detail on this DETERMINING THAT CORRECT BOTTLES WERE SUBMITTED FOR THE REQUESTED TESTS Check the Analysis codes requested to be sure that all of the correct bottles have been submitted Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 48 of 57 Refer to the bottle type charts to make your determinations If you determine that the wrong bottles have been submitted some substitutions can be made Thiosulfate Bacteriology bottles can be used for fluoride and nitrite but not for nitrate or sulfate Non thiosulfate Bacteriology bottles can be used for fluoride nitrate nitrite and sulfate General bottles can be used for nitrate if sample is 2 days old or less Nutrient bottles can be used for nitrate this is routinely done by the MPCA Free Cyanide and Total Cyanide bottles are interchangeable if there is adequate sample volume Other substitutions may be possible check with the lab when incorrect bottl
67. of accuracy while the Relative Percent Difference RPD between the MS MSD is a measure of precision The MSD is the same as Laboratory Fortified Matrix Duplicate LFMD Maximum Contaminant Level MCL The maximum permissible level of a contaminant in water which is delivered to the free flowing outlet of the ultimate user of a public water system See 40 CFR Part 141 2 Maximum Contaminant Level Goal MCLG The maximum level of a contaminant in drinking water at which no known or anticipated adverse effect on the health of persons would occur and which allows an adequate margin of safety Maximum contaminant level goals are nonenforceable health goals See 40 CFR Part 141 2 May Denotes a permitted but not a required action Method A scientific technique for performing a specific measurement as published by a recognized authority Method Blank MB An aliquot of reagent water or other blank matrix known to be free of interfering amounts of target analytes or other interferences The MB is treated exactly as a sample including exposure to all glassware equipment solvents reagents acids internal standards and surrogates that are used with samples The Method Blank is used to determine if target analytes or other interferences are present in the laboratory environment reagents or Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effecti
68. of last signature Page 38 of 57 SAMPLES SUBMITTED WITHOUT A LAB SHEET Occasionally samples are received without a lab sheet We first try to fill out a sheet in Sample Receiving using information that may be on the mailing carton or bottle To do this you must have at least a PWS or location and be able to determine what type of sample analysis it is supposed to be for If it is unclear what it is for or if there are other problems in filling out a lab sheet email the Community or Non Community groups in Environmental Health 1 Use what ever information may be provided on the bottle or shipping container to look up site information from the LIMS see section on Lab Review Screens _ 2 As you obtain information record it on an MDH Lab sheet The minimum information needed to submit a sample to the laboratory 1s as follows Program Code PWS ID or Facility Name Collection date or postmark information Analysis Code s 3 If you can not figure out enough information to submit the sample contact an EH e representative for assistance Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 39 of 57 LABELING THE SAMPLE CONTAINERS Most bottles we use now are single use disposable bottles For these bottles we can place the whole label 8 the bottles We still use some bottle types that are washed and re
69. on the PEEK body These are the inlet and outlet of the unit If needed 50 or 100 cm of 0 022 i d tubing can be added at the outlet of the debubbler connected to Port 6 of the valve Note 9 One O ring is installed on each of the flares provided with the diffusion cell Then attach the tan fitting and then a union is attached to each of the flared tubing s 17 3 Quik Chem 8000 17 3 1 The timing values listed below are approximate and may need to be optimized using graphical events programming Sample throughput 60 samples hour 60 seconds sample Pump speed 35 Cycle speed 60 Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 27 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc e nariaam 17 3 2 Analyte Data Concentration Units mg L of NH3 N Expected Inject to Peak Start 20 seconds Expected Peak Base Width 49 seconds Chemistry Direct 17 3 3 Calibration Data Level 3 4 5 Hi 7 Concentration mg L N 0 50 0 10 0 05 0 0 Calibration Fit Type 1 Order Polynomial Calibration Rep Handling Average Weighting Method None Force through Zero No 17 3 4 Sampler Timing Min Probe in Wash Period 5 seconds Sample Period 24 seconds 17 3 5 Valve Timing Load Period 15 seconds Inject
70. oxide fume Formaldehyde Cartridge These samples must be sent to a private lab They should be delivered to the metals unit Organics Code 597 Solvents Air This code is assigned to all OSHA Organics samples The di is a partial list of solvents that fall under this code Epichlorohydrin Ethanol Ethyl Benzene Heptanon Isobutyl Alcohol Methylene Chloride Petroleum Distillates Stoddard Solvents Toluene Xylenes Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 57 0f 57 We do not analyze for formaldehyde as a solvent but the Metals unit can run a different type of analysis for it See metals codes on previous page Misc Samples If there are no codes for the wanted tests ex Ozone contact the assistant lab manager to set up subcontracting them to a different laboratory MINNESOTA OSHA SAMPLE PROCESSING PROCEDURE LABELING OSHA SAMPLES Do not remove the samples from their bags the labs will do this Just clip the labels and paperwork to the bag containing the samples The laboratory personnel will deal with labeling themselves MAKE A COPY OF THE DATA SHEET The copy is for the clerical unit Attach the original to the bag labels The Metals Department wants the copy of the sheet to be delivered to them and the original to be sent to the Clerical Unit MISCELLANEOUS SAMPLE
71. pd ie A a Diada ini rs RA o a A A e Sampling Point PATO CottormGT 338 i e pos 0 s ee EEES ENS E Rev 11 07 2008 Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 46 of 67 http fyi health state mn us phl environmental index html Sample analysis request form a k a Chain of Custody form Example of a form used by the Minnesota Pollution Control Agency e PR MDH Stream Lake Lab Sheet AR d Date Time Collected by Project Code __ Rec dby Lab MDH ID Report to Phone Sienature on Chain of Custody block is mandatory See back of this page sumrzmmuanc a 8 o JOE att e e PLE o Xue o ee ten FIELD ID Project Station ID TARE NAME pa ee suae EEE IES EEE IEA ECC 0000 EEN FEA E EE dos om ooo pp Lake Only Fc iN RN 2 Ont El ij dme PH ma poo YAA AA co 0000000 p dB UR EU FILTER VOLUME ercer ESE LAB TEMP C dentis Pruject ID fer rampie colecion examples LAKETRND LAKE LAE gt See Buck te Sebert am Aaa Crop Identified by n Nombor Code YD Fold DagiicamReglicats SE Sampler Blank SS Spbz Semple TE Trip Bbak BB Bottle Blank EB Rrogvat Elmk ENTER THE IA AED QA SALDLES IN SEPARATE COLUIESS Bau E Write the TOTAL NUMBER of each bottle type collected af the t op of each associat
72. phosphorus determinations Glassware should be washed with 1 1 HCl and rinsed with deionized water Commercial detergents should rarely be needed but if they are used use special phosphate free preparations for lab glassware Special Apparatus Please see Parts and Price list for Ordering Information Lachat sample preparation module A30X03 X 1 for 110V X 2 for 220V with UV 254 nm lamp Heater PVC PUMP TUBES MUST BE USED FOR THIS METHOD BS AT ES Glass standard and sample vials must be used for this method A A A AA A SS ee Revised by S Tucker 3 December 2010 Written and copyrighted O by Lynn Egan on 02 May 2002 by Lachat Instruments 5600 Lindburgh Drive Loveland CO 80539 USA Phone 970 663 1377 FAX 970 962 6710 This document is the property of Lachat Instruments Unauthorized copying of this document is prohibited CONTENTS 1 SCOPE AND APPLICATION eeettt CN C aA J SUMMARY OF WIS TIO Di a a a a 1 3 DEFINITIONS ce 1 d IN TEREERENGESmAt ami ds 2 S BABEIYS eciam b pred utn arbeit netten aad aie deb 3 6 EQUIPMENT AND SUPPLIES tia 3 7 REAGENTS AND STANDARD dad dd 4 7 1 PREPARATION OF REAGENTS a ote ance non 4 7 2 PREPARATION OF DIGESTION REAGENTS eene 5 73 PREPARATION OF STANDARDS sida 6 74 PREPARATION OF DIGESTION CHECK STANDARDS e 7 8 SAMPLE COLLECTION PRESERVATION AND STORAGE eene 8 9 QUALITY CONTROL ertt sienten 8 10 CA
73. prior to performing the PT to detect any shifts or trends that may have affected PT results Check the calibration records if applicable to determine if it is time to recalibrate Check to see if there is an action log indicating problems prior to running the PT Check to see if there is any remaining sample and if so re analyze Verify that the QCS associated with the calibration curve used for analyzing the PT was within range Other please explain Operations Data Affected Corrective Action Taken Results of Corrective Action Data Corrected Acceptance Signatures of Corrective Action s Print this form sign and date and route to Analyst Initiator signature amp date Unit Supervisor signature amp date Quality Assurance Officer signature amp date Laboratory Section Manager signature amp date Original Quality Assurance Officer Copy SAQA Records Env Corrective Actions 2008 CAF Minnesota Department of Health Environmental Laboratory Sample Acceptance Policy The Operations Unit of the MDH Environmental Laboratory is responsible for the use and updating of this policy In general the staff attempts to resolve issues before the laboratory must reject a sample When we note a sample does not meet the conditions for acceptance for accurate testing we will contact the responsible party for instructions We define our minimum level of acceptability by the terms required in federal law state laws and re
74. provide Nutrient bottles and VOC vials for routine tests Therefore the bottle order for this site is as follows 12 Two liter General bottles 12 Metals bottles 12 Mercury bottles 12 Nutrient bottles 12 sets of VOC vials 1 set of VOC Trip Blanks MPCA BAYWEST Meth Samples The samples from Baywe st are usually Meth samples The normal numbering procedure is still used The program code for these samples is LG The analysis code should be 484 which is the drug analysis code The distribution of the paperwork is however different The paperwork is one of the three page Chain of Custody forms The pink copy goes to the collector The yellow copy will be the one sent to Clerical The white copy will be sent with the samples upstairs to the Organics Lab They will keep a log book of the forms DRO Samples Baywest will bring in DRO samples for the Reserve Mining Project from time to time Do not change the program code to LG The pH of these samples will have to be checked and recorded on the pH verification sheet A copy of this sheet will go with the samples and another one will go to Bill Scruton The pH will have to be less than 2 so you might have to adjust as needed When entering in the samples a comment must be made for samples that are to be used for Matrix Spikes MS or Duplicate MSD This helps to notify the laboratory personnel that they have to do some spikes Also put an orange dot with MS or MSD on the bottle Deli
75. receiving area until our staff receives the necessary information and authorization from you to proceed The paperwork submitted with the samples does not match the information on the sample container The laboratory receives the samples after the method specified holding time A sample submission form or chain of custody was not provided or the form supplied is incomplete The labels on the bottles do not have a unique identifier that matches a corresponding item on the form We cannot read the sample labels The collector did not use the correct sample containers for the tests requested The samples were not maintained at the proper temperature to prevent deterioration Legal chain of custody samples received with evidence of tampering e g the custody seals are broken If you have questions or comments about this policy or about samples you have submitted to our laboratory please contact our Operations Unit at 651 201 5300 Environmental Laboratory ops010 Sample Acceptance Policy 601 Robert Street N rev 1 revised September 19 2011 St Paul MN 55164 Page 1 of 1 DEPARTMENT OF HEALTH 651 201 5300 DEPARTMENT oF HEALTH Sample Receiving Procedure Manual For the Public Health Laboratory Division Environmental Laboratory 601 Robert Street North P O Box 64899 St Paul Minnesota 55164 0899 Author Reviser Description of Change 10 17 06 4 ten Updated for new alee pov Andrew Mittendorff Laura Fisc
76. sample that the analysis system is in control l l 9 1 4 The laboratory should maintain records to define the quality of data that is generated INITIAL DEMONSTRATION OF PERFORMANCE 92 1 Method Detection Limit MDL To establish the ability to detect the analyte the analyst shall determine the MDL per the procedure in 40 CFR 136 Appendix B using the apparatus reagents and standards that will be used in the practice of this method An MDL less than or equal to the MDL in section 1 2 must be achieved prior to the practice of this method 10 115 01 3 E Post MUR Page 8 3 December 2010 sat 9 3 9 22 Initial Precision and Recovery To establish the ability to generate acceptable precision results the op rator shall perform 10 replicates of a mid range standard according to the procedure beginning in Section 11 i 9 2 2 1 9 2 2 2 Using the results of the replicates compute the average percent recovery X and the standard deviation s for the analyte Use the following equation for the calculation of the standard deviation Where n Number of samples x concentration in each sample Compare s and x results with the corresponding data in Section 17 If the results meet the acceptance criteria system performance is acceptable and analysis of samples may begin If however s and x do not match the data in Section 17 system performance is unacceptable Tn tbis event correct the problem and repeat the t
77. samples were split with another laboratory Examples of sample analysis request forms a k a chain of custody forms are provided in Appendices 4 and 5 pp 45 47 After the sample bottles have been examined and the sample receipt custodian is satisfied the samples have been collected in appropriate containers shipped properly and arrived in acceptable condition the samples are accepted Samples accepted by the sample receipt custodian are logged into the LIMS With samples that require thermal preservation the sample receipt custodian records the temperature of a representative sample on the sample analysis request form The sample receipt custodian assigns sample identification numbers documents these sample identification numbers on the sample analysis request form and attaches the sample identification numbers using LIMS generated labels to the l corresponding sample containers The LIMS automatically evaluates information for received samples to determine if holding times have been exceeded If samples were received past the holding time for the tests to be conducted the LIMS generates a message via electronic mail to the authorized recipient for the project code requested All issues are referred to the Operations Unit for resolution The electronic message requests a reply from the recipient for permission to reject the sample or for permission to analyze the sample and report the associated data with qualifiers For some
78. shall be identified and corrected and the sample reanalyzed l Compute the relative percent difference RPD between two sample results using the following equation D1 D2 RPD Di Da 2 x 100 Where Dl Concentration of analyte in the sample D2 Concentration of analyte in the second duplicate sample l The RPD for duplicates shall meet the current laboratory acceptance criteria If the criteria are not met the analytical system is judged to be out of control and the problem must be immediately identified and corrected and the analytical batch reanalyzed Laboratory blanks Laboratory reagent water blanks are analyzed to demonstrate freedom from contamination l 9 4 1 942 Analyze a laboratory reagent water blank initially with the test in Section 9 2 and with each analytical batch of no more than twenty samples The blank must be subjected to the same procedura steps as a sample If analyte is detected in the blank at a concentration greater than the Minimum Level Section 1 2 analysis of the samples is halted until the source of contamination is eliminated and a blank shows no evidence of contamination All samples must be associated with an uncontaminated method blank before the results may be reported for regulatory compliance purposes Calibration Verification Verify calibration using the procedure described in Section 10 On going Precision and Recovery OPR Wi
79. should be submitted by whoever provides the sample filters The blank filter is used to determine background levels of the target analyte s that might be in or on the filters Blind Sample A sample submitted for analysis to the laboratory with the true value s known only by the submitter It is used to test the laboratory s proficiency in the execution of the measurement process Bottle Blank BB or Container Blank A QC check of sample containers in which a blank matrix reagent water methanol etc is added to selected containers and then processed and analyzed like any other sample A representative number of bottle blanks usually an amount equal to 196 of lots larger than 100 bottles are tested from each lot of sample containers to determine whether container lots are free of target analyte s or interferences that may give positive results that are not from the actual sample s For further details see the Bottle Blank procedures for individual Laboratory Units Calibration The process of quantifying an instrument s response to known values under specified conditions Calibration Blank A zero standard that contains the reagents present in the calibration standards but does not contain the target analyte s It can be used as a zero point standard in a calibration or for background subtraction Calibration Curve The mathematical relationship between the known values such as concentrations of a series of calibration standards a
80. similar conditions The most commonly used estimates of precision are standard deviation S percent relative standard deviation RSD and relative percent difference RPD Preservation Chemical or physical treatment of the sample to retard the chemical and biological changes that occur after the sample was collected from the parent source Procedural Standard Calibration A calibration method in which aqueous calibration standards are prepared and processed e g extracted and or derivatized in exactly the same manner as the samples All steps in the process from addition of sampling preservatives through instrumental analyses are included in the calibration Using procedural standard calibration compensates for any inefficiencies in the processing procedure Proficiency Testing PT A procedure for evaluating an analyst s or laboratory s performance relative to a given set of criteria through the analysis of unknown samples provided by an external source Proficiency Test Sample A sample obtained from an approved provider to evaluate the ability ofthe laboratory to produce an analytical test result meeting the definition of acceptable performance The concentration of the analyte s in the sample is unknown to the laboratory at the time of analysis Quality Assurance QA An integrated system of activities involving planning quality control quality assessment reporting and quality improvement to ensure that a product or service
81. such as analysis of duplicates MS MSD or LCS LCSD It is calculated with the formula below Ici Ca AL x 2 2 RPD 100 Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 16 of 67 http fyi health state mn us phl environmental index html where l C1 Measured concentration of the first sample aliquot C2 Measured concentration of the second sample aliquot OR more simply Difference between duplicates RPD x100 Mean of duplicates Relative Standard Deviation RSD See percent relative standard deviation Replicate Two or more aliquots of a sample analyzed independently and used to determine precision In some analytical methods the reported value is an average of all of the replicate analyses Report Level RL The lowest concentration of a target analyte that can be reliably measured within specified limits of precision and accuracy during routine laboratory operating conditions RL is also known as reporting level report limit reporting limit and quantitation level Report Level Verification RLV A procedure that determines whether the established report level is valid for a target analyte within an analysis and or analytical run This procedure is performed by the analysis of a standard at or below the report level For further details see the Po
82. sulfate diffusion and reaction in sediment by December 15 2013 These reports will be distributed to the appropriate managers at the MPCA The MPCA Project Team also updates management about project progress on a routine basis Section A 7 Quality Assurance Objectives and Criteria Section A 7 1 Overview Quality assurance objectives are developed for sampling in the sediment incubation microcosms chain of custody laboratory analysis and reporting see detailed procedures in Section B 2 and B 3 Meeting these objectives will provide the MPCA with defensible information to be in the project The work order coordinator or graduate researcher will be responsible for microcosm sampling and chain of custody until the laboratory accepts samples Specific procedures to be used for sampling quality control audits preventive maintenance and corrective actions are described in other sections of this document The purpose of this section is to define quality assurance goals for precision accuracy and completeness Establishing these goals allows the State to judge the adequacy of the results and whether corrective actions are necessary Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 7 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 17 of 44 Laboratory reports include the date of sampling the date of analysis the signed Chain of Custody for
83. sulfur d Press the reset button on the sulfur coulometer e Wait 10 minutes or until the ug S has changed less than 0 5 in 1 minute and record the ug S in the Sulfur_Coulometry_Template as outlined in the Data Analysis section 8 Standard runs Precision and evaluation of the instrument set up is determined by running sodium sulfate standard Na2S04 22 596 S or sulfanilamide standard 18 6 96 S Accept results that are 5 0 of the expected S value Weigh 3 7 mg of sodium sulfate and cover completely with vanadium pentoxide Standards should be prepared in the same manner samples are prepared 9 Copper Reduction Method a disconnect the Teflon tubing from the combustion tube outlet fitting b furnaces should be at 5002C c turn off the oxygen flow d fill the scrubber tube with 2 5 ml MeOH e Insert a piece of Teflon tubing through the top piece of the scrubber extending to the bottom of the scrubber f Disconnect the Teflon tubing from both the breech block inlet and the nitrogen gas exit connection g Use or 1 8 unions and 1 8 od Teflon tubing to complete the following connections h Connect the nitrogen gas line to the top of the scrubber i Connect the exit of the methanol scrubber to the combustion tube outlet fitting j Connect the breech block inlet to a container filled with water k Set the nitrogen flow to 100 150 ml min on the instrument regulator 7 10 psi on the tank regulator and allow the N2
84. the 4 C solution and wash with 1 or 2 squeezes of ice cold Milli Q save the white solid Discard the filtrate from the sidearm flask Rinse the flask used to cool the solution with Milli Q Fill the flask with 450ml of Milli Q and heat to 60 C Add the istas from step 5 and mix into solution Repeat steps 4 and s The white granules on top of ilie filter are crystals Dry crystals in vacuo over anhydrous calcium chloride Rapid drying in a good vacuum and thus at a low temperature is essential as this will minimize the sulfuric acid formation on the crystals The yield is about 80 The effect is illustrated by the blank obtained in the standard procedure 0 178 for the original reagent 0 02 after one re crystallization and 0 01 jmole of N after two re crystallizations Reagent 4 Buffer Solution for Digestion y Volume In a 1 L volumetric flask dissolve 25 0 g disodium tetraborate decahydrate Na2B407 10 H20 and 3 0 g sodium hydroxide NaOH in approximately 7 2 900 mL water Adjust to pH 9 0 with sodium hydroxide or hydrochloric acid Add a magnetic stirbar dissolve and dilute to the mark with DI water Gentle heating may be required for complete dissolution Invert to mix PREPARATION OF STANDARDS To prepare the stock and working standards the following containers will be required By Volume Two 1 L volumetric flasks and seven 250 mL volumetric flasks By Weight Two 1 L containers and seven 250 mL container
85. the MDL study 2 The MDL should be less than the report level 18 If the initial MDL study fails the analyst should consult with the QAO before conducting a second MDL study at a different level If the second trial fails a third may be attempted Indicate on the worksheet if this is the first second or third MDL trial for that analyte 19 A copy of the instrument raw data sheet s used to calculate the MDL must be attached to the worksheet Each raw data sheet must indicate the target analyte MDH LIMS code or analyses name if the LIMS code is not applicable and analyst s name and or initials The MDL worksheet should include all of this information along with the submission date Submit the MDL study packet to the QA Office Note For additional information on MDL see Appendix B to 40 CFR Part 136 Definition and Procedure for the Determination of the Method Detection Limit Revision 1 11 Minnesota Department of Health Public Health Laboratory Division Environmental Laboratory http fyi health state mn us phl environmental index html Quality Assurance Manual Filename qao001 Revision 9 Effective Date Date of last signature Page 56 of 67 Formulas for the MDL Single Analyte Worksheet and included as part of the MDL Single Analyte Worksheet Instructions prepared by Jesse Fillmore March 2007 Sp 4 Recovery Result 1 Mean E aes Recovery Std Dev mty
86. the information obtained during the on site visits to your laboratory and your responses to our draft findings the United States Environmental Protection Agency grants to the Minnesota Department of Health 601 Robert Street North St Paul MN 55164 0899 full certification for the chemistry microbiology and radiochemistry methods and parameters identified in Enclosure A If you have any questions or require clarification concerning this memo please contact Patrick Churilla at 312 353 6175 by FAX at 312 886 6171 or by E mail at churilla patrick epa gov Sincerely Timothy C Henry Acting Director Water Division Enclosure Recycled Recyclable Printed with Vegetable Oil Based inks on 100 Recycled Paper 50 Postconsumer Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 62 of 67 http fyi health state mn us phl environmental index html Minnesota Department of Health Public Health Laboratory Division Environmental Laboratory http fyi health state mn us phl environmental index html Quality Assurance Manual Filename qao001 Revision 9 Effective Date Date of last signature Page 63 of 67 USEPA Certification for Laboratory Analyses for Drinking Water LABORATORY CERTIFICATION SUMMARY Minnesota Department of Health Parameters Method 1 Metals ICP AES 200 7
87. the results produced by the laboratory remain within the acceptable limits for precision and accuracy This should not be confused with a calibrating standard LABORATORY DUPLICATE LD Two aliquots of the same environmental sample treated identically throughout a laboratory analytical procedure Analysis of laboratory duplicates indicates precision associated with laboratory procedures but not with sample collection preservation or storage procedures QUALITY CONTROL CHECK SAMPLE QCS A sample containing analytes of interest at known concentrations true values of analytes The QCS is obtained for a source external to the laboratory or is prepared from standards obtained from a different source than the calibration standards The purpose is to check laboratory performance using test materials that have been prepared independently from the normal preparation process METHOD DETECTION LIMIT MDL The lowest level at which an analyte can be detected with 99 percent confidence that the analyte concentration is greater than zero 10 107 04 3 D Page 2 l 2 Dec 2010 sat 4 INTERFERENCES 4 Chloride is a suspected interference 5 SAFETY 5 1 5 2 5 3 The toxicity or carcinogenicity of each reagent used in this method has not been fully established Each chemical should be regarded as a poteritial health hazard and exposure should be as low as reasonably achievable Cautions are included
88. to flow through the methanol until the copper is completely reduced l Add more methanol as need to the scrubber tube m Water will accumulate in the right side of the combustion tube Blot this away with a Kimwipe 10 Troubleshooting a Low results i leaks ii bad sample wt iii not enough vanadium pentoxide iv portion of evolved SO2 missed didn t close combustion tube promptly V copper oxide consumed vi Reduced copper consumed b High results i bad sample wt ii Takes too long to finish titration iii One of the electrodes flaky Try very delicately touching the electrode wires Clean Up 1 Pour the used cathode and anode solutions into the appropriate waste container Make sure the stir bar does not fall into the waste container this is easily avoided by using a small necked funnel to transfer the anode solution to the waste container 2 Rinse the cell and caps with water 3 Pour methanol into the anode cell compartment Use vacuum to pull the MeOH through the cell frit into the cathode compartment Rinse with large volumes of DI water 4 Keep S coulometry cell in dry storage area a Water left in glass frit will cause cathode solution to discolor during next use It may be helpful to place S coulometry cell empty in a desiccator overnight before the next use 5 Electrodes should be rinsed with DI water and blotted dry before storage Data Analysis 1 Enter your blank ug S reading and time in
89. when they receive the lab report e O Original Routine All scheduled routine samples fall into this category e R Repeat This type should be used for bacteriology repeat samples only e C Confirmation This type should be used for nitrate confirmation samples only e I Investigative This type should be used for all samples collected as part of follow up investigation of positive or MCL violations e X Other 10 Field Number This number is assigned by the collector to a given sample For example if a e collectors initials are A B C they might assign their first sample of the quarter the number ABC 001 11 Location ID there are 2 types of location ID s Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 34 of 57 E Entry point This is used for Nitrate Nitrite and most other samples such as IOC VOC and SOC D Distribution This is used for Bacteriology samples some Fluorides and Radiation samples If there is more than one entry point and or distribution at one facility the collector will assign numbers along with the letter code For example E01 D01 E02 D02 Because the Nitrate Nitrite and Bacteriology samples are collected from different locations they must be listed in separate columns on the data sheets Usually the Entry point is listed in the first column and the Distribution is
90. with the samples in the cooler 2 All volatile organics samples go in this fridge The top two shelves are for 468 VOCs the lower shelves are for 498 VOCs Lab sheet copies go in the basket just opposite the cooler 3 OSHA organics samples go in the locked half size cooler in this room Paperclip the bagged samples labels and original lab sheets together and place in the cooler Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 43 of 57 e LABS MAP SOUTH Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 44 of 57 E PCR l Jean Keith n A EE E 4 i A pr i Steph Jeff EX L Pe ODIO STRESS Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 45 of 57 e LABS MAP NORTH I aan a PD O O Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 46 of 57 e MINNESOTA POLLUTION CONTROL AGENCY MPCA SAMPLES The MPCA collects a gr
91. years Wild Rice Sulfate Standard Sediment Incubation Experiment Ouality Assurance Project Plan Section No B 1 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 21 of 44 Section B Data Generation and Acquisition Section B 1 Experimental Design and Sampling Process Design Field Collection of Sediment Approximately the top 10cm of sediment was collected through the ice using a modified screen shovel Approximately 90 liters of bulk wet mud was collected from each site North Bay in the St Louis River 1 19 13 46 39 1731N 92 14 2168W and the Partridge River 1 18 13 47 31 2705N 92 11 4350W just upstream from Second Creek Fifty liters of water was also collected through the ice prior to disturbing the sediment Replicate 2 5 diameter cores were collected from each site with a piston corer in order to characterize in situ physical and geochemical conditions All mud core and water samples were transported back to UMD and stored at 5 5 C until the initiation of experiments Lab Sample Analysis of Initial In Situ Cores Field collected 2 5 cores were immediately within 24 hours sectioned into 6 depth intervals 0 1 cm 1 2 cm 2 4 cm 4 6 cm 6 10 cm 10 15 cm and replicate cores were composited into 500 mL plastic sample jars Composite 2 or 3 cores sections from each site were immediately within 20 minutes placed into an oxygen free 95 N2 5 96H2 atmosphere after m
92. 1 9 3 2 2 Spike two additional sample aliquots with the spiking solution and analyze these aliquots to determine the concentration after spiking A 9 3 3 Calculate the percent recovery P of the analyte in each aliquot using the following equation p A B 100 BOE Where A Measured concentration of analyte after spiking B measured background concentration of analyte T True concentration of the spike 9 3 4 The percent recovery of the analyte should meet current laboratory acceptance criteria 9 3 4 1 Ifthe results of the spike fail the acceptance criteria and the recovery of the QC standard in the ongoing precision and recovery test of the analytical batch is within the current laboratory acceptance criteria an interference is present In this case the results may not be reported for regulatory compliance purposes and the analyst must assess the potential cause for the interference If the interference is attributable to sampling the site or discharge should be resampled If the interference is attributable to a method deficiency the analyst must modify the method repeat the test required in Section 9 1 2 and repeat the analysis of the sample and the matrix spike 9 3 42 If the results of both the spike and ongoing precision and recovery test fail the acceptance criteria the analytical system is judged to be out of control and the problem shall be identified and corrected and the sample reanalyzed 9 3 5
93. 11 1 SAMPLE PRETREATMENT PROCEDURE eee 12 11 2 CALIBRATION PROCEDURE midst E R a 12 11 3 SYSTEM NOTES ins UR ME RS 12 12 DATA ANALYSIS AND CALCULATIONS cetonas 13 13 METHOD PERFORMANCE P ueete 14 14 POLLUTION PREVENTION cd ida 14 15 WASTE MANAGEMENT eee vA A MM ML LEE 14 16 REFERENCE S ntes ni ts E UN Su EE A Ad atta 14 17 TABLE DIAGRAMS FLOWCHARTS AND VALIDATION DATA eee 6 17 1 DATA SYSTEM PARAMETERS FOR QUIKCHEM 8000 8500 doses 16 17 2 SUPPORT DATA FOR QUIKCHEM 8000 8300 eene 17 17 3 TOTAL NITROGEN MANIFOLD DIAGRAM mE WERE 26 17 4 DEBUBBL ER otitis SS 28 17 5 MEASURING NITRATE NITRITE UTILIZING TN MAMIE OLD nt eii ii 29 QuikChem Method 10 107 04 3 D DETERMINATION OF TOTAL NITROGEN BY IN LINE DIGESTION BY FLOW INJECTION ANALYSIS COLORIMETRY 1 SCOPE AND APPLICATION 1 1 1 2 1 3 1 4 1 5 2205 259 Nitrogen compounds are oxidized in line to nitrate using alkaline persulfate UV digestion Oxidation of nitrogen containing compounds to nitrate is achieved at 105 C with additional energy supplied by exposure to UV light The digestion occurs prior to the injection valve Results for wastewater influent may be up to 3096 low when compared with a rigorous TKN digestion because of sediment in the sample test tube If effluent samples are preserved and filtered in line digestion
94. 22 of 67 http fyi health state mn us phi environmental index html understood the referenced policies and procedures that are pertinent to my analytical assignments I understand that I am expected to comply with the Quality Assurance Manual and the referenced policies and procedures The professional development of staff is a vital component of fiscal planning throughout the department Laboratory management encourages memberships in professional organizations The department maintains membership in the American Water Works Association and the Association of Public Health Laboratories Laboratory staff maintains membership in associations related to their technical disciplines such as the Minnesota Chromatography Forum the American Chemical Society the American Society for Microbiology the American Society for Mass Spectrometry and the American Water Works Association Additional educational opportunities at colleges or universities are encouraged and may be paid in part or in full at the discretion of the unit supervisor and division management Supervisors may recommend attendance based on the applicability of the course to current duties of the applicant or based on the course s applicability to future goals of the division or department In some cases release time from work to attend courses may be permitted in addition to or in lieu of registration payment The PHLD Health and Safety Officers provide safety training to all new PHLD
95. 3 Revision 0 Effective Date Date of last signature Page 7 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc CH3 2NCe6H4NH2 2HC in approximately 800 mL 3 M hydrochloric acid reagent Stir until dissolved Dilute to volume with 3 M hydrochloric acid reagent Prepare fresh monthly Degas if necessary 7 11 Ferric Chloride Reagent In an acid rinsed 500 mL volumetric flask dissolve 6 65 g of ferric chloride hexahydrate FeCls 6H20 in approximately 450 mL 0 20 M hydrochloric acid reagent Stir until dissolved Dilute to volume with 0 20 M hydrochloric acid reagent Prepare fresh monthly Degas if necessary 7 12 Digestion Solution In an acid rinsed 1 L volumetric flask add approximately 700 mL of degassed reagent water then add 90 mL of concentrated phosphoric acid H3PO4 Dilute to volume with degassed reagent water Prepare fresh monthly Degas if necessary 7 13 Alkaline Antioxidant Reagent In an acid rinsed 500 mL volumetric flask add approximately 300 mL of degassed reagent water then add 40 g sodium hydroxide NaOH 17 5 g ascorbic and 33 5 g disodium ethylenediamine tetraacetate dehydrate Na2EDTA 2H50 Stir until dissolved Dilute to volume with degassed reagent water Prepare fresh monthly Degas if necessary 7 14 Zinc Acetate Preservative 2N In an acid rinsed 200 mL flask add approximately 100 mL degasses reagent water then add 88 g zinc
96. 3 The distilled hydrogen sulfide H2S then reacts in acid media and in the presence of ferric chloride with two molecules of N N dimethyl p phenylenediamine to form methylene blue The resulting color is read at 660 nm and is proportional to the concentration of H5S in the sample 3 0 DEFINITIONS 3 1 Definitions that are common to all areas of the laboratory appear in the QA Manual 4 0 INTERFERENCES 4 Method interferences may be caused by contaminants in reagent water solvents reagents glassware and other sample processing apparatus that can lead to discrete artifacts elevated baselines or that may otherwise bias analyte response All reagents and apparatus must be routinely demonstrated to be free from interferences by analyzing a Method Blank BLK with each batch of no more than 20 samples 4 2 Strong reducing agents at levels of several hundred ppm inhibit color formation 4 3 Iodide interferes at levels greater than 2 mg L 4 4 The method is relatively free from interferences because gas dials separates the sulfide from sample matrix 4 5 During sample collection sulfide might be lost by oxidation reaction with air or oxidizing agents in sample such as chlorine 5 0 SAFETY 5 1 The toxicity or carcinogenicity of reagents and chemicals used in this SOP has not been fully established Each chemical should be regarded as a potential health hazard and exposure to these compounds should be as low as reasonably achiev
97. 4 695 696 697 Mercury 200 202 Nutrient 60 64 69 78 VOC Vials 498 462 3 vials for each code Tests not run at MDH Sometimes there are parameters on the list that are not run at MDH but are analyzed by the collectors in the field They are not assigned test codes on the parameter list or by us These analyses are as follows Eh mV Iron II Methane and Sulfide Note that when Iron II is field analyzed our lab must run Iron codes 152 154 This may not be marked on the parameter list Cation Anion Balance Code 996 If this code is on a parameter list do not enter it in the computer Itis a calculation that is done automatically when certain other tests are ordered Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 54 of 57 Anoka Landfill Wetlands Samples These are collected on a monthly basis but Interpoll always faxes the order when needed it is not a standing order done on a specific day The order includes the parameter analysis code list You can recognize the order by the sampling points Cascade Lift Station Sed Basin Splitter Tank Manhole MH 1 AB 2AB 3AB 4AB and MH 1BC 2BC 3BC 4BC This is a total of 12 sites and they will need one set of VOC trip blanks BOD code 96 and TSS code 3 are run on these samples so we givethem 2 liter General bottles We also
98. 612345 4 The same sample will default into the Ending Sample field but you can enter a series of samples together if they have the same program code AN codes and collection date Use the arrow keys to move the cursor and type over the number s you want to change 5 Press Enter Tab key twice to get to Program Received date time will default automatically and type in the two letter Program Code The full name of the program should default into Client Program box at the bottom of the screen e 6 The next field List is optional For most routine samples analysis lists have been created to make entering AN codes easier Initially the list will show the number 0 To use a default list type in the chosen list number for that program and press Enter Tab key The analysis codes from that list will appear in the AN analysis column If the 0 is left in the list amp field and the previous sample had the same program code the previous samples analysis codes will automatically be entered So if you are entering a series of similar samples with the same program code you can use list 0 to repeat the same analysis codes If you don t want to use a list and the sample has the same program code as the one before it you will need to use the mouse to move the cursor to the next field If the program code is different than the previous sample you can just Enter Tab past this field and no analysis codes will be entered 7
99. 750 8500 25000 Fe 10000 40 100 300 750 1700 5000 K 100000 400 1000 3000 7500 17000 50000 Mn 10000 40 100 300 750 1700 5000 Mo 50000 200 500 1500 3750 8500 25000 Ag 10000 40 100 300 750 1700 5000 Al 50000 200 500 1500 3750 8500 25000 B 50000 200 500 1500 3750 8500 25000 Ba 10000 40 100 300 750 1700 5000 Bi 100000 400 1000 3000 7500 17000 50000 Cd 10000 40 100 300 750 1700 5000 Co 10000 40 100 300 750 1700 5000 Cr 50000 200 500 1500 3750 8500 25000 Cu 10000 40 100 300 750 1700 5000 Li 50000 200 500 1500 3750 8500 25000 Ni 50000 200 500 1500 3750 8500 25000 12 Pb 100000 400 1000 3000 7500 17000 50000 Sr 10000 40 100 300 750 1700 5000 Ti 50000 200 500 1500 3750 8500 25000 Zn 10000 40 100 300 750 1700 5000 Table 2 Example of standard concentration for multiple elements Low concentration Target Concentration ppb Siemens orginal Stdi std2 std3 std4 stds std6 Ca 20000 03 1 3 10 30 100 Mg 20000 03 1 3 10 30 100 Na 20000 03 1 3 10 30 100 Fe 20000 03 1 3 10 30 100 K 20000 03 1 3 10 30 100 Mn 20000 03 1 3 10 30 100 Mo 20000 03 1 3 10 30 100 Ag 20000 03 1 3 10 30 100 Al 20000 03 1 3 10 30 100 B 20000 03 1 3 10 30 100 Ba 20000 03 1 3 10 30 100 Bi 20000 03 1 3 10 30 100 Cd 20000 03 1 3 10 30 100 Co 20000 03 1 3 10 30 100 Cr 20000 03 1 3 10 30 100 Cu 20000 03
100. A and summaries of the project activities will be presented at the February 2013 Conference Section B 9 4 Data Rejection Analytical data which does not meet the established QA QC criteria defined in this QAPP is verified and either flagged as estimated or rejected Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 9 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 34 of 44 Section B 9 5 Data Tracking MPCA staff contact the analytical laboratory on a regular basis regarding the status of sample analysis Section B 9 6 Data Storage and Retention For MPCA data storage and retention is dictated by Minnesota statute and department policy Official laboratory records are managed using an inventory of records with a schedule establishing retention periods and disposal requirements Wild Rice Sulfate Standard Sediment Incubation Experiment Ouality Assurance Project Plan Section No C 1 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 35 of 44 Section C Assessment and Oversight Section C 1 Response Actions Section C 1 1 Laboratory Audits Internal audits take place on an annual basis These audits review the quality policies and implementation of the policies at the laboratory The reports of these audits are sent to the laboratory manager and quality assurance officer for revi
101. Compute the relative percent difference RPD between two sample results using the following equation _ Di D E 100 DisDiyl3 Where D1 Concentration of analyte in the sample D2 Concentration of analyte in the second duplicate sample 9 3 6 The RPD for duplicates shall meet the current laboratory acceptance criteria If the criteria are not met the analytical system is judged to be out of control and the problem must be immediately identified and corrected and the analytical batch reanalyzed 9 4 Laboratory blanks Laboratory jeag nt water Banks are analyzed to demonstrate freedom from contamination 10 107 04 3 D Page 10 l 2 Dec 2010 sat 9 5 9 6 9 7 9 8 9 4 1 Analyze a laboratory reagent water blat initially with the test in Section 9 2 and with each analytical batch The blank must be subjected to the same procedural steps as a sample 9 4 2 If analyte is detected in the blank at a concentration greater than MDL Section l 3 10 analysis of the samples is halted until the source of contamination is eliminated and a blank shows no evidence of contamination All samples must be associated with an uncontaminated method blank before the results may be reported for regulatory compliance purposes Calibration Verification Verify calibration using the procedure described in Section 10 On going Precision and Recovery OPR With every analytical batch a midrange standard must be prepared u
102. D 0 n 0 0 0 n 0 D 0 N N N N N N N N N N 3000 3500 Precision data for phosphorus using 250 ppb orthophosphate RSD 1 22 Mean 254 72 ug P L Std Dev 3 11 ug P L known value 7250 ug P L residual 1 89 Data Filename 050102A fdt Acq Date 01 May 2002 Tine 3551 85 Seconds Amp 134443 Volte E ad TEES 20 ed a 5 a E z ta 00 617 4802 ug PA 500 542 8808 ug PSL 0 0 0815 ug PL 0 0 2379 ug P L 0 1 1334 ug PL O 1 0183 ug PL 3 5 PS E 3 Seconde Carryover Carryover passed Data Filename 042502E fdt Acq Date 25 April 2002 10 115 01 3 E Post MUR Page 18 3 December 2010 sat lt a o Recovery of Digestion Check Standards at 500 ppb Time 2453 13 Seconds Amp 193194 Volts 2 2 Ht Ye Sn vz age de GOS va Bn GLOL rar do 00S Vd Bn ese ost do 009 ya Bn Leer ger do 009 id Bn gez Sgr d OBAd 009 Vg Bn azee rer d OHAd 009 Vad nzzLg eet d OA DOS Vd Bn 8186 L9v d OMA 009 ve 8n 828w68t d Avayd DOS ya Sn peso zab d jAueud DOS ua On nezo Ber d jAueud OOS ya 8n voz eb d Aueud 009 Va Bn Loss ese SWLOOS Va Bn 8 eO 86t aANLOOS Ve Sn ZLLZ L86 ANWLOOS Wa 8n ELBE err dNLOOS ya 8n egoe srr dat 00S We 9n plete ler dat DOS Ya Bn pate rar dot OOS Vd Bn LLES ELP ddl oos Seconds 300 Data Filename 050102C fdt Acq Date 01 May 2002 recovery relative to e a y ad
103. Detail and pictures in Manual P5 14 Remove the two skimmer cones special special tool in the door slide out for the first cone and unscrew out for the second one Clean the cones by immersing the tips only in soapy water and sonicating for 30 min Rinse thoroughly with Milli Q water and allow dry Reinstall cleaned dry sampler and skimmer cones Inspect torch and load coil for damage or contamination 1 If torch has dirty spot open the torch box uninstall the torch clean it by immersing it in 296 HNO3 for at least 3 hours If the spot is not washed out put it in 596 HNO3 or allow extra time and rinse it with Milli Q water While a torch is being washing ask Bryan for another one to use 2 Reinstall the cleaned torch make sure to use the black alignment tool to alight the torch according to the directions of the manual There are two steps to alighn the torch consult Manual P5 16 21 for detail This is a very important step the plasma will not turn on if the torch has not been well alighted and installed Slide back the vacuum chamber and main interface to position be sure to hear the click sound for locking cover back the main chamber e Tuning solution Be sure to have unexpired tuning solution and Milli Q water ready and handy when the system is warming up f Checkthe washing solution and waste tank Make sure there is enough washing solution 296 HNO3 in the tank refill as needed Make sure the tubing
104. Effective Date Date of Last Signature Page 8 of 44 Section A 3 Distribution List The listed individuals will receive copies of the approved Quality Assurance Project Plan QAPP and subsequent revisions Nathan Johnson Ph D University of Minnesota Duluth UMD 218 726 6435 Will DeRocher Graduate Researcher University of Minnesota Duluth UMD 218 720 4294 John Pastor Ph D University of Minnesota Duluth UMD 218 724 4061 Shannon Lotthammer MPCA 651 757 2537 Edward Swain Ph D MPCA 651 757 2772 Patricia Engelking MPCA 651 757 2340 William Scruton MPCA 651 757 2710 Paul Moyer Minnesota Department of Health MDH 651 201 5669 Jeff Brenner MDH 651 201 5353 Shane Olund MDH 651 201 5357 Amy Myrbo Ph D University of Minnesota Twin Cities UMN and National Lacustrine Core Facility Limnological Research Center LacCore LRC 612 626 7889 Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 4 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 9 of 44 Section A 4 Project Organization and Responsibility Section A 4 1 UMD Work Order Coordinator Nathan Johnson Ph D The UMD Work Order Coordinator will Review and approve the Quality Assurance Project Plan QAPP including subsequent revisions With guidance from the MPCA Project Manager and Principle Investigator de
105. Excess oxygen will consume the reduced copper prematurely 4 Set up the coulometer a Mode selection thumb wheel position 1 units in display will be ugS b Time Set thumb wheel 10 minutes c Run Latch switch RUN d Counts Time Counts although it is OK to switch during run to see time elapsed e Cell filling Anode large side place a magnetic stir bar in the cell and fill with 50 100 ml of sulfur anode solution insert the cell top platinum anode electrode and dual platinum detector electrode position the electrodes so the anode electrode is closest to the frit The dual platinum detector electrodes should spaced about the width of a credit card apart from one another Cathode small side Fill with 12 20 ml sulfur cathode solution to the same level as the anode solution Place the platinum cathode in the side arm with the platinum submerged in the solution f Place the assembled cell in the coulometer cell holder Note Mesh type electrodes should be oriented parallel to the frit 5 Turning On Coulometer a Turn off the coulometer cell current b Turn on the main power switch c Attach the anode and cathodes to the cell outlet terminals they are color coded d Plug in the detector electrode e Turn on the coulometer cell current f Allow the cell current to titrate the solution to its endpoint 6 PI amps i The anode solution should be a slightly yellow color when the titration reaches its endpoint Note At th
106. G BOTTLES FOR IDENTIFICATION cnonosooesnisnccinesioconccnanincnanoncccanonnonoconcancan ones 35 Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 3 of 57 NUMBERING THE SAMPLE DATA SHEET S scsssccssscssssrsssocsscccsssscssssscssscsessccssssesnsscesssesces 37 SAMPLES SUBMITTED WITHOUT A LAB SHEET C 38 LABELING THE SAMPLE CONTAINERS ii esasesne saspe ska natia eua p ap aues psa a P En Pesos EE RENE P Vn RES 3 9 PRINTING SAMPLE ENTRY LOG AND COMPARING TO DATA SHEETS 40 DELIVERING SAMPLES TO THE LABORATORY MM 41 LABS MAP SOUTH ovio triente irse dali easi sectional ior ilipgDrg ee 43 LABS MAP NORTH seccesteetecesoteriinis 45 MINNESOTA POLLUTION CONTROL AGENCY MPCA SAMPLES 46 MPCA SAMPLE PROCESSING PROCEDURE eres esee eee eene ens tata adn ee these tn ette eene tao 46 MPCA CLOSED LANDFILL PROGRAM eeeeen eene eene tn ennt enses etat aa ihe en ense atn tnan 51 Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 4 of 57 INTRODUCTION TO SAMPLE RECEIVING CLIENTELE The Minnesota Department of Health Environmental Laboratory receives samples from the
107. L of deionized water in a specific information Refer Sample cell to the user manual for orientation I 10 mL 5 Use the dropper to add 0 5 mL Sulfide 2 Reagent to each cell 6 Caporstopper the cell and immediately invert to mix The solution will turn pink initially and then turn blue if sulfide is present Zero 9 ZERO the instrument 10 Wipe the prepared The display will show sample and insert it in the cell holder 0 00 ug L S2 Sulfide Page 2 of 4 10 mL 3 Prepared Sample Use a pipet to add 10 mL of sample to a second sample cell Do not mix the sample more than necessary to prevent sulfide loss ER 05 00 7 Start the instrument timer 4 Use the dropper to add 0 5 mL Sulfide 1 Reagent to each cell Swirl to mix 8 When the timer expires wipe the blank and insert it in the cell holder A five minute reaction time will begin Read 11 READ the results in ug L S2 Sulfide Soluble sulfides Complete the following steps to measure soluble sulfides 1 Centrifuge a sample in completely filled capped tubes 2 Use the supernatant in place of the sample and follow the Methylene Blue Method procedure To estimate insoluble sulfides subtract the soluble sulfide concentration from the total sulfide concentration Interferences Table 394 Interfering substances Interfering substance Interference level Strong reducing substances such as sulfit
108. LIBRATION AND STANDARDIZATION erernernntntnetnennntt tentent tnnt 11 PE PROCEDUR esce ceteri ect dust tutatus ova oth etica aM o a NAME 11 112 CALIBRATION PROCEDURE m 12 o A Lu One po T HR RI MU 12 2 DATA ANALYSIS AND CALCUTA TON iaa amatam im dete 13 i3 METHOD PERFORMANCE tap n 13 a POLLUTION PREVENTION airo s etimepa esum ate ibn ete 14 is WASTE MANAGEMENT di da clas 14 iC REFERENCO reali ca ipud 14 17 TABLE DIAGRAMS FLOWCHARTS AND VALIDATION DATA 15 17 1 DATA SYSTEM PARAMETERS FOR QUIKCHEM 8000 8500 cce 15 17 2 SUPPORT DATA FOR QUIKCHEM 8000 8500 ias 16 173 TOTAL PHOSPHORUS MANIFOLD DIAGRAM 4244 meme 21 17 4 DEBUBBLER esseeeeeeseen eerie nennen cee ene eniin net nnne nieen eee ene nntnne nennen nee 23 QuikChem Method 10 115 01 3 E DETERMINATION OF TOTAL PHOSPHORUS BY FIA COLORIMETRY WITH ON LINE DIGESTION 1 SCOPE AND APPLICATION 1 1 1 2 1 3 This method covers the determination of total phosphorus in drinking ground and surface waters and domestic and industrial wastes Wastewater samples are acid preserved and filtered When this is the case in line digestion results match the manual off line digestion If samples are not filtered in line results will be 1 15 low compared with off line digestion Surface water samples may not require filtration but this should be verified with a sample containing high levels of solids The method of determination is based on r
109. LN samples will also be accompanied by a check which should be directed to the Assistant Lab Manager Laboratory Consult Non Billable Program Code Program code LM is used for testing that is done internally for MDH and as described above we do not bill ourselves Quality Control Code Program code LQ is used for several different types of special samples The Bio Terrorism Chemical Terrorism group uses it for emergency and QC samples they receive It is also used for Proficiency Testing PT samples Environmental Health Codes Most samples from Environmental Health use codes that start with the letter H Some ens programs will use an I program code Department of Transportation Codes The DOT uses codes that start with the letter D Pollution Control Agency Codes The MPCA uses codes that start with P Q R or S depending on the program DATA SHEETS Data Sheets must accompany all samples submitted to the Laboratory A wide variety of Data Sheets are used but they should all include the Program Code Analysis Codes Collection Date Etc Each type of data sheet is described in more detail in the client specific sections of this manual Minnesota Department of Health sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 6 of 57 GENERAL TASKS Tasks to be performed in the morning Check the refrigerator in Sample Receiving a
110. MUST BE USED FOR THIS METHOD Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 26 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc Note 1 650 cm x 0 8 mm i d tubing wrapped on the heater at 30 C Note 2 200 cm x 0 5 mm i d backpressure loop Note 3 The sample line is replaced with a red red pump tube 45 cm x 0 8 mm i d is used to connect the sample line to the mixing tee which merges with phosphoric acid Note 4 1200 cm x 0 8 mm i d wrapped on the 65 C heater The lengths of tubing on the heater inlet and outlet are 53 cm Note 5 The 53 cm lead of tubing from the outlet of the 65 C heater is covered with 52 cm of high temperature sleeving 1 16 i d Lachat Part No 50364 for heat insulation and then connected to the diffusion cell inlet on the bottom half Note 6 Diffusion cell Lachat Part No 50332 is mounted on the manifold board The Donor bottom and Acceptor top streams flow in the same direction Note 7 To the diffusion cell outlet bottom half connect 100 cm x 0 8 mm i d manifold tubing plus a waste line Lachat Part No 50932 Note 8 The Debubbler is mounted on the manifold board near the valve Replacement membranes are part number 85363 To install unit Cut tubing with 2 nuts in half Screw half into each port
111. Minnesota Department of Health s Public Health Laboratory Division PHLD In addition to the Environmental Laboratory Section division management oversees the Environmental Laboratory Accreditation Program the Clinical Laboratory Section and the Newborn Screening Section The Technical Services Unit and Clerical Services Unit are directly supervised by the Assistant Division Director The PHLD organizational chart focusing on the environmental testing units is presented in Appendix 1 p 42 The Environmental Laboratory Section supports public health and environmental protection functions of state government by performing chemical bacteriological and radiological analyses of environmental samples including drinking water surface water waste water sediment air fish soil and hazardous waste The laboratory provides these testing services for programs in the Environmental Health Division at the Minnesota Department of Health for the Minnesota Pollution Control Agency the Minnesota Department of Transportation the Minnesota Department of Labor and Industry and various agencies of local government The MDH Environmental Laboratory Handbook http fyi health state mn us phl environmental index html lists current partners and clients along with established LIMS project codes The laboratory maintains the capability to respond to chemical and radiological emergencies within Minnesota and with limited abilities to analyze clinical specimens
112. Perkin Elmer Elan DRC Il Monthly Repairing and Maintenance Log Serial Number 20130310 age 1 Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 51 of 67 http fyi health state mn us phl environmental index html Appendix 8 Policy and Procedure for Detection Level Study for the Environmental Testing Units of the Public Health Laboratory Division Minnesota Department of Health A Detection Level DL Study must be performed for each method for each environmental matrix for each analyte and for each instrument as part of an Initial Demonstration of Capability IDC and periodically thereafter as described below This requirement pertains to inorganic and organic chemical analyses it is not applicable to microbiological and radiological analyses The Quality Assurance Officer QAO may waive this requirement when it is not feasible to conduct a DL study The analyst must follow requirements for the performance of a DL study cited in the reference method or applicable regulatory program for which the data are to be used A project or client may also specify the type of Detection Level Study If no such requirements exist the analyst shall utilize the DL procedure described in 1 below The analyst with the approval of the QAO and the Supervisor may choose the procedure outlined in 2
113. QO If QC results are within acceptance limits the LIMS will allow reporting of the results without further qualification by the analyst When sample results do not meet the acceptance limits the LIMS highlights the affected results and requires acknowledgment or further action from the analyst before the sample results may be reported Acknowledgment may include re analysis of the samples or ifthe analysis cannot be repeated the results may be flagged with a data qualifier s indicating which acceptance limits were not met The laboratory may issue results either electronically or via printed copy depending on the need of the client When the analyses for all samples on one work order are completed the LIMS generates a final report and puts it into a review queue The unit supervisor or designated analytical staff receives a notice that data are ready for review The electronic Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 37 of 67 http fyi health state mn us phl environmental index html copy of the data is reviewed and approved in the LIMS The review process is used to assure that the sample results are reported without systematic errors that samples are analyzed within holding times that instruments are within calibration and that the QC data are within the acceptance limits or flagged ac
114. QuikChem Method 10 115 01 3 E Total Phosphorous In Line Persulfate Digestion 10 to 500 pg P L Principle The method is based on the digestion of various phosphorous forms and conversion to phosphate by peroxodisulfate with an in line UV digestion Organic phosphorus is converted to orthophosphate by UV catalyzed persulfate digestion Polyphosphates are converted to orthophosphate by sulfuric acid digestion The digestion process occurs prior to the sample valve A portion of the digested sample is then injected and phosphate is determined by FIA Wastewater samples are acid preserved and filtered When this is the case in line digestion results match the manual off line digestion If samples are not filtered in line results will be 1 15 low compared with off line digestion Surface water samples may not require filtration but this should be verified with a sample containing high levels of solids After digestion the orthophosphate ion PO reacts with ammonium molybdate and antimony _ potassium tartrate to form a phosphomolybdate complex This complex is reduced with ascorbic acid to form a blue complex which absorbs light at 880 nm The absorbance is proportional to the concentration of orthophosphate in the sample Interferences 1 Silicate is not a significant interference when using this method 1000 mg L SiO gives a response of approximately 6 ug P L 2 Glassware contamination is a problem in low level
115. REAGENTS 2 Use deionized water 10 megohm for all solutions Degassing with helium M gS oy To prevent bubble formation degas all solutions except the standards with helium Use He at 140kPa 20 Ib in through a helium degassing tube Lachat Part No s0199 Bubble He through the solution for one minute Reagent 1 Imidazole Buffer pH 7 4 By Volume In a 1L volumetric flask add 600 ml of DI water 6 8 g of Imidazole C3H4N2 and 2 ml of concentrated HCI it is recommended that addition of the HCI be carried out in a hood Swirl to dissolve the imidazole and dilute to 1 L with DI water The imidazole buffer was shown to be stable for at least one month Reagent 2 Sulfanilamide Color Reagent By Volume To a 1 L volumetric flask add about 600 mL DI water Then add 100 mL 85 phosphoric acid H3PO4 40 0 g sulfanilamide and 1 0 g N 1 naphthyl ethylenediamine dihydrochloride NED Shake to wet and stir to dissolve for 30 minutes Dilute to the mark with DI water and invert to mix Store in a dark bottle and discard when the solution turns pink By Weight To a tared dark 1 L container add 876 g DI water 170 g 85 phosphoric acid H3PO4 40 0 g sulfanilamide and 1 0 g N 1 naphthyl ethylenediamine dihydrochloride NED Shake until wetted and stir with a stir bar for 30 minutes until dissolved Store in a dark bottle and discard when the solution turns pink Reagent 3 Potassium Persulfate Oxidant N 3 of By Volume I
116. S PRIVATE WELL WATER TESTING The only analysis that we do for private homeowners on a routine basis is the testing of new homeowner drilled wells through the New Well Program These samples should be accompanied by the appropriate paperwork We also test flooded well samples when there has been flooding in a given area of the state In this case we will be notified ahead of time that the Flooded Well Program has been activated and we should expect samples These samples should also be accompanied by the appropriate paperwork All other private well testing must be pre arranged through the Well Management program In most cases the homeowner will be directed to a local or county program for their esie needs Direct any inquiries to Well Management at 651 201 4600 OR Francine Lafayette at 651 201 4592 Section No Appendix C Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 42 of 44 Appendix C MDH Environmental Laboratory Standard Operating Procedures Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan QuikChemn Method 10 107 04 3 D DETERMINATION OF TOTAL NITROGEN IN WATERS BY IN LINE DIGESTION FOLLOWED BY FLOW INJECTION ANALYSIS IMIDAZOLE BUFFER METHOD 0 05 to 5 0 mg N L Low Range 0 2 to 20 0 mg N L High Range Method also includes Manifold Alterations to Analyze Nitrate Nitrite Written by Scott Tucker Applications
117. SOR R p h o o S T Y n m te o9 T ipe N N o N o ki m x q po oR Se X d 3 g 9 2 g 3 2 o N 9 x 9 9 9 8 o o o o a o o 3 o o a T o T o o o o o a f g o8 UH i20 38 ORC ES Som EA D RE D LO 2 8 9 151 430 L 9500 7 499 s 4500 3000 Method Detection Limit using 10 ug P L as orthophosphate MDL 1 ug P L claiming 1 4 ug P L due to carryover Mean 9 69 yg P L Std Dev 0 37 ug P L RSD 3 71 Yoresidual 3 1 Data Filename 042502E fdt Acq Date 25 April 2002 Time 1328 23 s Amp 13442 Yoke m i202 i 2 00 looo va el tsel los 1 Ea vc joo isd nM d amp X d ER 2 b t 8 G 1924 a o o 5 0 o 9 o o D 192 i 3 3 3 J F mf 3 a 5 3 i o Y o N e o N a N o9 E 9 9 0 K T Y M o QN EE D o o o o o s D a T T dE m m a y n Mel 8 9 3 3 8 8 3 a 3 dd Q o a o o o Q o Q a d z e 0 E E 3 E 7 ise m a m ibe Precision data for phosphorus using 100 ppb orthophosphate RSD 132 Mean 7 104 39 ug P L Std Dev 1 38 ug P L Yeresidual 4 4 known value 100 ug P L Data Filename 042502E fdt Acq Date 25 April 2002 10 115 01 3 E Post MUR Page 17 3 December 2010 sat Tee 698 26 Seconds Amp 133152 Voks y v 153 aa 9 j t y 18 J d d d E d d d e E a a a a a a f a L o v o i a D D o o 3 3 3 3 3 3 3 3 3 3 o n o 3 t N a o m r Q 3 o N o r o n N o T o N 9 a 9 T y a M 7 N N r x d r N o y o 0 Q gt n ga LY 0 0 0 0 0 0 0 0 0 N N a N N N a N N N o a o o o o a o Q o
118. Spikes MSs Matrix spikes may be used by a laboratory to determine if there are any effects related to the sample matrix One spike should be spiked prepared and analyzed per batch of up to 20 samples The recoveries of the MS are used to measure accuracy of the analysis The recoveries should be within the ranges listed in Tables 4 5 or 6 Refer to the laboratory s QAM if available or specific analytical method located in the appendix of this QAPP for details of this QC activity Section B 5 1 3 Laboratory Control Sample LCS A laboratory control sample LCS is an aliquot of clean matrix as the environmental samples One LCS is prepared with each batch of up to 20 samples The LCS is spiked with the same target analytes and at the same concentration as the MS The recoveries of the LCS are used to show that the analysis is in control if there is a matrix effect associated with the analysis of the sample matrix in the MS The recoveries should be within the ranges listed in Tables 5 and 6 Refer to Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 5 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 31 of 44 the laboratory s QAM if available or specific analytical method located in the appendix of this QAPP for details of this QC activity Section B 5 1 4 Laboratory Duplicates Laboratory duplicates are used to measure p
119. TIONS OVERVIEW OF SAMPLE ENTRY SCREENS Log in by opening the Sample Entry website than enter your Username and Password This initial screen is also used to change your password Logging in will bring you to a screen with several menu options Operations not used by Sample Receiving are not included in this overview although they may be available onscreen Bold underlined text indicates a principal operation on the main screen Bold text indicates an operation that is accessed through the principal operation Italics text indicates second level menu options Bold Italics text indicates a field on the screen where information is entered by the user Editing Initial entry This is used to edit data that was entered on the4nitial entry screen Up to 20 sample numbers can be edited at one time Default lists This is used to edit the Program Code Analysis Code default lists Ed Labels bottle This is used to change the number of labels that will print for each analysis code Entry Initial Entry This is used to perform initial data entry and to edit Trip Blank Field Blank information Reject Pending List This brings up the list of samples that have been placed in the rejection list Based on responses from clients samples are checked either Run Anyway or Reject Logs Lists Daily Entry Log This is used to print the Sample Entry Logs that we compare to the data sheets before delivering them to clerical AN Analy
120. The laboratory also develops new analytical methods and provides technical training and consultation at the request of its clients The Environmental Laboratory ensures that testing capacity is available to support the public health and environmental protection objectives of the state The MDH Environmental Laboratory Section is organized into 4 units Three of these units viz the Inorganic Chemistry Unit the Organic Chemistry Unit and the Operations Unit comprise the environmental testing units They include the following technical areas General Chemistry Metals Chemistry Organic Chemistry Radiation Chemistry Water Microbiology as well as administrative functions carried out in the Operations Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 19 of 67 http fyi health state mn us phl environmental index html Unit Additional administrative and technical support is provided by the Sample Receiving Unit B Facility Description and Location The Public Health Laboratory Division is located at 601 Robert Street North St Paul Minnesota The laboratories are co located with the Minnesota Department of Agriculture The two departments operate under separate quality systems analytical staff and management The MDA MDH laboratory building measures 176 500 gross square feet three levels are occu
121. This document is made available electronically by the Minnesota Legislative Reference Library as part of an ongoing digital archiving project http www leg state mn us Irl Irl asp Section No A 1 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 1 of 44 Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan November 2013 Minnesota Pollution Control Agency 520 Lafayette Road North St Paul Minnesota 55155 4194 E Minnesota Pollution Control Agency Wild rice Sulfate Standard 3eaument 1ncubation rxperument uuaury Assurance Project Plan tdr qapp1 05 Section No A 1 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 2 of 44 Section A Project Management Elements Section A 1 Approvals Approval Date Tas 12 07 2013 Nathan Johnson Ph D Assistant Professor University of Minnesota Duluth UMD Civil Engineering Work Order Coordinator 218 726 6435 nwjohnso d umn edu L 10 11 2013 John Pastor Ph D Professor University of Minnesota Duluth UMD Biology Department Principle Investigator 218 726 7001 jpastor d umn edu SAR 11 17 2013 Shannon Lotthammer Minnesota Pollution Control Agency Division Manager 651 757 2537 shannon lotthammer state mn us Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan
122. USEPA Certification for Laboratory Analyses for Drinking Water Ux Parameters Method Certification Status 15 Haloacetic Acids 552 2 Fully Certified Bromoacetic Acid Chloroacetic Acid Dibromoacetic Acid Dichloroacetic Acid Trichloroacetic Acid 16 Pesticides 508 1 Fully Certified Aldrin Alachlor Atrazine Butachlor Dieldrin Endrin Heptachlor Heptachlor epox de Hexachlorobenzene Hexachlorocyclypentadiene Lindane Methoxychior Metolachlor Metribuzin Propachlor Simazine Toxaphene Technical chlordane 17 Herbicides 515 4 Fully Certified 2 4 D 2 4 5 TP Dalapon Dinoseb Pentachlorophenol Picloram co 18 Volatile Organic Chemicals 524 2 Fully Certified Benzene Carbon tetrachloride Chlorobenzene Dichloromethane 1 1 Dichloroethene 1 2 Dichloroethane cis 1 2 Dichloroethene Erans 1 2 Dichloroethene 1 2 Dichloropropane Ethylbenzene Styrene Toluene Tetrachloroethylene Trichloroethylene 1 1 1 Trichloroethane 1 1 2 Trichloroethane 1 2 4 Trichlorobenzene vinyl chloride Xylene total Total Trihalomethanes Chlorotorm Bromodichloromethane Dibromochloromethane Bromoform Ro 19 Glyphosate 547 Fully Certified Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 65 o
123. a using the computer Acceptance or control limits should be established using the difference between the measured value of the calibration solution and the true value concentration After the calibration has established it must be verified by the analysis of a suitable quality control sample QCS If measurements exceed 10 of the established QCS value the analysis should be terminated and the instrument recalibrated The new calibration must be verified before continuing analysis Periodic reanalysis of the QCS is recommended as a check standard 11 PROCEDURE 11 14 11 1 2 11 1 3 11 1 4 Prepare a series of standards covering the desired range and a blank by diluting suitable volumes of standard solution suggested range in section 7 3 Calibrate the instrument as described in section 11 2 Prepare standard curve by plotting instrument response against concentration values A calibration curve may be fitted to the calibration solution concentration response data using the computer Acceptance or control limits should be established using the difference between the measured value of the calibration solution and the true value concentration After the calibration has established it must be verified by the analysis of a suitable quality control sample QCS If measurements exceed 10 of the established QCS value the analysis should be terminated and the instrument recalibrated The new calibration must be
124. a before subsampling Milligram quantities of sample were packed into tin capsules and weighed on a microbalance Sample FS 63 Caribou was not stable weight wise The entire sample was placed in a 60 C oven for 3 hours and cooled in a desiccator before subsampling Instrumentation Analysis and Quality Assurance Acetanilide was used as a calibration standard and as a quality assurance sample A MN Lake Sediment sample prepared in duplicate and a QA sample were run at least every tenth sample AII QA samples were within 5 of the known Carbon Nitrogen weight percent for that material Elemental analysis was performed using a Costech 4010 ECS Paraphrasing from Costech literature At the start of an analytical cycle helium carrier gas was switched to a volume of oxygen Samples were dropped sequentially into a combustion reactor at 1020 C prior to the arrival of oxygen The sample and tin capsule reacted with oxygen and combusted at 1700 1800 C The sample was broken down into elemental components N2 CO2 and H20 High performance copper wires at 700 C absorbed excess oxygen not used for sample combustion The gases flowed through a water trap and then through a gas chromatography GC separation column at 35 C As the gases passed through the GC column they were separated and detected sequentially by a thermal conductivity detector TCD The TCD generated a signal proportional to the amount of element in the sample Costech EAS software com
125. able 5 0 Analysts who work in the lab are required to read the following MDH safety policies located in the MDH Policy and Procedure Manual POLICY TITLE 902 02 1 Occupational Safety and Health 420 01 1 Right to Know Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 4 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc P RE 5 3 5 4 5 5 5 6 5 7 In addition the analyst should read the MDH Public Health Laboratory Division Chemical Hygiene Plan http fyi health state mn us phl safety index html Questions regarding the Chemical Hygiene Plan should be referred to the Laboratory Health and Safety Officer The analyst should read the Lab Building Emergency Procedures plan http fyi health state mn us phl safety index html and know what to do in a variety of emergency situations Safety glasses should be worn by all analysts at all times while in the laboratory area Visitors are given temporary safety glasses while in the laboratory Lab coats and other protective clothing should be worn by analysts when appropriate The analyst may contact the Minnesota Poison Control System regarding employee exposures to hazardous chemicals www mnpoison org or 1 800 222 1222 The system is available
126. acetate dehydrate Zn O2CCH3 2 H20 Stir until dissolved Dilute to volume with degassed reagent water Prepare fresh every 6 months 7 15 NaOH preservative 15 M In an acid rinsed 200 mL flask add approximately 100 mL degassed reagent water then add 125 g sodium hydroxide pellets NaOH Stir until dissolved Dilute to volume with degassed reagent water 7 16 Acid Volatile Reagents 7 16 1 NaOH 2N In an acid rinsed 500 mL flask add approximately 300 mL degassed reagent water then add 100 mL 10N NaOH Dilute to volume with degassed reagent water Prepare freshly each month 7 16 2 Acid volatile Catch Solution In an acid rinsed 500 mL flask add approximately 300 mL degassed reagent water then add 100 mL alkaline antioxidant reagent and 12 5 mL 2N NaOH Dilute to volume with degassed reagent water Prepare freshly dail Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 8 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc 7 163 Hydrochloric Acid 9N In an acid rinsed 250 mL flask add approximately 100 mL degassed reagent water then slowly add 186 mL concentrated hydrochloric acid Dilute to volume with degassed reagent water 7 16 4 Stannous Chloride Solution 0 53M Dissolve 50 g SnCl into 250 mL 9N HCI solution
127. aeneae es eere rennen nenne 23 16 0 BIBLIOGRAPHYJY i oPosn cneniceecedenviam e 24 17 0 TABLES FIGURES VALIDATION DATA sese nennen 24 Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 2 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc SCOPE AND APPLICATION 1 1 1 2 1 3 1 4 1 5 1 6 Sulfide is often present in groundwater especially in hot springs Its common presence in wastewaters comes from the decomposition of organic matter industrial wastes mine run off and the bacterial reduction of sulfate Hydrogen sulfide escaping into the air from sulfide containing wastewater causes odor nuisances The threshold odor concentration of H5S in clean water is between 0 025 and 0 25 ug L Gaseous H3S is very toxic and has claimed the lives of numerous sewer workers At levels toxic to humans it interferes with the olfactory system so that it cannot be detected It attacks metals directly and indirectly has caused serious corrosion of concrete sewers because it is oxidized biological to H2SO on the pipe wall Dissolved H3S is toxic to fish and other aquatic organisms Hydrogen sulfide in sediments can combine with iron and other metals to form slightly soluble precipitates Acid volatile sulfides AVS is an main class of
128. al CCV is reanalyzed If the analyte is still outside the 10 limit the instrument is recalibrated and all samples following the last acceptable CCV solution are reanalyzed 9 2 6 Accuracy With every batch of 20 samples processed as a group analyze a laboratory control sample BS Accuracy as percent recovery is calculated as follows V NE dE Found Concentration of BS 100 A ZAAPA ee Y True Concentration of BS Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 15 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc 9 2 7 Ifthe recovery of the analyte falls outside the required control limits of 90 110 the analyte is judged out of control The source of the problem should be identified and the situation resolved before sample analysis can continue 9 2 8 Matrix Effect Run a matrix spike MS with each batch of 20 field samples processed as a group or 5 of the samples analyzed whichever is greater The same solution used to fortify the BS is used to fortify the MS Accuracy as percent recovery after background correction is calculated as follows Concentration of MS Concentration of Matrix Sample a True Concentration of MS Recovery 100 9 2 9 If the recovery of the MS falls outside of 80 120 limits the MS is repeated If th
129. al Laboratory Effective Date Date of last signature Page 26 of 57 SAMPLE RECEIVING MONTHLY REPORTS The Sample Receiving Lead worker is responsible for preparing monthly reports The reports include the following information 1 A per Unit Metals Organics etc sample count for the month along with the totals from the same month of the previous year 2 Total number of samples received all types this 1s really the total of sample numbers used along with the same total from one year before 3 News of procedural changes additions and other pertinent news After the report is completed one copy is emailed to the Laboratory Services Supervisor and a hardcopy is kept in the Sample Receiving Monthly Reports Logbook CREATING THE MONTHLY REPORT The Monthly Sample Count is sent to sample receiving via email This is a report of the total number of samples received listed by Unit On the report Unit numbers are listed first followed by a date then the sample totals The Unit numbers are assigned as follows per Unit Metals Organics etc sample count the month along with the totals from the same month of the previous year 0 Administrative code do not put in the peport Y 2 Metals 4 Organics 6 Radiation 7 Micro particulate 8 Bactichem To find the total number of samples received in a month use the Lab Review function to find the first and last sample numbers used in the month The total will be th
130. ample and delete the appropriate analysis codes Add a receiving comment indicating which codes were removed who requested the cancellation and the reason Code 994 No Sample Received This code is used very infrequently to indicate that a sample indicated on a lab sheet was not received Environmental Health uses mostly preprinted lab sheets for their sampling In some cases not all the samples indicated on the sheets are collected The well may be out of service or a sampling point may be inaccessible Usually the collector will indicate in some way that the sample was not collected by crossing it out or writing a note on the lab sheet e If this is the case just do not assign that particular sample point a number Code 994 should only be used in cases where there is no indication why a sample is missing Code 997 Number Not Used This code is assigned to a sample number when the number was assigned in error and a correction to the data sheet is not possible When an error is noticed we first try tocorrect it by moving the extra number to another sample or sheet If no simply solution is possible code 997 is used See the next section for more information on correcting numbering errors Code 999 Analysis Can Not be Run This code is assigned when a problem is noticed in Sample Receiving that would prevent the sample from being analyzed such as a broken bottle e During initial data entry type in code 999 d of the affected codes and a b
131. andard Operating Procedures esses 42 Appendix D University of Minnesota Civil Engineering Laboratory QA Procedures and Standard Operating leves MO NON 43 Appendix E National Lacustrine Core Facility Limnological Research Center Laboratory QA Procedures and Standard Operating Procedures sess entretenir enne enne trennen entree 44 Table 1 Experimental Target Analytes in Overlying Water esses enne nn 15 Table 2 Experimental Target Analytes in POreWateT ooo cccccconocoonnnnonncnnonoononnnncnnnnnnnnnnnnnonnnonononnnnncnnnonennnnnnncnnnns 15 Table 3 Experimental Target Analytes in Sediment sess eene nnne nnne th nnns nns nnn 16 Table 4 Quality Control Elementsin nan e EE e ea a Ea ENE E E aa 29 Table 5 QC Acceptance Criteria for Target Analytes in Overlying Water and Porewatel ccccscsecscsssseceeseees 29 Table 6 QC Acceptance Criteria for Target Analytes in SediMent oocconoccconinnnnnnncnnonanononnnnnno non enne enne 30 Figure 1 Acrylic Tubing Polyester base and steel hose claMp oooocccccncconononoonnonccnnononnnononcnnnnnonnnnnnncnnonnonannnnnos Figure 2 Assembled microcosm base Figure 3 Side view of microcosm Figure 4 Top view of microcosm Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 3 Revision No 0 Date 12 9 2013
132. ansparent the aser also cisclosas that a Modif od Mathod X not just Malthad X ls belag used This annotation is especially important when modifying a method pualished by a standards oreanization guch as the Standard Methods Committee AOAC Intemational or ASTM International Tor oxamplo a lab win a CWA Imitod tke approval otter may canduet a luminescant messurement of dissolved oxygen DG with any approved method that requires a DO measurement such as BOD or CBOD by SAIS210B However to do so ihe tab will have a copy of adimiledase ATP aapnyvel teller The lay SOP also wil cile use uf SM 52108 as modified for luminesrant measyrameanl of CIO ws accondanee wilh Iha limitod 1sa ATP latter from tho regian or similar wordiag Why do we recommend uae oflimted vee ATP approva s rather ihan wait for nation wide approval Because rulemaking can be a lengthy process Thes n ou national ATP Jeller wa racenimern Thai regions consider approvirg use of ita ATP under their limited use ATP aparovol authority Is t necessary for a limited usa ATP applicant to submit dala or do a side by side comparison in these cases Our answer is generat y ro because methods that we review under Jie OWA ATP program alreagy have mulli lab and comperability data Feel free to share this memo with your co regulatose and the laboratory and method development coriunily Your contacts are the CWA ATP coordinator Lemuel Walker watkacJomual epa gav or the CWA methods t
133. any ribbon slack DATE TIME CLOCK We use an Amano Cincinnati PIX 3000 Electronic Time Recorder to stamp the date and time on Data Sheets Spare ink cartridges and the key to open the recorder are kept in the drawer right below it To change the ribbon cartridge or to re program the time date etc refer to the owner s manual e To reset the recorder after a jam unplug it and immediately plug it back in E Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 25 of 57 PHOTOCOPIER We have a Hewlett Packard Model 280 Color Copier i in Sample Receiving The ci Manual and extra inkjet print cartridges are stored in the drawer just below Replacement inkjet print cartridges are available from the MDH Stockroom Black HP inkjet cartridges Stockroom item 4375 0025 Color HP inkjet cartridges Stockroom item 4375 0570 Note The color copy function no longer works There appears to be a problem with the print head However since we don t make color copies this is not a problem FAX MACHINE We have a Brother Intellifax 4100 Laser Fax Machine in Sample Receiving It can also be used to make copies The number is 651 201 5362 and it is shared with Clinical Accessioning Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environment
134. ard select Delimited Next in step 2 select Tab Space and Comma Next and Finish From the report you can see the detail information based on options that you have defined in the report template If desired You can change the template and reprocess the data for other forms of results For a short and quick report that only shows the resulted cpt for each sample open the summary report you just defined before reprocess process Once you open your text report file in Excel save it as Excel file so that it can be easily open next time 16 Section No Appendix E Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 44 of 44 Appendix E National Lacustrine Core Facility Limnological Research Center Laboratory QA Procedures and Standard Operating Procedures Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan STANDARD OPERATING PROCEDURE TOTAL CARBON TOTAL NITROGEN TC TN Preparation and analysis of MN lake sediments submitted to the LLO for TC TN analysis Sample condition Samples were received from the LRC freeze dried and ground Myrbo in snap top plastic containers Some samples contained visible vegetative material Some samples contained small pebble sized material Inhomogeneity may result in greater analytical variability or misleading results Preparation Samples were mixed with a metal spatul
135. are contamination is a problem in low level phosphorus determinations Glassware should be washed with 1 1 HCl and rinsed with deionized water Commercial detergents should rarely be needed but if they are used use special phosphate free preparations for lab glassware 10 115 01 3 E Post MUR Page2 3 December 2010 sat 5 SAFETY 5 1 5 2 5 5 The toxicity or carcinogenicity of each reagent used in this method has not been fully established Each chemical should be regarded as a potential health hazard and exposure should be as low as reasonably achievable Cautions are included for known extremely hazardous materials Each laboratory is responsible for maintaining a current awareness file of the Occupational Health and Safety Act OSHA regulations regarding the safe handling of the chemicals specified in this method A reference file of Material Safety Data sheets MSDS should be made available to all personnel involved in the chemical analysis The preparation of a formal safety plan is also advisable The following chemicals have the potential to be highly toxic or hazardous for detailed explanation consult the MSDS 5 3 1 Sulfuric Acid 5 3 2 Sodium Dodecyl Sulfate SDS 5 3 3 Potassium persulfate 5 3 4 antimony potassium tartrate 6 EQUIPMENT AND SUPPLIES 6 1 62 6 3 6 4 Balance analytical capable of accurately weighing to the nearest 0 0001 g Glassware Class A volumetric fla
136. as developed by the Information Resources Management IRM Steering Committee through its Security Subcommittee The Security Subcommittee is a cross divisional group of managers with budget and policy authority and IT staff with technical expertise The security policy was created with input from individuals throughout the department who have responsibilities for the security of information resources C Additional Software The laboratory uses a variety of software programs for data production reduction verification and validation In addition to routine office software MS Office Professional the laboratory uses instrument software that varies according to the vendor and the intended purpose The laboratory uses validated software as supplied installed and maintained by the vendor SECTION 7 0 SAMPLING The laboratory does not perform its own sampling nonetheless the laboratory and the sample accessioning receiving area do provide guidance to field personnel for proper submission of samples to the laboratory The laboratory s clients or their contracted staff or volunteers are responsible for training collectors collecting samples and delivering samples to the laboratory The laboratory does not routinely accept samples collected by the general public i Instructions on the proper submission of samples bottle type preservative labeling and forms are included in various sample receiving area procedures and in the MDH Environme
137. at collect closed landfill samples The two standard MPCA forms are signed on the back of the white copy of the form This is not strictly enforced but 1f the collector or courier signs the form then we should as well The lab received date should also be recorded in the space provided on the front of the form upper right Fe Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision l Environmental Laboratory l Effective Date Date of last signature Page 49 of 57 The other forms are signed on the front of the top copy so that the information goes through all copies For all types of forms the collector or courier will sign their name in the relinquished by column They will also record the date and time of sample delivery A Sample Receiving employee must sign their name in the received by column then record the date and time of sample acceptance MPCA SAMPLE SCHEDULING Some MPCA collectors send us samples on a routine basis while others send samples more sporadically They are all supposed to inform us of any BOD CBOD Fecal Coliform Fecal Strep and Ortho Phosphorus samples they will be submitting The most important samples to know when they are coming are the Fecal Coliform samples since they only have a 24 hour hold time They should also inform us of any other unusual samples they will bring in such as Chain of Custody or Priority One samples They may notify
138. ate and Local regulations pertaining to hazardous waste disposal Prevent pollution at the source whenever possible Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 24 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc Consider environmental impact when purchasing materials handling chemicals and disposing of waste Promote awareness and provide training opportunities for pollution prevention and hazardous waste management within the Division Define the responsibilities of managers supervisors and staff so that Division activities will be conducted appropriately and effectively with regard to waste management Develop policies and procedures as needed to further these objectives 15 2 For additional information regarding the laboratory s waste management policy see the current version of the Public Health Laboratory Division Hazardous Waste Manual http fyi health state mn us phl safety ndex html 16 0 BIBLIOGRAPHY 16 1 Standard Methods for the Examination of Water and Wastewater Method 4500 S1 and J 21 Edition On line 16 2 Lachat Instruments QuikChem Method 10 116 29 3 A Determination of Dissolved Sulfide by Flow Injection Analysis 163 Appendix B to Part 136 Definition and Procedure for the Determinati
139. ate the mean concentration and the standard deviation for the data set The percent recovery of the mean must be between 95 and 105 while the percent relative standard deviation RSD must be less than 10 Both conditions need to be satisfied before sample analysis can begin 9 1 5 Where this documentation is not available the Quality Assurance Officer can establish other criteria to measure accuracy and precision for each analyst and each method 9 1 6 Demonstration of Low Background Analyze at least one Method Blank BLK to determine reagent or laboratory contamination The BLK result must meet the criteria established for the on going demonstration of low background in Section 9 2 3 9 1 7 Other Requirements for an IDC An IDC may also be required if there are significant changes to the SOP matrix or instrument that could affect the precision accuracy or sensitivity of the analysis Consult with the Quality Assurance Officer QAO to determine if any changes require an IDC 9 1 8 IDC Documentation An IDC for each analyst must be on file in the QA office along with an IDC for the method matrix and instrument 9 2 Ongoing demonstration of acceptable performance With every analytical run the laboratory must perform the following 9 2 1 Daily Calibration Calibrate the instrument at the beginning of the analytical run or whenever the curve verification fails Calibrate the instrument with a calibration blank and 7 standards
140. ater and Wastes EPA 600 R 93 100 Revised March 1993 Method 365 1 L Woo W Maher Analytica Chimica Acta 315 1995 123 135 Guideline and Format for EMSL Cincinnati Methods EPA 600 8 83 020 August 1983 Richard L Benson lan D McKelvie and Barry T Hart Analytica Chimica Acta 291 1994 p 233 242 Lachat notebook 133 Ninglan Liao page 81 to 150 Lachat QuikChem Method number 10 115 01 3 A 10 115 01 3 E Post MUR Page 14 3 December 2010 sat 17 TABLE DIAGRAMS FLOWCHARTS AND VALIDATION DATA 17 1 DATA SYSTEM PARAMETERS FOR QUIKCHEM 8000 8500 The timing values listed below are approximate and will need to be optimized using graphical events programming Sample throughput 32 samples h 110 s sample Pump Speed 35 Cycle Period 110 7 Analyte Data Concentration Units ug P L Chemistry Brackish Inject to brackish baseline start 20 8 Inject to br ckish baseline end 129 6 Inject to brackish integration start 40 0 Inject to brackish integration end 61 0 Calibration Data Concentration ug P L 250 100 Calibration Rep Handling Average Calibration Fit Type l 1 Order Polynomial Weighting Method Vx Force through zero No Sampler Timing is Min Probe in Wash Period 19s Probe in Sample Period gt 70s Valve Timing Load Period 358 Inject Period 75s Sample to the first valve 280 S Time to first valve must be measured Value given is as a starting
141. balt 136 137 Metals Copper 145 146 Metals Iron 152 154 Metals Lead 157 158 Metals Magnesium 696 697 Metals Manganese 166 168 Metals Mercury 200 202 Mercury Nickel 171 172 Metals Nitrate nitrate nitrite 69 Nutrient Nitrite 67 General 1 liter J Minnesota Department of Health Public Health Laboratory Division Environmental Laboratory Nitrogen Ammonia Potassium Sodium Solids total dissolved Solids total suspended Sulfate Volatile Organic Compounds Vanadium Zinc 64 255 256 257 258 5 3 28 498 248 249 194 195 Sample Receiving Procedure Manual Revision Effective Date Date of last signature Page 52 of 57 Nutrient Metals Metals General 1 liter General 1 liter General 1 liter 40 ml VOC vials Metals Metals Special dissolved analyses Some of the metal and mercury samples will be filtered in the field Make sure that you make note of which ones are filtered on the paperwork The paperwork should be noted but many times the paperwork is incorrect and it needs to be checked When entering the analytical codes make sure dissolved codes are entered in for the samples that were filtered The parameter lists might not indicate what the dissolved codes are so they will have to be look up in the Environmental Laboratory Handbook This tends to take up a lot of time so if there are any other samples that need to be delivered to the labs do that before working on the Interpol samples
142. below as an alternative to an MDL when they have determined that it is more appropriate 1 Method Detection Limit MDL The study must be performed as described in Appendix B to Part 136 Definition and Procedure for the Determination of the Method Detection Limit Revision 1 11 The calculated MDL must meet the acceptance criteria established for each analysis or analyte by the Quality Assurance Officer 2 Minimum Reporting Level Confirmation MRLC The MRLC is described in the UCMR2 Unregulated Contaminant Monitoring Regulation Laboratory Approval Manual version 2 0 October 2006 For the MRLC fortify extract and analyze seven replicate laboratory fortified blanks LFBs at or below the MRL concentration These LFBs must contain all method preservatives described in the method contain each analyte of interest at concentrations at or below the MRL and be processed through the entire method procedure ie including extraction where applicable The mean and standard deviation are calculated Using the formulas in Section 7 of the UCMR2 Laboratory Approval Manual calculate HR half range for the prediction interval of results upper PIR prediction interval of results limit and lower PIR limit The recoveries must meet the acceptance criteria established for each analysis by the Quality Assurance Officer Note the UCMR2 requires that the upper PIR limit must be lt 150 96 recovery and the lower PIR limit must be gt 50 recovery
143. brane in the debubbler if it begins to weep around the edges 11 3 8 Check list before running samples 11 3 8 1 Check that the method s timing has been correctly set by running food dye 11 3 8 2 Check the temperature of digestion module 11 3 8 3 Check that all reagents were prepared correctly 11 3 84 Check that the debubbler is in good condition with no leaking The debubbler should be tested by running one standard in duplicate or triplicate 11 3 8 5 If precise duplicate peaks are produced real samples can be run Otherwise adjust the timing and troubleshoot further 11 3 9 Maintain environmental temperature around 20 25 C for best results Jf temperature is significantly higher or lower the heater temperature in the in line module may need to be adjusted accordingly higher or lower 3 5 to start 13 DATA ANALYSIS AND CALCULATIONS AAA A A A e 12 1 12 2 12 3 Calibration is done by injecting standards The data system will then prepare a calibration curve by plotting response versus standard concentration Sample concentration is calculated from the regression equation Report only those values that fall between the lowest and highest calibration standards Samples exceeding the highest standard should be diluted and reanalyzed Report results in ug P L 13 METHOD PERFORMANCE 13 1 13 2 The method support data are presented in Section 12 This data was generated according to a Lachat Work Instr
144. cal methods that are to be used are identified in these tables by the laboratory performing them along with their location in the appendices of this document Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 6 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 15 of 44 Table 1 Experimental Target Analytes in Overlying Water Analytical Method Location of Target Analyte Report Level RL Reference Laboratory Method vanas O to 50 mg L with 0 01 Hydrolab UMD Civil Appendix D ye mg L resolution Multiparameter Sonde Engineering T 0 to 100 mS cm with Hydrolab UMD Civil Appendix D Conductivity 0 0001 unit resolution Multiparameter Sonde Engineering B O to 14 units with 0 001 Hydrolab UMD Civil Appendix D P unit resolution Multiparameter Sonde Engineering 5 to 50 C with 0 01 C Hydrolab UMD Civil Appendix D Temperature resolution Multiparameter Sonde Engineering n UMD Civil Appendix D Sulfate 0 05 mg L Modified EPA 300 1 Engineering Chloride 0 05 mg L Modified EPA 300 1 UMD Civil Appendit D Engineering UMD Civil A dix D Bromide 0 05 mg L Modified EPA 300 1 ed MNT Engineering Fluoride 0 05 mg L Modified EPA 300 1 OE Appenditp Engineering QuikChem Method 10 MDH Appendix C Dissolved Phosphate 0 01 mg L 115 01 3 E Environmental QuikChe
145. can define a file receiving a summary report of each reprocessing of the data Autosampler is important part for running a batch of sample Switch to device tab by clicking Device on main menu Switch to autosampler tab Select autosampler Cetac ASX 500 Tray name ceasx500 as500d try Select Port GPB1 Initialize the sampler by clicking Initialize Numbering the location of the sampler 1 The first row on the top fit for 50 ml centrifuge tube is numbered as one to ten from left to right Standard solutions are used to put in these locations There are four sampling trays sitting on the floor of the auto sampler each tray holds 24 sample tubes 3 columns and 8 rows from left to right the sample tubes located at the first tray are numbered as 11 to 18 for the first column 19 to 26 for the second column 27 to 34 for the third column in the second tray from left to right the first column is number as 35 to 42 the second column is number as 43 to 50 and so on Total 106 samples including standard solutions can be put in the auto sampler at the same time The table below shows the setup of the tray in auto sampler 10 After defining sampling file putting samples in the appropriate location in the auto sampler and initializing the auto sampler you can click the button of Analyze Batch in sampling window The batch of sample
146. can select different isotopes of each element or use equation for reducing interference in the process of measurement Calibration Tab This is important for setting up your file 1 In this window you need to define the concentrations of each elements in your standard solution 2 This information is used by the system to automatically calculate the results of your sample 3 Make sure the list of analytes and their Mass numbers in calibration window are the same as they are in the Processing and Time Tabs 4 Double check and make sure sample unit and calibration unit are consistent for each element Sampling Tab 1 Here to define the criteria of sampling process such as the time for sample flush read delay washing time If you see any contamination between samples from the results of your measurement you can come back here to adjust the time of washing and speed of the pump Report Tab 1 This Tab located at the right hand side of the method window 2 Onreport view you can define the template of report for measurement results defined and use two template files Johnson report rop and Johnson report simple rop you are welcome to use or to adjust them Don t check sent to Printer or Generate NetCDF file 3 On Report to file check report to file select the right report template file in the box of Report options template define the report file name otherwise the results of a new run or reprocess will
147. ce of sampling on the surrounding filters Figures 3 and 4 illustrate the arrangement of the pre installed filters Filter assemblies consisted of a modified Rhizon filter sealed in a 1 8 ID barbed to NPT fitting which was inserted into tapped holes in the microcosm body The Rhizon sample line was sealed to the fitting using epoxy to seal a 1 8 ID Tygon tubing sheath around both Rhizon sample line and NPT fitting See Table 2 for what analyses are to be done on sediment porewater the laboratory to do the analyses and location in the Appendix of the analysis specific sampling requirements as defined in the laboratory s SOP Timing It is expected that porewater samples will be extracted 2 times during each experimental phase 2 5 days after the initiation of the phase and near the end of the experimental phase Less than 4mL of water will be extracted in order to minimize the disturbance of the porewater profiles The limited pore water volume will be prioritized for analysis of sulfate and other anions lon Chromatography pH sulfide and ferrous iron Final Sediment Collection and Characterization Method In each microcosm one 2 diameter sediment core will be taken to identify and enumerate the various types of benthic microorganisms that may contribute to variations in flux of target analytes into and out of the sediment Organisms will be filtered out of sediment samples using 500 micron sieves Organisms are then immediately preserved
148. ce procedures Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 21 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc 11 6 2 Samples that are over concentrated should be diluted with the diluent and not reagent water 11 7 Acid Volatile Samples 11 7 1 Allow samples to thaw to room temperature 11 7 2 Using an analytical balance weigh out 1 g of soil into Teflon vial When balance stabilizes record weight in spreadsheet Data transfer program will insert weight in selected spreadsheet cell eliminating need for typing weight and the possibility of transcription errors 11 7 3 Add 25 mL Acid volatile catch solution to each 50 mL trap and label each with specified sample number 11 7 4 Set flow meters to a scale reading of 20 Loosely cap each Teflon vial and allow nitrogen to purge for at least three minutes 11 7 5 Using a syringe inject 15 mL stannous chloride solution into each Teflon vial Quickly screwing on each cap so that no sulfide is lost 11 7 6 Turn on stir plate and allow nitrogen to purge at room temperature for 3 hours 11 7 7 After 3 hours remove 2 5 mL of sample and dilute with 2 5 mL of diluent and proceed to step 11 4 3 11 8 Acid Volatile dry weight 11 8 1 Allow samples to thaw to room temperature 11 8 2 Tare t
149. ceptance criteria and any action the analyst must take if the acceptance criteria are not met Results of the modified RLV MRLV check or alternative QC procedure shall be recorded as directed by the Unit Supervisor or Quality Assurance Officer Note The effective date of this document is the date of the last signature on this document On the effective date this document becomes an appendix to the Quality Assurance Manual for the Environmental Testing Units of the Public Health Laboratory Division Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 61 of 67 http fyi health state mn us phl environmental index html Appendix 12 USEPA Certification for Laboratory Analyses for Drinking Water D 85 QC UNITED STATES ENVIRONMENTAL PROTECTION AGENCY c REGION 5 ZA Pw KEA ANAA 77 WEST JACKSON BOULEVARD ro EA CHICAGO IL 60604 3590 AUG 2 9 2008 REPLY TO THE ATTENTION OF WG 15J Dr Louise Liao Minnesota Dept of Health Division of Public Laboratories 601 Robert Street North P O Box 64899 St Paul MN 55164 0899 Dear Dr Liao On May 5 7 2008 Patrick Churilla inspected your laboratory for proficiency in chemical microbiological and radiochemical drinking water methods pursuant to the National Primary Drinking Water Regulations as implemented by 40 CFR Parts 141 and 142 Based on
150. chematic of the experimental phases and timeline for measuring flux with overlying water measurements Overlying water composition Overlying water amendments consist of a mixture of magnesium sulfate sodium sulfate and calcium sulfate designed to mimic water composition of mining impacted streams on the Mesabi Iron Range Tracers in the form of sodium chloride sodium bromide or sodium fluoride will be added for each respective phase of the experiment Sulfate and chloride bromide and fluoride in site water immediately after collection was used to define in situ sulfate concentrations and tracer levels for each phase of the experiment sufficiently large to be clearly identified above background in pore water samples During each experimental phase concentrations of sulfate and tracers in the overlying water will be monitored and may be amended with appropriate volumes of magnesium sulfate and sodium tracer stock solutions when concentrations drop below 80 9096 of their target values Additional water will be collected from the site when necessary to periodically replace overlying water minimum of once per experimental phase Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 2 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 24 of 44 Section B 2 Sampling Methods Overlying Water Collection Method Samples from the overlying water will b
151. chnical expertise of the analyst is needed for evaluation of the data reviews of the report produced from the raw data and verification that the QC checks are within required limits e g spikes surrogates blanks duplicate spikes etc The raw data and final report are submitted for verification Section D 1 2 Data Verification Methods The laboratory manager or designated experienced chemist verifies data is correct as reported A manager reviews 10096 of the raw data against the report to verify data interpretation made by the chemist and that QC checks are correct and makes sure no transposition errors were made The laboratory QA Officer reviews a percentage of all reports to verify that data meets all requirements of the QAPP The specific procedures to be followed by the laboratory are described in the laboratory QAM if available The flags used on the data will be consistent with those used by EPA for CLP data J R U B etc The laboratory stores all raw data in their archives for five years Raw data is available to MPCA staff as needed The MPCA Project staff does a data review when the analytical report is received MPCA staff review data to verify all QC is acceptable the project requirements are met holding times and reporting limits and that all required information is present in the report The MPCA project manager reviews the data to ensure that all quality control requirements are met The project manager also reviews
152. cipated usage and reagent stability For information about pollution prevention that may be applicable to laboratories and research institutions consult Less is Better Laboratory Chemical Management for Waste Reduction available from the American Chemical Society s Department of Government Regulations and Science Policy 115 16th Street N W Washington D C 20036 202 872 4477 15 WASTE MANAGEMENT 15 1 The Environmental Protection Agency USEPA requires that laboratory waste management practice be conducted consistent with all applicable rules and regulations Excess reagents samples and method process wastes should be characterized and disposed of in an acceptable manner The agency urges laboratories to protect the air water and land by minimizing and controlling all releases from hoods and bench operations complying with the letter and spirit of any water discharge permit and regulations and by complying with all solid and hazardous waste regulations and by complying with all solid and hazardous waste regulations particularly the hazardous waste identification rules and land disposal restrictions For further information on waste management consult the Waste Management Manual for Laboratory Personnel available from the American Chemical Society at the address listed in Sect 14 3 16 REFERENCES 16 1 16 2 16 3 16 4 16 5 16 6 U S Environmental Protection Agency Methods for Chemical Analysis of W
153. complished using Commvault backup software where tapes are cycled weekly to an offsite vendor on a 2 week rotating Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 24 of 67 http fyi health state mn us phl environmental index html m 5 5 en nl system B Computer Security All laboratory employees must follow the MDH Information Resources Security Policy http fyi health state mn us comm irm sc infosec se010122securitypolicy pdf This policy is designed to counter risks to information security that are internal and external to the organization Such risks include loss of privacy reading of information by unauthorized persons loss of data corruption or erasure of information and loss of service filling of data storage space use of computational resources denial of network access Although intruders on security systems and computer viruses are the most highly publicized security breaches many computer security surveys show that the greater risk is from individuals working inside an organization In order to design cost effective security policies and plans the threats to the security of the information resources of an organization must be analyzed in terms of how they affect the availability confidentiality and integrity of those resources The departmental security policy w
154. cordingly A discrepancy found during the review process triggers a recheck of data or reanalysis of the samples Once the unit supervisor or designated analytical staff approves the data the LIMS recognizes the approval as an authorization to release the final report B Reporting At times the client may need to view data prior to the final review and approval Any authorized user can generate a preliminary report All preliminary reports are indicated as such in the header of the report Some clients are also authorized by the laboratory to view reports via a secure password protected internet based application Reports that have been amended are indicated as such in the header of the report In addition the item s in the report that have been changed are described at the end of the report with the corrected value reported alongside the previous value SECTION 15 0 SYSTEM AUDITS A Proficiency Testing The laboratory participates in proficiency testing PT studies for the SDWA CWA RCRA and OSHA programs to demonstrate laboratory capability for analytes of interest The samples are purchased from approved providers certified by the American Association for Laboratory Accreditation A2LA a NELAP recognized proficiency testing oversight body that require analytical quantification within the acceptance limits established by USEPA and the NELAC standard The true value of the concentration of the reference material is unknown to the labo
155. ctive Date Date of last signature Page 40 of 67 http fyi health state mn us phl environmental index html SECTION 16 0 REFERENCES Methods for Chemical Analysis of Water and Wastes EPA 600 4 79 020 Revised March 1983 Methods for the Determination of Metals in Environmental Samples EPA 600 4 91 010 June 1991 Standard Methods for the Examination of Water and Wastewater 20th Edition APHA AWWA WPCF Washington D C 1998 Methods for the Determination of Organic Compounds in Drinking Water EPA 600 4 88 039 Revised July 1991 Methods for the Determination of Organic Compounds in Drinking Water Supplement 1 EPA 600 4 90 020 July 1990 Methods for the Determination of Organic Compounds in Drinking Water Supplement 2 EPA 600 R 92 129 August 1992 Prescribed Methods for Measurement of Radioactivity in Drinking Water EPA 600 4 80 032 EPA Requirements for Quality Assurance Project Plans for Environmental Data Operations EPA QA R 5 Draft January 29 1993 Manual for the Certification of Laboratories Analyzing Drinking Water 5 Edition USEPA January 2005 Microbiological Methods for Monitoring the Environment EPA 600 8 78 017 December 1978 Minnesota Department of Health Environmental Laboratory Sample Receiving Procedure Manual Rev 4 Laboratory Information Management Systems and Technical Services Section 2006 IUPAC Compe
156. ctory performance must be maintained over the effective time of the QAPP Copies of the results of the PE studies must be supplied to the MPCA s QA Coordinator Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No C 2 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 36 of 44 Section C 2 Corrective Action Reports to Management For each analytical activity employed in this Project the laboratory regularly tracks the overall quality assurance issues When a quality control sample or QA issue is found to be out of control Corrective Actions CA are implemented Corrective action includes re analysis of samples re sampling flagging of data or rejection of the data MPCA is informed of any major CA that is performed on any Project sample Section C 2 1 MPCA Corrective Actions The individual identifying a potential issue first documents the problem in the laboratory notebook The project manager who has final sign off authority on any problem or issue tracks the problem The project manager tracks all CA The PM is responsible for identifying the problem verifying proper documentation is written and implementing the correct action The project manager will place final documentation into the site record Any major CA involving the laboratory is tracked by the both the laboratory QAO and the MPCA project manager The MPCA project manager has final
157. d at their discretion publish results from the project in a peer reviewed journal Section A 4 3 The University of Minnesota Duluth Principal Investigator John Pastor Ph D The Principal Investigator will Review and approve the Quality Assurance Project Plan QAPP including subsequent revisions Work in a collaborative capacity with Work Order Coordinator and Graduate Researcher to support all aspects of the experiment described within Section A 4 4 The MPCA Division Manager Shannon Lotthammer The MPCA Division Manager will Provide administrative direction to assigned staff as needed Implement the elements of the Project as well as any required quality control measures Manage the budget to assure that goals are met and funds and resources are responsibly allocated Review and approve the QAPP including subsequent revisions Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 4 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 10 of 44 Conduct annual performance appraisals of assigned staff specific to their position description relating to the Sulfate and Wild Rice Project Section A 4 5 The MPCA Project Manager Edward Swain Ph D The MPCA Project Manager will Provide administrative direction to assigned staff and to the MPCA QA QC coordinator as needed Implement the elements of the Project as well as a
158. d deliver with the samples to the Microbiology bench e For Cryptosporidium samples code 347 note the received temperature of the samples and make a copy of the sheet Put the samples either 10 liter jugs or plastic filter pipes in the walk in cooler in bactichem and place the lab sheet copy on the lab bench OSHA SAMPLES Samples from OSHA are always program code MG specific analysis codes can be found in the OSHA section later in the manual The submitters will wait to leave until sample custody is signed over Make a copy of all OSHA sheets For organics samples deliver the samples with the original sheet and send the copy to clerical For metals samples deliver the copy with the samples and send the original to clerical MICROPARTICULATE SAMPLES We no longer analyze micro particulate or asbestos samples at MDH They are subcontracted out to Braun Intertec Labs Most of the samples we receive for this type of analysis are from Northshore Mining They send both air and water samples They are supposed to notify David Foster before they send any samples When they arrive let him know and he will fill out the special form and make the arrangements to send them out Some of the samples have very short hold times so let David Foster know right away so he can get them processed Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division E Revision Environmental Laboratory l Effective Date Date
159. d in the U S A Edition 7 Standard Operating Procedure for Analysis of sulfide by the methylene blue method spectrophotometry Johnson Research Group UMD Civil Engineering Updated 4 1 2013 The methods outlined in the Standard Methods for the Analysis of Water and Wastewater Method 4500 S2 D as implemented in Hach Sulfide method 8131 are followed on a Hach DR 2800 portable UV VIS spectrophotometer Briefly an appropriate volume of sulfide Reagent I 596 is added to a clean sample vial to which sample is carefully delivered with a pipette Sulfide reagent II is immediately within 30s added to the vial capped and gently mixed Absorbance is read at 660nM within 30 minutes and compared to absorbance of blanks and standards For low concentrations blanks and standards are prepared in deoxygenated but formerly oxidized matrix water Standard Operating Procedure for Analysis of anions by Ion Chromatograph Johnson Research Group UMD Civil Engineering Updated 4 1 2013 The methods outlined in EPA Method 300 1 are followed on a Dionex ICS 1100 Integrated IC system AS DV Autosampler Each sample is injected into the 25 uL sample loop and separated using a Thermo Scientific AS22 IonPac 4x250 mm anion exchange column after which each anion passes through the conductivity cell for detection The eluent is 4 5 mM sodium carbonate and 1 4 mM sodium bicarbonate pumped at a rate of 1 2 mL min 1 The suppressor current is set at 31 nA and th
160. d repeat the test Matrix spikes The laboratory must spike in duplicate a minimum of 10 percent of all samples one sample in each batch of ten samples from a given sampling site or if for compliance monitoring from a given discharge The two sample aliquots shall be spiked with the stock standard section 7 2 9 3 1 The concentration of the spike in the sample shall be determined as follows 9 3 1 1 If as in compliance monitoring the concentration of the analyte in the sample is being checked against a regulatory concentration limit the spiking level shall be at that limit or at 1 to 5 times higher than the background concentration of the sample determined in Section 9 3 2 which ever is higher 9 3 1 2 If the concentration of the analyte in a sample is not being diee against a limit the spike shall be at the concentration of the precision and recovery standard used in Section 9 2 5 or at 1 to 5 times higher than the background concentration whichever concentration is higher _10 107 04 3 D l Page 9 2 Dec 2010 sat 9 32 Analyze one sample aliquot out of each set of ten samples from each site or discharge according to the procedure beginning in Section 11 to determine the background concentration of B of the analyte 9 3 2 1 If necessary prepare a standard solution appropriate to produce a level in the sample at the regulatory compliance limit or at 1 to 5 times the background concentration per Section 9 3
161. dated April 14 2008 Please contact the EPA or Lachat Instruments for copies of the above mentioned EPA correspondence EPA Contacts for MUR questions are CWA ATP Coordinator Lemuel Walker walker lemuel epa gov The CWA methods Team OSTCWAMethods Mepa gov Lachat would love to hear about your lab s experiences with the MUR Is the intent to allow for more flexibility helping your lab Please send Lachat any comments good or bad on the MUR to Lachat Technical Support support lachatinstruments com Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 31 of 31 nape inside mn Bo ies MOE a en Chem pii capt doc Appendix II ats S fa gt UNITED STATES ENVIRONMENTAL PROTECTION AGENCY NZ WASHINGTON D C 20460 a n Pite April Et 2008 CeEKE OF A A WATER Yo Re omil Ay Coordinelurs end From Richard Rating Ph D Chic Engines ring amt Analyhest Sig it indi Urjyinecring amp Anelysis Division Ofdee of Scienve amp l ecknofeuy Fonte Citing Claan Waler Aa Limlled Use ATP Mehads as Modficalons i am wriling to our regional pariners about citing a method for which a Region has issued alicdted use ATP approval teller tael results in roditring arolher aaproved melhod In addition ta documentisig Ural the medificalion works to be fully tr
162. dated using a concrete consolidation table with a variable frequency rheostat For each site an extra microcosm was prepared identically in order to measure solids density after an initial settling period by extracting a sub core Solids density in this extra microcosm will be used to provide a comparison of the test conditions with those measured in situ Overlying Water Mixing Aeration A slow stream of air bubbles were introduced into the overlaying water through PTFE tubing at approximately 10 25 96 of the water depth from the sediment to provide a well mixed oxygenated system similar to what would be experienced in situ Aquarium pumps 70 liters min at 13 8 kPa were used to push air through two filters and a saturation chamber A HEPA filter in series with an activated carbon filter was used to ensure contaminants were not introduced into the microcosms through the air stream The air was then pushed through a filter flask filled with site water in order to saturate the air with water vapor prior to bubbling through the microcosm overlying water and reduce evaporation within the microcosm The air line runs out of the saturation flask through a flow controller and into a polycarbonate gas manifold from which it was distributed to six microcosms through 1 8 ID Tygon lab tubing and PTFE tubing into the microcosm overlying water Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Sectio
163. de technical representation at meetings Prepare reports Review the QAPP including subsequent revisions Section A 4 11 University of Minnesota LacCore LRC Laboratory Manager Amy Myrbo Ph D Ensure that the analytical requirements of the QAPP are implemented Provide direct supervision and project assignment to assigned staff Provide direction for the daily work activities Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 4 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 12 of 44 e Provide technical representation at meetings e Provide direction for analytical requirements e Perform final review of analytical data reports to ensure requirements are met e Review and approve the QAPP including subsequent revisions Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 5 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 13 of 44 Section A 5 Definition Background Minnesota currently has a water quality standard of 10 mg L sulfate applicable to water used for production of wild rice during periods when the rice may be susceptible to damage by high sulfate levels Minn R 7050 0224 subpart 2 This 10 mg L sulfate standard was adopted into the MPCA water quality standards in 1973 to protect wild rice Wild rice is an
164. dissolved turbidimetric 50 Silica dissolved reactive 59 Phosphate total 60 Phosphate dissolved 64 Ammonia Nitrogen total 65 Organic Nitrogen total 68 Kjeldahl Nitrogen total 69 Nitrate 74 Organic Nitrogen dissolved e 77 Ammonia Nitrogen dissolved 78 Nitrate dissolved 79 Kjeldahl Nitrogen dissolved 85 Phenol 94 COD chemical oxygen demand dissolved 97 COD total 98 TOC Total Organic Carbon 99 Dissolved Organic Carbon 200 Mercury low level total in water 202 Mercury low level dissolved in water 294 Perchlorate 400 EDB amp DBCP SDWA 408 Carbamates 452 Chlorophyll A lab filtered 637 Mercury SDWA 698 Mercury high level total in water 699 Mercury high level dissolved in water TESTS WITH A 30 DAY HOLD TIME 450 Chlorophyll A field filtered e 45 Pheophytin A TESTS WITH A 6 MONTH HOLD TIME Preserved metals except mercury Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division l Revision Environmental Laboratory Effective Date Date of last signature Page 31 of 57 ENVIRONMENTAL HEALTH SAMPLES Environmental Health Public Water Supply samples must be handled in accordance with Environmental Protection Agency drinking water rules and regulations The Environmental Health Division 1s organized as follows Division Environmental Health Section Drinking Water Protection Units 1 Community Public Water Supply Sub unit Corrosion Control 2
165. e 5 21405 Precision Data for Ortho Phosphate using a 250 ug P L standard RSD 0 128 Standard Deviation s 0 322 pg P L Mean x 250 9 ug P L Known Value 250 0 pg P L File Name 12 3 cal support omn Acq Date 3 Dec 2010 10 115 01 3 E Post MUR Page 27 3 December 201 0 sat 0 03554 q 3 E s 99 66 ug L 100 100 i8 100 109 8 9 i B i 98 64 ug L 9 99 59 ug L 99 89 ug L 99 54 ug L El E 70 ug L E 57 ug L o 8 99 73 ug L a 99 09 ug L Volts DA e mmt 21333 Time s Precision Data for Ortho Phosphate using a 100 ug P L standard RSD 0 393 Standard Deviation s 0 391 ug P L Mean x 99 54 ug P L Known Value 100 ug P L File Name 12 3 cal support omn Acq Date 3 Dec 2010 0 4528 un E El 2 e S 8 2 a 504 4 ug L 502 8 ug t i 30033 Time s Carryover Study Two 500 ug P L standards followed by three blanks Carryover Passed File Name 12 3 cal support omn Acq Date 3 Dec 2010 10 115 01 3 E Post MUR Page28 3 December 2010 sat Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 1 of 3 https inside mn gov sites MDH bureaus hpb phld
166. e thiosulfate and hydrosulfite Interfere by reducing the blue color or preventing its development Sulfide high levels High concentrations of sulfide may inhibit full color development and require sample dilution Some sulfide loss may occur when the sample is diluted Turbidity For turbid samples prepare a sulfide free blank as follows Use this blank in place of the deionized water blank in the Methylene Blue Method test procedure 1 Measure 25 mL of sample into a 50 mL Erlenmeyer flask 2 Add bromine water by drops with constant swirling until a permanent yellow color just appears 3 Add phenol solution by drops until the yellow color just disappears Use this solution to replace the deionized water in step 2 of the procedure This pretreatment procedure removes sulfide from the sample but the turbidity and any color will remain The interference from turbidity or color will be corrected when the instrument is set to zero with this solution step 9 Sample collection preservation and storage Collect samples in clean plastic or glass bottles Fill completely and cap tightly Prevent excessive shaking or prolonged exposure to air Analyze samples immediately Method performance Precision Sensitivity Program Instrument Standard 95 Confidence Limits of Concentration change Distribution per 0 010 Abs change 690 DR 5000 520 pg L S2 504 536 pg L S2 5ug L S Summary of meth
167. e Last sample number minus the First sample number plus 1 Make note at the bottom of the report of any procedural changes new programs or analysis codes or other important events that took place during the month Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division l Revision Environmental Laboratory dd Effective Date Date of last signature Page 27 of 57 HOLD TIMES LIST TESTS WITH A ONE DAY 24 HOUR HOLD TIME 34 Chromium Hexavalent 54 UV Absorbance 254 nm 55 UV Absorbance 440 nm 302 MPN Total Coliform P 304 MPN Fecal Coliform DW 305 MPN Fecal Coliform P 309 MF Fecal Coliform DW Confirmatory 310 MF Fecal Coliform 311 ME E Coli 312 MF Enterococcus 313 MF Fecal Strep Refrigeration to 4 degrees C is required for these codes and is recommended for all other microbiology samples Enforcement samples for fecal coliform and fecal strep 304 305 309 310 313 must be received within 6 hours of sampling Any deviation from this standard must be okayed by the collector and or the Bactichem lab Make note of it on the comment line when entering initial data All safe drinking water samples DW should be analyzed within 30 hours of collection Any samples older than 30 hours but less than 48 hours will be analyzed and the data flagged as possibly invalid Make note of it on the comment line when entering initial data Minnesota Department of Healt
168. e Period Analyte Data Concentration Units Peak Base Width Inject to Peak Start Chemistry Calibration Data Concentration mg N L Calibration Rep Handling Calibration Fit Type Weighting Method Force through zero Sampler Timing Min Probe in Wash Period Probe in Sample Period Valve Timing Load Period Inject Period Sample Reaches 1 Valve 3 Asp A 7 58 20 0 5 00 17 TABLE DIAGRAMS FLOWCHARTS AND VALIDATION DATA 17 1 DATA SYSTEM PARAMETERS FOR QUIKCHEM 8000 8500 _ The timing values listed below are approximate and will need to be optimized using 40 samples h 90 s sample 35 90 mg N L 42 s 30 8 s Direct Bipolar Lug s ie T ou o 0 40 0 20 0 10 0 05 0 00 2 00 1 00 0 40 0 20 0 00 Average 2 Order Polynomial 1 x No 19s 60 s 30s 60 s 160 s The time it takes the sample to reach the valve needs to be timed for the specific manifold being utilized The time listed is just a starting point The best way to calculate the time to valve is as follows When the sampler probe travels to the sample it will draw up an air slug Start timing when the sampler probe goes into the sample then watch the air slug travel through the heater then out of the UV lamp Once it reaches the debubbler stop timing and add 5 to 10 seconds for the beginning of the sample slug to reach the valve This recorded time with the additional 5 to 10 seconds added
169. e all collected on the same day and the same test is being requested randomly choose a bottle for each sampling point Write the following comment on the data sheet for each sample number involved No ID on bottles randomly chose one bottle for each sampling point Write your initials by the comment so the clerical unit knows they need to enter the comment during secondary entry If you are at all unsure about the samples follow the directions below e If the samples were collected by an EH collector contact the person directly e Ifthe samples were collected by the facility or by a contract collector such as a county that we do not have direct access to contact the appropriate EH Program Representative s Send an email message to the appropriate group of people from the contact list Compare Data Sheets with the Samples Submitted Make sure the field numbers location ID s and sampling points on the forms correspond with the info on the samples If the information does not match Change the data sheet to correspond to the info on the bottles Using a red pen cross out the data sheet info and write in the new info On Lab Comment line write Sampling point altered Determine that the Correct Bottles were Submitted i Check the Analysis codes requested to be sure that all of the correct bottles have been submitted Refer to the bottle type charts to make your determinations If you determine that the wrong bottles have been s
170. e collected from the PTFE tube used to bubble air into the overlying water into polypropylene syringes and filtered for analysis of anions sulfate chloride bromide fluoride via lon Chromatography Sulfate and tracer concentrations will be carefully monitored in the well mixed overlying water during each experimental phase in order to quantify the flux of chemicals into the sediment The way in which a sample is processed preserved stored and transported is determined by the laboratory and specific analytical procedure to be done on the sample See Table 1 for what analyses are to be done on overlying water samples the laboratory to do the analyses and location in the Appendix of the analysis specific sampling requirements as defined in the laboratory s SOP Timing Replicate samples SmL will be collected from each microcosm and filtered approximately weekly during each experimental phase It is expected that two three sulfate flux estimates based on concentrations in the overlying water will possible during each experimental phase in order to quantify the transient changes in response to the treatment Porewater Collection Method Porewater samples will be collected with 5cm long Rhizon filters 0 2 um and 3 mL syringes The Rhizon filters were installed prior to the microcosms being filled with sediment Six filters were installed in a helix pattern around the perimeter of the tubing The goal of this arrangement was to reduce the influen
171. e column is continuously heated at 30 C In general and especially when high sulfide is present samples are filtered with 0 45uM polyethersulfone PES filter membranes and acidified to lt pH 4 5 with concentrated HCl to convert all dissolved sulfide species H2S HS and S2 to H2S which reduces the amount of sulfide available to oxidize to sulfate prior to analysis When chloride analysis is desired the sample is split and analyzed separately for chloride After acidification samples are stored at 4C until analysis Samples are diluted with Millipore water 18 2MQ resistance if necessary and placed in new 5 mL or 0 5mL Dionex polyvials with 20 um pore filter caps and loaded into the autosampler If excessive iron has precipitated out of samples they are re filtered with 0 45 um PES filters A Thermo Scientific Anion Standard is used for preparing calibration standards ongoing recovery checks and matrix spikes Standard Operating Procedure for Analysis of ferrous iron by the phenanthroline method spectrophotometry Johnson Research Group UMD Civil Engineering Updated 4 1 2013 The methods outlined in the Standard Methods for the Analysis of Water and Wastewater Method 4500 Fe D are followed on a Hach DR 5000 UV VIS spectrophotometer Briefly an appropriate volume of reagents HCl Acetate buffer Phenanthroline DI water are added to a clean sample vial to which sample is carefully delivered with a pipette If concentration
172. e is above 80 C is necessary Since the digestion occurs prior to injecting the sample and sin e there is an air segment between the sample and the sampler wash solution the valve and sample timing parameters are critical It is important to verify that center of the sample zone is injected Timing is verified using Universal dye as the Sample The color will be faded by the digestion reagents Red food dye FD amp C 40 can also be used for this as it is decolorized less than the universal dye Flow from sampler Air Sample Slug Portion to inject onto manifold Digestion efficiency should be verified by determining condensed and organic standards at regular intervals If experiencing problems with air bubbles on the peaks change all o rings in the union fittings between heater valve and UV lamp Change the o rings in valve and possibly sample loop if it is crimped Occasionally it has been found 10 115 01 3 E Post MUR Page 12 3 December 2010 sat necessary to increase the backpressure on the outlet of the debubbler using a longer length of 0 022 i d tubing to connect it to port 6 on the valve and or increasing the length of the backpressure coil at port 5 Ifthe membrane begins to weep around the sides the amount of backpressure is too high Condensation at the back of the debubbler is not uncommon 11 3 7 System Maintenance 11 3 7 1 Change PVC pump tubing every three days 11 3 7 2 Change the mem
173. e is available in the QA Office or Element 13 2 Current MDL data are available in the QA Office 13 3 Precision and accuracy data are available in the QA Office or Element NA NA ASLO EOI RIC nc 14 0 POLLUTION PREVENTION 14 1 For information regarding the laboratory s pollution prevention policy and procedures see the current version of the Public Health Laboratory Division Hazardous Waste Manual http fyi health state mn us phl safety index html 14 2 The quantity of chemicals purchased should be based on expected usage during its shelf life space available for storage and disposal cost of unused material Actual reagent preparation volumes should reflect anticipated usage and reagent stability 14 3 For information about pollution prevention that may be applicable to laboratory operations consult Less is Better Laboratory Chemical Management to Waste Reduction available from the American Chemical Society Department of Government Relations and Science Policy 1155 16th Street N W Washington D C 20036 15 0 WASTE MANAGEMENT 15 1 The Public Health Laboratory in carrying out its mission will do so in such a manner as to minimize pollution of the environment and manage its hazardous wastes in a safe and environmentally sound manner The Public Health Laboratory Division shall Conserve natural resources through reduction reclamation recycling Ensure that the Division meets all Federal St
174. e recovery of the repeat analysis also falls outside the control limits the possibility of matrix effects is investigated by analyzing a diluted sample that has been fortified If the recovery of the analyte still falls outside the designated MS recovery range and the BS and ICV CCV for that analyte is shown to be in control the recovery problem encountered with the MS is judged to be matrix induced and the results for the diluted sample and the MS are reported using an elevated report level reflective of the dilution used and the qualifier QD Recovery in MS not within acceptance limits is added to the MS 9 2 7 1 Ifthe MS recovery of the diluted sample is within acceptable limits the sample is reported with an elevated Report Level reflective of the dilution used 9 2 10 Precision Analyze a laboratory duplicate DUP with each batch of field samples processed as a group or10 of the field samples analyzed whichever is greater Calculations of the Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 16 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc 9 absolute difference between the duplicates and the relative percent difference RPD between the duplicates are used to monitor the precisio
175. e system you need a new standard calibration for a new run iii Use 296 HNO3 to dilute the stock and make standard solution As a stock solution contains multiple elements that are of interest in your sample multiple calibrations for different elements can be create at the same time given that the appropriate concentration settings in each step of standards for each element is well defined Table 1 and 2 below are examples to prepare calibration solutions for both low and high concentrations 11 iv V The target concentrations of the elements in each standard solution were calculated based on one specific element e g concentration of Ag is used as base in this example to calculate concentrations for other elements set up a spreadsheet to quickly calculate the corresponding element concentrations for each level of standard solution This information is necessary to fill in the Method file A spreadsheet is also helpful on calculating the volume of stock solution and 2 HNO3 for making standard solutions Table 3 and 4 are examples for it The calculation is based on the concentration of Ca Table 1 Example of standard concentration for multiple elements High concentration Target Concentration ppb Flements Original Sidi std2 std3 std4 stds std6 Ca 10000 40 100 300 750 1700 5000 Mg 10000 40 100 300 750 1700 5000 Na 50000 200 500 1500 3
176. e used Standardized 0 0250 N Iodine Solution Purchased commercially Standardized 0 0250 N Sodium Thiosulfate Titrant Purchased commercially Starch Indicator Solution 2 w v Purchased commercially Degassing with Helium To help prevent bubble formation reagent water used to make reagents should be degassed Use 20 Ib in through a helium degassing wand Bubble He through the reagent water for at least 10 minutes Hydrochloric Acid 3 M In an acid rinsed 1 L volumetric flask add 600 mL of degassed reagent water then slowly add 248 mL of concentrated hydrochloric acid HCI Dilute to 1 L with degassed reagent water Prepare fresh monthly Hydrochloric Acid 0 20 M In an acid rinsed 1 L volumetric flask add 700 mL of degassed reagent water then add 16 5 mL of concentrated hydrochloric acid HCD Dilute to 1 L with degassed reagent water Sodium Hydroxide 0 025 M In an acid rinsed 2 L volumetric flask add 2 g of sodium hydroxide NaOH to approximately 800 ml of degassed reagent water Stir until dissolved Dilute to volume with degassed reagent water Prepare fresh daily This reagent is used for standards diluent and carrier reagent Remake 2 L portions as needed N N Dimethyl p phenylenediamine Reagent In an acid rinsed 1 L volumetric flask dissolve 1 0 g N N Dimethyl p phenylenediamine Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 201
177. e wrap the filter or group of filters in foil Place another label with sample number only on the foil For a group of samples use a label from the first and last numbers only it is not necessary to put a label from each number on the foil Clip all of the labels from one group together and save them for delivery to the lab Total Ortho Phosphate samples These samples are collected by community systems on behalf of Environmental Health They are collected in an unpreserved nutrient bottle Put the Total Phosphorus label on the bottle as normal For the Ortho label peel back 1 3 of the backing and stick it to the cap Multiple program samples Occasionally the MPCA will submit samples that they want analyzed under two different programs The sheets are given separate numbers and the labels are attached similarly to phosphate samples One programs label on the side of the bottles and one on the top Metals bottles Place the entire label on the bottle Peel off one label with just the sample number and place on top of the bottle cap The metals lab holds samples for several months Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division l Revision Environmental Laboratory l Effective Date Date of last signature Page 40 of 57 o Having the numbers visible from the top makes it easier for them to find samples on their carts Organics bottles Place one small label with the sample number and test c
178. eactions that are specific for the orthophosphate PO ion The applicable range is 10 to 500 ug P L The statistically determined method detection limit is 1 4 ug P L The method throughput is 32 injections per hour 2 SUMMARY OF METHOD 2 1 22 The method is based on the digestion of various phosphorous forms to phosphate by peroxodisulfate with an on line UV digestion Organic phosphorus is converted to orthophosphate by persulfate digestion catalyzed by UV light Polyphosphates are converted to orthophosphate by sulfuric acid digestion The digestion process occurs prior to the sample valve A portion of the digested sample is then injected and or the phosphates determined by FIA The orthophosphate ion PO reacts with ammonium molybdate and antimony potassium tartrate under acidic conditions to form a complex This complex is reduced with ascorbic acid to form a blue complex which absorbs light at 880 nm The absorbance is proportional to the concentration of orthophosphate in the sample 3 DEFINITIONS 3l 32 3 3 3 4 CALIBRATION BLANK CB A volume of reagent water in the same matrix as the calibration standards but without the analyte CALIBRATION STANDARD CAL A solution prepared from the primary dilution standard solution or stock standard solutions The CAL solutions are used to calibrate the instrument response with respect to analyte concentration INSTRUMENT PERFORMANCE CHECK SOLUTION IPC
179. ealth Laboratory Division i Revision Environmental Laboratory Effective Date Date of last signature Page 33 of 57 e ENVIRONMENTAL HEALTH DATA SHEETS MDH DATA SHEET This type of data sheet is used to submit most samples collected for the Environmental Health Public Water Supply Unit l The following is a description of each section of the form 1 Program Code This is used for billing purposes 2 PWS ID This is required for all samples submitted for Environmental Health Public Water Supply samples If there is no PWS on the form you can look it up on the computer through Lab Review 3 Facility Name If no facility name is given you may look it up on the computer by using the PWS ID through Lab Review 4 City Town Township These can be looked up via the same method as the Facility Name 5 Date Collected This information is essential because we must know if the sample is valid e See section on Basic Sample Processing for instructions on handling samples that are submitted without collection dates 6 Time Collected This information is important for samples with short hold times 7 Collector ID and Collector Name The collector should fill in this information 8 Original Sample Number and Field Blank Number These fields are not necessary to process samples 9 Sample type If this information is missing do not choose a type unless you are absolutely sure of the correct one EH personnel will make corrections
180. eam OSTCWAMathocs Depa Gav ca Lenraiol Walken OWA ATP consdinatar Steve Wendelken SOWA AUP courdinater iiteTatAdbess MAL Espz wewepa gue Bory sted Hie ychobie o Parteja Ih Vectra OI Riut hs en Fick Paper erem yes Dod mem Section No Appendix D Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 43 of 44 Appendix D University of Minnesota Civil Engineering Laboratory QA Procedures and Standard Operating Procedures Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan UMD Civil Engineering QA Procedures Quality Assurance Quality Control QA QC procedures for Johnson Research Group N Johnson Updated 9 19 12 In order to ensure the quality of analytical data from a variety of techniques used to quantify chemicals in our lab this document lays out procedures for how to ensure that the analytical equipment is giving consistent results and functioning as we expect for samples These guidelines apply to Anions and cations by lon Chromatograph Ferrous iron by phenanthroline method Sulfide by ISE Sulfide by methylene blue spectrophotometric method Metals by ICP MS Sulfate by turbidometric method pH amp ORP by electrodes DOConTOC analyzer Total elemental analysis on CHNS analyzer The principle of QA QC is to run checks with the instrument at the beginning and periodically throughout the samples to ensure that
181. easuring pH with a glass pH electrode Samples were homogenized in the oxygen free atmosphere and a representative subsample was removed to measure water content as an estimate of porosity Rhizon filters 0 2 um polyethersulfone were used to collect approximately 35 mL of water from composite sections into polypropylene syringes The filters syringes were left overnight to collect sample and filled completely A quantitative volume 10 mL by mass of filtered water sample was transferred into 20 mL glass serum bottles preloaded with Zinc Acetate 20 uL of 1 M ZnAc and Sodium Hydroxide 100 uL of 0 6 N NaOH in the oxygen free atmosphere for sulfide analysis Of the remaining filtered pore water 2 5 mL was used to quantify ferrous iron phenanthroline method and 10 15 mL was stored at 4 C until analysis for sulfate and other anions by lon Chromatography Microcosm Preparation Sediment handling Within 3 weeks of collection bulk sediments from each site were composited while attempting to minimize oxidation Large plant material gt 3 length 2 mm diameter was removed by pouring aliquots of the material into a plastic bin picking any large articles by hand then gently raking with a garden rake to remove smaller plant material and begin to homogenize the sediment The final mixing was completed by compositing all material from a site into a rubber garbage can and using a paint mixer attached to an electric drill at low RPM to gently fold
182. eat variety of samples from numerous locations around the state They submit water samples from lakes streams rivers feedlot run off closed landfill monitoring wells drinking water rarely Superfund sites etc They also submit sediment soil sludge fish filters paint and other samples They collect some samples on a routine basis for monitoring purposes In other cases they respond to complaints spills fish kills or other crises gt The MPCA submits most of the high priority and Chain of Custody samples that we receive They also submit most of our sediment soil fish sludge and paint samples Shipping Protocol Most MPCA samples are transported shipped on ice incoolers because they are supposed to be maintained at a temperature of 4 degrees Celsius or less The temperature needs to be checked and noted when the samples arrive Program Codes The MPCA uses over 50 different MDH pga Codes There are a few that are used for routine samples but many that are specialized It is nearly impossible for us to determine the correct code if it is not provided by the collector The routine codes are as follows Q o MPCA 23 EOD Lake Monitoring PG MPCA 27 EOD Routines QW MPCA Closed Landfill Assessment MPCA SAMPLE PROCESSING PROCEDURE The MPCA courier delivers most of the samples we receive from them Samples may be delivered by other courier services depending on where they are coming from Open coolers and boxes carefully Y
183. ecovery sample Three samples Duplicate sample s Four samples A method blank Matrix spike matrix spike duplicate Five samples Ongoing Precision Recovery sample Four samples Method spike An analytical blank Seven samples Ongoing precision recovery An analytical blank Although the above sequence involves 48 analytical runs for only 30 samples the quality of the data will be much higher if these QA guidelines are followed and results can be reported with confidence A typical analytical sequence for a matrix that we have tested before and had reliable results for matrix spikes could leave out matrix spikes If OPR results consistently come out within 1096 of expected values over a period of months of performing analysis subsequent batches of samples run on the same instrument can proceed without a full calibration but maintaining blanks and OPR checks Sulfide DOC316 53 01136 USEPA Methylene Blue Method Method 8131 5 to 800 ug L Scope and Application For testing total sulfides H2S HS7 and certain metal sulfides in groundwater wastewater brines and seawater 1 USEPA approved for reporting wastewater analysis Procedure is equivalent to Standard Method 4500 S D 2 Adapted from Standard Methods for the Examination of Water and Wastewater Test preparation How to use instrument specific information The nstrument specific information table displays requirements that may va
184. ect Management Elements eee ener en nennen nete t nennen nre nenne enne een 2 Section A SEP eL Sii 2 Section A 1 Approvals Continued sese neee trente enne cn nena rennen ener 3 Section A 2 Table of Contents eerte ere tere ten a Rex rep SE baee me ER TERRE aba eee E eR HP ek epe ire eds 5 Section A 3 Distribution Last tete tire ttene EE EEEE EPEE hepate nde en ek ee ee Eee ebore eden 8 Section A 4 Project Organization and Responsibility eese enne 9 Section A 4 1 UMD Work Order Coordinator Nathan Johnson Ph D ocoooonnnnnnnnononononcnnncncncnnnnnnnnos 9 Section A 4 2 Graduate Researcher Will Derocher eese enne 9 Section A 4 3 The University of Minnesota Duluth Principal Investigator John Pastor Ph D 9 Section A 4 4 The MPCA Division Manager Shannon Lotthammer ooooccnoncnccnnonnnonnnoncnnanonoronono nono nonononos 9 Section A 4 5 The MPCA Project Manager Edward Swain Ph D see 10 Section A 4 6 The MPCA Contract Manager Patricia Engelking eee 10 Section A 4 6 MPCA QA Coordinator William Scruton eese enn 10 Section A 4 7 MDH Inorganic Unit Supervisor Jeff Brenner 00 0 eee eee eeeeeeeeeeeeeseeeeenseenaeenaes 11 Section A 4 8 MDH Public Health Laboratory Manager Paul Moyer sese 11 S
185. ect Manager Quality Assurance Coordinator Quality Assurance Officer Quality Assurance Manual Quality Assurance Project Plan Quality Assurance Quality Control Quality Management Plan Relative Standard Deviation Relative Percent Difference Sampling and Analysis Plan Standard Operating Procedure Sample Receipt Form University of Minnesota Duluth University of Minnesota Twin Cities Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No Appendix B Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 41 of 44 Appendix B MDH Environmental Laboratory QA Manuals Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 1 of 67 http fyi health state mn us phl environmental index htm DEPARTMENTOFHEALTH Quality Assurance Manual for the Environmental Laboratory Testing Units Public Health Laboratory Division Minnesota Department of Health 601 Robert Street North P O Box 64899 St Paul Minnesota 55164 0899 Revision Record Updated content due to change in lab S Drier 10 06 2006 location New QA officer Included revision l history Enhanced QC definitions Section 2 0 K Peacock Enhanc
186. ection A 4 9 MDH QA Officer Shane Olund esses eene enne enne nennen nnns 11 Section A 4 10 MDH Laboratory Staff ooooonnncinnnicnnnonnonnconnconoconoco nono nono nono nono ncnn nro nrnn arc n nan nn trennen nennen 11 Section A 4 11 University of Minnesota LacCore LRC Laboratory Manager Amy Myrbo Ph D 11 Section A 5 Definition Background sessi nono nono esis rees tene tren trennen trennen enne 13 Section A 6 Project DescprptioDs e eene stie Eod reni toe EE rr dpa eS o eire bern es Fonte ida iii 14 Section oS E R RER 14 Section A 6 2 SCOPE into tesis ire eite deberes estes be ebd pe dee aee rece t eae tidie desee deet estet e epe pde 14 Section A 6 3 Analytical Samples civic esiti erien aeee ENEE EE Deidad ii 14 Section A 6 4 Intended Data Usage sees neret enne ennt tene trennen trennen nennen 16 Section A 6 5 Technical Repotts ue eee eee ei deti e rt ee be ede etre Een 16 Section A 7 Quality Assurance Objectives and CritOlla ooocnnnnocnnonnconnconccononnonononn nono nnnonnn nono nennen 16 Section MES ul ET 16 Section A72 LIE pes 17 Section A 7 3 Duphcate Samples iii iii 17 Section A 7 4 Matrix Spike and Laboratory Control Samples sse 18 Section A 7 5 Laboratory Activities c ccccciseiscsesenscedesessesnessastinnsonssonesonscesecersoteecsosbseshsossnedsensensesesSenseapacis 18 Sectio
187. ed Signs and Symptoms of Exposure Any irritation or burning of the eyes skin or respiratory system or violent gastroenteritis Medical Conditions Aggravated by exposure Pre existing skin disease or respiratory disorder Compound Specific PPE Wear nitrile gloves safety goggles or face mask and lab coat when pouring anode solution in calibration cell Storage Store in tightly closed container away from heat or flame Storage area should be well ventilated Store away from strong bases Disposal Dispose of by means in compliance with all State Local and Federal Regulations Methanol Acute Effects Hazardous in case of skin contacts irritant ifingested inhaled or ifin contact with eyes Slightly hazardous in case of skin contact permeator Severe over exposure can result in death Chronic Effects Prolonged contact with skin can cause dermatitis or aggravate existing skin problems Methanol is readily absorbed into the body following inhalation and ingestion Skin absorption may occur if the skin is broken or exposure is prolonged Once absorbed methanol is rapidly distributed to body tissues Compound Specific PPE All sample prep work that involves methanol should be conducted in a fume hood while wearing a lab coat goggles and nitrile gloves Storage Store in a segregated and approved area Keep container in a cool well ventilated area Keep container tightly closed and sealed until ready for use Avoid all poss
188. ed QC policies and procedures L Liao 99102209 Section 13 0 Minor edits throughout Interim QA Officer Enhanced QC definitions Section 2 0 Organizational changes Section 3 0 Enhanced chain of custody procedures Suzanne Section 8 0 Enhanced data reduction and Skorich rd validation procedures Section 14 0 Enhanced system audits Section 15 0 Updated certificates and forms Section 17 0 Minor edits throughout Organizational changes Section 3 0 Description of Promium Element LIMS Detail for system audits Section 15 0 Minor edits throughout Susan Wyatt 09 26 2011 CONTROLLED DISTRIBUTION COPY 1of1 ISSUED TO PHLD Intranet Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 2 of 67 http fyi health state mn us phl environmental index html Quality Assurance Manual Revision 9 Written Revised By s Susan Wyatt for quality manager Date 09 29 2011 Susan Wyatt Environmental Laboratory Accreditation Program Manager Approved By s Paul Moyer Date 09 29 2011 Paul Moyer Environmental Laboratory Section Manager Approved By s Joanne Bartkus Date 09 29 2011 Joanne Bartkus Public Health Laboratory Director Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revisi
189. ed column below BACTICHEM Hold Time c BACTICHEM Hold Time MDH A C Plastic Genaral Bottio Plastic Sulferic Acid Bottle Alkalinity Total 4 Le TT carton Dissolved ore G8 69 1 ee E BOD 5Day 2L dortio 48 hr 096 L Carbon Total Org Q8 os T 11 CBOD SDay 2 Bortle 48 hr 083 con Temps few Chloride ToniQ8d 397 Ammonia Nitrogen Total 28 4 064 A AA NOg Tai sD os l Chlorophyil a Lab Filter 38h 452 __ Ejeldabl Nitrogen Tots 28 d 068 Nitrite Nitrogen Tol 48t 067 Phosphorus TouQsc ess pHLab Immediste 013 e e ee Solids Susp Volatile 7d 004 _ Paso Sterile Bottle Solids Total Dissolved 7d 005 2eormnocsn o o o o 335 Solids Total Sup 74 Lw T AA AS UA HEU HERES Rp ERN Solids Total Volstile 7 d J 002 __ METALS Hold Time MDH A B C D E Solids Ton 7d on e Pise Nae Acid Bolo Ae o Le Wee Sul ste SO T d Caicium CaCO 180 d 2313 jio Tomaso 152 _ Pomssinm Tomlcisod 258 Y __ sodium To 80 257 2 MDH A B C D E Cilorophyttc Field Fiter 7d 450 Y MDH Copy See Back for Analysis Groups Project Codes and Chain of Custody talk revised 04 09
190. eet to ensure quick entry 9 The Sample Receiving copy is kept in the file folder on the overhead shelf The most recent should be put in the front of the folder Maximum Analytical Times Priority Options Chart Priority 3 l Priority 1 Emergency M Water Soil Sed Water Soil Water Bactichem Bacti only 2 days 2 days 24 36 hours General Chem 21 days 25 days 7 days 72 hours Metals 21 days 21 days 5 days 48 hours Organics Volatiles 2 days 21 days 3 days 24 hours Non volatiles 21 days 25 days 5 days 48 72 hours Radiation 25 days 25 days 7 days 72 hours Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 23 of 57 SPECIAL SAMPLE HANDLING ORGANICS SAMPLES e Make a copy of lab sheets for all VOC samples not collected by EH as part of regular monitoring This includes samples from MPCA and any other special projects The copy is placed in the basket in the VOC room Make a copy of lab sheets for all PFOS PFOA samples and place it on the desk of Yongyi Julia Jiang e Make a copy of lab sheets for Organics samples other than routine samples collected by EH analyses 407 408 409 and 415 The copy can be go P aed to the appropriate analyst or placed with the samples in the cooler BACTI CHEM SAMPLES e Make a copy of lab sheets for all bacteriological samples other than 327s an
191. eme See Section 17 11 4 5 Add approximately 5 mL of each properly preserved and prepared sample filter blank or sample aliquot diluted to 5 mL into corresponding 10 mL borosilicate test tubes and place in sample tray Set up 1 DUP for every 10 samples and a BS and MS for every 20 samples 11 4 5 1 After preservation and preparation samples must be extracted from glass bottles using safety lock syringes Discard locked syringe and needle in sharps container 11 4 6 Calibrate the instrument by injecting standards The data system will then associate the concentrations with the instrument responses for each standard and evaluate the curve 11 4 7 After acceptable curve is achieved and initial QC is obtained and acceptable continue with analysis 11 5 System Shut Down 11 5 1 At the end of the run place all reagent lines into water to rinse for 15 minutes Pump air through the manifold for 30 minutes to dry the distillation system especially the membrane Keep the heater at 65 C until 30 minutes of air drying is complete 11 5 2 Turn off the pump and the power strip Release the tension levers on the pump tube cassettes 11 6 System and Procedure Notes 11 6 1 For information on system maintenance and troubleshooting refer to the Troubleshooting Guide in the System Operation Manual Guide is also available on request from Lachat Consult the Instrument Book for the Lachat systems for current information on preventative maintenan
192. ent of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 55 of 67 http fyi health state mn us phl environmental index html 11 Calculate the mean of the results of the MDL standard and the average recovery Percent recovery of the replicates should be reasonable for that analyte but no universal criteria for percent recovery have been established 12 Calculate the standard deviation for n 1 and enter that value 13 Select the Student s t value corresponding to the number of replicates or n done automatically if using the MDL calc spreadsheet 14 Multiply the Student s t value x the Standard Deviation to get the MDL value 15 Divide the True Value of your MDL Standard by the calculated MDL and enter that result 16 Then answer the questions shown 17 As a guideline the following criteria should be met for an acceptable MDL study 1 The true value TV of the standard should be within the range of 1 to 10 times the calculated MDL If the calculated MDL is greater than the TV of the standard TV MDL 1 the MDL study should be repeated with a standard of higher concentration If the TV is greater than 10 times the MDL TV MDL gt 10 the MDL should be repeated with a standard of lower concentration unless the TV is already equal to or smaller than the RL TV lt RL then it is not necessary to repeat
193. ents of an Initial Demonstration of Capability are as follows 1 Initial Calibration Perform an initial calibration using standards that will bracket the range of concentration found in samples and that will define the working range of the instrument analysis Enough standards must be used to show that the curve is linear or to clearly define any area s of the curve that may be nonlinear 2 External Verification of Calibration A quality control sample QCS from an external source is analyzed The results of the QCS must be within acceptable limits otherwise remedial action is taken and the entire IDC is repeated 3 Initial Precision and Accuracy Analyze four reagent blanks spiked at the concentration of the calibration check standard or mid range standard Calculate the mean concentration and the standard deviation of the set The percent recovery and the percent relative standard deviation RSD must meet the criteria established in the SOP 4 Demonstration of Low Background Analyze at least one Laboratory Reagent Blank LRB to determine reagent or laboratory contamination The LRB result must meet the criteria established in the SOP for on going demonstration of low background Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 58 of 67 http fyi health state mn us phl environmental
194. env inorganics Gen Chem SOPs gen26 doc NUMBER REVISOR Dane 03 23 13 This is the first release for a controlled Huber standardized format for General Chemistry PROCEDURE FOR THE DETERMINATION OF DISSOLVED SULFIDE IN WATER AND SOIL WITH INLINE DISTILLATION BY FLOW INJECTION ANALYSIS COLORIMETRY Sulfide amp Acid Volatile Sulfide Table of Contents Section Page 1 0 SCOPE AND APPLICATION cccccccccsssccsccssseveoscsscccesevassvasessnsvatcsssessesssecseessnenseeses 2 2 0 SUMMARY OF METHOD eerte Peer ava go vui d Vea eoe veh Versu rende 2 3 0 DEFINITIONS A OM m 3 4 0 INTERBERENTGCES 5 2 3 2 nro ira E Sea Oe ey ux 3 5 0 SABEEY audeo dtd tu rebat ute deat nase 3 6 0 EQUIPMENT AND SUPPLIES siesta axe knee rne deo kno eva Petar kn rre e 4 7 0 REAGENTS AND STANDARDS GG cierre rera reete ntes eerie teniente en 6 8 0 SAMPLE COLLECTION PRESERVATION SHIPMENT AND STORAGE 10 9 0 QUALITY CONTROL eder titii Elsa uri rk aci 11 10 0 CALIBRATION AND STANDARDIZATION ccccccccscsscrcescscessesrscerecessnteeseas 17 PEO PROCEDURE 000 ects reset eles od ial ads a 19 12 0 DATA ANALYSIS AND CALCULATIONS 0e eterne eene nennen 22 13 0 PERFORMANCE aeiiaaie tota o vias cry o evi Pea su yo Vau aen ou dE de aea ae Sog ao Cis a a Use 23 14 0 POLLUTION PREVENTION eese eren ren tenerent nennen annee raten 23 15 0 WASTE MANAGEMILENT eese nannte
195. er to tee fitting 1 The white pump tube is cut 2 cm outside of the tabs on both sides The outlet of the sample pump tube is connected to tee snes i with 50 cm a 0 8 mm id manifold tubing 10 107 04 3 D Page26 2 Dec 2010 sat Note 4 Note 5 Note 6 Note 7 Note 8 Note 9 _Note 10 Note 11 10 107 04 3 D Persulfate red and borate orange pump tubes are connected to tees 1 and 2 with 50 cm lengths of 0 8 mm id manifold tubing The Debubbler is mounted on the manifold board near the valve Replacement membranes are part number 85363 To install unit Cut tubing with 2 nuts in half Screw half into each port on the PEEK body These are the inlet and outlet of the unit Please note that condensation may form at the outlet of this debubbler A truly failed membrane will leak around the edge of the disc not only through these ports If needed 50 or 100 cm of 0 022 i d tubing can be added at the outlet of the debubbler connected to Port 6 of the valve The 100 cm back pressure loop is 0 5 mm 0 022in i i d tubing The 200 cm back pressure loop is 0 5 mm 0 022 in i d tubing PVC PUMP TUBES MUST BE USED FOR THIS METHOD Heater inside of the sample prep module 1200 cm of 0 032 i s manifold tubing tubing is wrapped on a high temperature heater with 90 cm remaining for connection at the inlet and outlet 1380 cm total length The outlet of tee 1 is connected to the heater inlet
196. erature blank bottle that is kept in the cooler with the samples see background information It is most important to record the temperature information for bacteriology BOD and Organic sampi but we should record it for all types of samples The MPCA courier takes and records the temperature for the samples he brings in and most other MPCA collectors do this for their own samples as well If there is no temperature blank use a general bottle be sure to clean the thermometer thoroughly first If there is no general bottle you may use water that has pooled in the bottom of the cooler If there is no pooled water but the samples are on ice or freezer packs record the comment no temperature blank but samples on ice on the data sheet If the samples are not on ice record the comment no temperature blank samples not on ice If there is ice IN a sample also make note of this CHECKING DATA SHEETS AND COMPARING THEM TO THE SAMPLE CONTAINERS Make sure there is a Program Billing Code on the Data Sheet We cannot enter any information in the computer without a program code If there is no code contact the collector or the report to person listed on the data sheet If you are unable to obtain the information before the samples must be submitted for testing choose the code that seems most appropriate Refer to the Chemistry Lab Handbook and background information in this section to aid you The code can be changed once you
197. erified by determining non nitrate standards at regular intervals A good plan is to use urea and nicotinic acid Urea recovery 10 107 04 3 D Page 12 7 2 Dec 2010 sat 11 3 6 11 3 7 11 3 8 11 3 9 goes down when the digestion is too rigorous and nicotinic acid requires optimal functioning of all digestion parameters for recovery 79594 To prevent ammonium contamination during system start up and shut down use a separate wash vessel dedicated to the ammonium chloride buffer It is advisable to periodically determine a nitrite standard to check column efficiency If column efficiency is 9096 replace the column System Maintenance for best results 11 3 8 1 Change PVC tubing every three days 11 3 8 2 Change tubular membrane of debubbler every two days The membranes in the alternate debubbler are changed only as required and may last 3 4 weeks or more 11 3 8 3 Change cadmium column every 200 samples Check list before running real samples 11 3 9 1 Check that the method s timing has been correctly set by running food dye bypass cadmium column at this time 11 3 9 2 Check the temperature of digestion module 105 for TN and 125 for TP 11 3 9 3 Check that all reagents are prepared correctly to ensure there is no l precipitation in the digestion buffer solution 11 3 9 4 Check that the debubbler is in good condition and it is efficiently debubbling by running one duplicate standard Cadmium colum
198. erved samples have a holding time of 28 days Samples may be homogenized or sonicated in a device designed for this purpose However turbid samples should be filtered since the digestion effectiveness on samples containing particles is unknown 9 QUALITY CONTROL 9 1 Each laboratory using this method is required to operate a formal quality control QC program The minimum requirements of this program consist of an initial demonstration of laboratory capability and the periodic analysis of laboratory reagent blanks fortified blanks and other laboratory solutions as a continuing check on performance The laboratory is required to maintain performance records that define the quality of the data that are generated An analytical batch shall be defined as environmental samples that are analyzed together with the same method and personnel using the same lots of reagents not to exceed the analysis of 20 environmental samples 9 2 9 1 1 Analyses of matrix spike and matrix spike duplicate samples are required to demonstrate method accuracy and precision and to monitor matrix interferences interferences caused by the sample matrix The procedure and QC criteria for spiking are described in section 9 3 9 1 2 Analyses of laboratory blanks are r quired to demonstrate freedom from contamination 9 1 3 The laboratory shall on an ongoing basis demonstrate through calibration verification and analysis of the ongoing precision and recovery
199. ery hazardous samples which are then returned to the site or lab packed for disposal at an appropriate facility Section B 4 Analytical Methods Information on the analytical methods to be used in this experiment is detailed in Tables 1 2 and 3 Their corresponding analytical methods and SOPs are identified by laboratory and their location in the Appendix of this QAPP Corrective actions taken in the process of microcosm sampling and analyzing samples are documented by the laboratory managers or staff and are ultimately reported to Dr Johnson and the appropriate MPCA Project management staff for the final decision Wild Rice Sulfate Standard Sediment Incubation Experiment Ouality Assurance Project Plan Section No B 5 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 29 of 44 Section B 5 Quality Control Laboratory QC checks are identified in Table 2 The frequency of analysis and the control limits are also listed If the results don t meet the QC acceptance criteria corrective actions are defined Section B 5 1 QC Types Table 4 Quality Control Elements QC Type Surface Water Porewater Sediment Blanks Method Blanks 1 per batch 1 per batch 1 per batch Spikes Laboratory Control Sample LCS 1 per batch 1 per batch 1 per batch Matrix Spike MS 1 per batch 1 per batch 1 per batch Calibration
200. es draw a line along the log list to indicate to Clerical staff that the log has been verified 5 If there are any errors make changes using the edit screens and note the changes on the log list If any analysis codes were entered incorrectly it is necessary to reprint the corrected labels Find the sample bottles in the lab and attach the correct labels 6 When you are finished paper clip the log list on top of the stack of lab sheets and deliver it to e clerical There is a basket for incoming work in the filing room Minnesota Department of Health ET Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 41 of 57 8 DELIVERING SAMPLES TO THE LABORATORY Deliver samples with short hold times first and notify lab personnel It may be helpful to load samples onto the transport cart in the same order that they will be needed in the labs Refer to the following descriptions for the correct ordering method Refer to the Labs Map South for the following sample delivery locations C of C Room All Chain of Custody Samples must go in the locked cooler in this room The C of C log book is also located here 1 Place radon samples in racks on this counter 2 Place all other radiation chemistry samples on this lab counter and put extra labels in the basket If it is late in the day and no one is in the radiation area put milk crop
201. es for the target analytes are a measure of accuracy while the Relative Percent Difference RPD between the LCS LCSD measures is a measure of precision It is also known as a Laboratory Fortified Blank Duplicate LFBD Laboratory Duplicates LD1 and LD2 Two aliquots taken from a single sample container in the laboratory and analyzed separately using identical procedures Analysis of LD1 and LD2 indicates precision associated with laboratory procedures for a specific sample matrix but not with sample collection preservation or storage procedures Laboratory Fortified Blank LFB See Laboratory Control Sample LCS Laboratory Fortified Blank Duplicate LFBD See Laboratory Control Sample Duplicate LCSD Laboratory Fortified Matrix LFM See Matrix Spike MS Laboratory Fortified Matrix Duplicate LFMD See Matrix Spike Duplicate MSD Laboratory Reagent Blank LRB See Method Blank MB Linear Calibration Range LCR The concentration range as determined by the analysis of calibration standards over which the calibration curve is linear Linear Dynamic Range LDR The concentration range over which the instrument response is linear The LDR may extend beyond the calibration range A LDR study is required to confirm the validity of reporting data beyond the calibration range Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9
202. es have been submitted In all cases above check with the laboratory before submitting the sample and record a receiving comment that briefly describes the bottle substitution Bacteriology samples must be submitted in a sterile bottle preferably our own Colilert Thiosulfate or Non Thiosulfate bottles Occasionally a collector may submit a bacteriology sample in their own sterile bottle and this is usually acceptable but check with the laboratory before submitting MPCA collectors rarely request code 327 The bacteriology codes they most commonly request are 310 fecal coliform and 311 fecal strep If the bottle submission problem cannot be resolved Notify the collector or report to person via phone or email List the analyses that cannot be run and why l If some of the analyses can still be run cross out the codes that will not be run Make note of the cancelled analyses and the date the collector was notified on the data sheet MPCA SAMPLE SIGN IN PROCEDURE SEE EXAMPLE OF DATA SHEET Most MPCA Data Sheets must be signed like a chain of custody form even when the samples are not officially chain of custody They use the following forms Standard MPCA form for water Standard MPCA form for sediment MPCA chain of custody form MDH chain of custody form MDH Organics Data Sheet Forms from MPCA sub contractors The most common sub contractors are Interpoll Labs Conestoga Rover and Foth amp Van Dyke the facilities th
203. est Matrix spikes The laboratory must spike in duplicate a minimum of 5 percent of all samples one sample in each batch of no more than twenty samples from a given sampling site or if for compliance monitoring from a given discharge The two sample aliquots shall be spiked with the stock standard section 7 2 l 9 3 2 9 3 1 1 9 3 1 2 9 3 1 The concentration of the spike in the sample shall be determined as follows If as in compliance monitoring the concentration of the analyte in the sample is being checked against a regulatory concentration limit the spiking level shall be at that limit or at 1 to 5 times higher than the background concentration of the sample determined in Section 9 3 2 whichever is higher If the concentration of the analyte in a sample is not being checked against a limit the spike shall be at the concentration of the precision and recovery standard used in Section 9 2 5 or at 1 to 5 times higher than the background concentration whichever concentration is higher Analyze one sample aliquot out of each set of no more than twenty samples from each site or discharge according to the procedure beginning in Section 11 to determine the background concentration of B of the analyte 9 3 2 1 9 3 22 If necessary prepare a standard solution appropriate to produce a level in the sample at the regulatory compliance limit or at 1 to 5 times the background concentrati n per Section 9 3 1 Sp
204. est forms a k a chain of custody forms examples 45 46 Chain of custody form for form for receipt of samples including those 47 subject to criminal or civil custody Chain of custody logbook page to internally track enforcement samples 48 Equipment maintenance logs examples 49 50 Policy and procedure for Detection Level Study 51 52 Method Detection Limit MDL single analyte worksheet MDL worksheet 53 56 instructions Policy and procedure for Initial Demonstration of Capability IDC Study 57 58 Policy and procedure for Report Level Verification 59 60 USEPA Enclosure A Laboratory Certification Summary Minnesota 61 64 Department of Health May 5 7 2008 Corrective action form for non conforming work 65 66 Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 6 of 67 http fyi health state mn us phl environmental index htmi SECTION 1 0 LIST OF ACRONYMS The list of acronyms herein is limited to terms that are used in this Quality Assurance Manual outside of those listed in Section 2 0 Definitions of QC Terms The reader is directed to Section 2 0 for acronyms that correspond to various QC terms adopted by this laboratory and used in this Quality Assurance Manual CFR Code of Federal Regulations CWA Clean Water Act LIMS Laboratory Information Management System
205. ev x Student s t t7 3 143 QAO Comments t8 2 998 t9 2 896 t10 2 821 t11 2 765 t12 2 718 Report Level True Value TV Number of Points Mean Recovery Std Dev n 1 Student s t MDL TV MDL TV MDL between 1 and 10 Is MDL s RL TVS RL Approved by QAO MDL Study entered Init 8 date init 8 date Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 54 of 67 http fyi health state mn us phl environmental index html 10 MDL Single Analyte Worksheet Instructions prepared by Keith Peacock 2 23 07 These instructions are applicable to the single analyte MDL worksheet There are two forms of this worksheet 1 a blank form that the analyst can generate and then fill in by hand and 2 a form that has all of the calculations built into the spreadsheet and designed to be completed electronically These worksheets should not be used for multi analyte analyses In the upper right hand corner of the MDL worksheet enter the target analyte MDH LIMS code and the date you are submitting the worksheet to the QA Office Also indicate if this is the first second or third study for the same analyte that is being submitted within a 3 month period For analyst use your LIMS name Analytical method refers to the reference method for the applicable SOP If the
206. evels also automatically adds a surcharge to the sample analyses The maximum analysis time for a given test at each priority level varies Refer to the chart at the end of this section for more information There are four priority levels Priority 3 This is the routine priority level and is used for most samples This priority level defaults in upon initial entry of sample data Priority 2 This priority level was used for some of the bottle blanks prepared by laboratory and laboratory services personnel We do not currently use this priority level Priority 1 This is the priority level that submitters usually want when they request a faster turn around on samples Most Priority 1 requests come from the PCA but occasionally EH will ask for this priority as well Priority 1 samples are assessed a50 surcharge because they require special handling Priority 0 Emergency This is the highest priority level and usually is requested after consultation with the lab A 150 surcharge is assessed if samples are accepted and analyzed during business hours A 200 surcharge is assessed if samples are accepted and analysis is begun during non business hours PRIORITY SAMPLE PROCEDURE A request for expedited sample analysis should be made in writing This can be written directly on the lab request or C of C form or in a separate email letter or fax The memo should list all of the analysis codes that the submitter wants run at the high priority sta
207. ew and improvement in operations The audit concentrates on the specific SOPs in each section quality assurance practices sample handling documentation and follow up on prior audits These audits are used by the laboratory to identify any problem in their operations before there is an effect to the data All audits are documented and kept in the QA office If problems occur or corrective action is initiated the QAC from MPCA is contracted immediately for assistance in corrective actions Copies of the internal audit findings along with any required corrective actions are submitted to the MPCA s QA Coordinator As a result of the internal audits the MPCA may audit at its discretion External audits of the laboratory may be performed by other accreditation bodies Copies of the findings of these external audits and any identified corrective action are submitted to the MPCA s QA Coordinator As a result of these external audits the MPCA may audit at its discretion Section C 1 2 Performance Evaluation PE Studies The laboratory analyzes Performance Evaluation Samples PE Samples which are blind samples prepared by external companies and shipped directly to the laboratory The samples are logged in and analyzed as standard samples with the results being reported back to the independent company for scoring The laboratory receives these scores and reports them to regulatory authorities or states requiring PE samples for certification Satisfa
208. ewers basements or confined areas Call for assistance for disposal Disposal Dispose of by means in compliance with all State Local and Federal Regulations Exposure Limits 0 1 mg m3 from OSHA respirable Record Keeping 1 Make sure to record the date number of blanks number of standards and number of samples for each batch of samples run in your lab notebook 2 Make sure to write down what you do at the time you do it The sulfur coulometer is a bit finicky and writing things down can reduce headaches later 3 Record any odd results or problems with the sulfur coulometer If you are unsure of a result or something seems odd we encourage you to ask questions We want you to know that mistakes happen even to those who have years of laboratory experience The critical requirement is the mistakes be noted and discussed when they happen so corrections or adjustments can be made It is generally best to start over 4 All sample mass and sulfur results should be entered into the Sulfur Coulometry Template to obtain the Total Sulfur TS for each sample a It is best to enter the samples while running the instrument to ensure duplicates and standards fall within an acceptable range for each batch of samples Reagents Used Reagents used are dispensed using the original holding container holding containers squeeze bottles or stainless steel spatulas Reagents used as supplied by the manufacturer include anode solution 30 Pyridi
209. f 67 http fyi health state mn us phl environmental index html USEPA Certification for Laboratory Analyses for Drinking Water 3 Parameters Method Certification Status 20 Other SOCs 525 2 Fully Certified Aldrin Alachior Atrazine Benzo A Pyrene Butachlor Dieldrin Di 2 ethylhexyl adipate Di 2 ethylhexyl phthalate Endrin Heptachlor Heptachlor epoxide Hexachlorobenzene Hexachlorocyclopentadiene Lindane Methoxychlor Metolachlor gt Metribuzin Propachlor Simazine Toxaphene Technical Chlordane alpha Chlordane gamma Chlordane trans Nonachlor ES 21 Total Coliform Fecal Coliform E coli Colilert P A Format Fully Certified Membrane Filter SM 9222B and G2 Fully Certified 22 E coli Enumeration Membrane Filter EPA 1103 1 SM9213D Fully Certified Most Probable Number SM9223B Fully Certified 23 Gross Alpha 900 0 Fully Certified 24 Gross Beta 900 0 Fully Certified 25 Radium 226 903 0 Fully Certified 26 Radium 228 904 0 Fully Certified 27 Uranium 200 8 Fully Certified 28 Tritium EPA600 4 75 008 March 1976 p34 Fully Certified 29 Btrontium 89 90 905 0 Fully Certified 30 Photon Emitters 901 1 Fully Certified 31 Radon SM 7500 Rn Fully Certified 32 SUVA UV Absorbance at 254nm Fully Certified 33 Disolved Organic Carbon M5310C Fully Certified Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Di
210. following clients State Agencies Listed in order of sample volume received 1 Minnesota Department of Health Environmental Health Division Subdivisions Sections Asbestos and Radiation Section Drinking Water Protection Section Environmental Health Services Section Well Management Section 2 Minnesota Pollution Control Agency 3 Minnesota Department of Transportation 4 Minnesota Occupational Safety amp Health Agency OSHA 5 Minnesota Department of Agriculture 6 Minnesota Department of Natural Resources Federal Clients 1 U S Forest Service 2 Pipestone National Monument 3 Army Corp of Engineers Private Companies 1 Northshore Mining 2 LTV Steel Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 5 of 57 PROGRAM CODES Program Client Specific Codes Each client or program is assigned its own two letter MDH Program Code which is used for billing We are unable to perform initial data entry without a program code More detail about the program codes can be found in the client specific sections of this manual Also refer to the Environmental Laboratory Handbook for a complete list of program codes Miscellaneous Program Code Program code LN is used for clients that we do not have a contract with A billing name and address must be included with these samples Some
211. for a data sheet and the next data sheet has exactly two assigned numbers write those two numbers on the first data sheet and renumber the second data sheet In some situations the numbering error cannot be easily resolved by shifting the numbers around e tis not possible to add a number to the data sheet because the sequential number was used on the next data sheet Therefore all the sample numbers on the incorrect data sheet are extra e All the remaining data sheetshave multiple sample numbers so the extra number cannot be reassigned to a single sample It is therefore necessary to create a new data sheet for the extra sample number Using a new blank MDH lab sheet write the extra sample number s in the spaces at the top Use program code LM for extra sample numbers Write 997 Number not used in the comments section Enter code 997 for the sample s If the error was noticed after initial data was entered it may be necessary to correct other sample information through the editing screens Make sure that all samples have the correct program codes AN codes and date time Deliver the data sheets including the one for code 997 and sample log list to the clerical unit as usual Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision j Environmental Laboratory Effective Date Date of last signature Page 18 of 57 CHAIN OF CUSTODY CUSTODY FORMS Chain of Custod
212. for known extremely hazardous materials i Each laboratory is responsible for maintaining a current awareness file of the Occupational Health and Safety Act OSHA regulations regarding the safe handling of the chemicals specified in this method A reference file of Material Safety Data sheets MSDS should be made available to all personnel involved in the chemical analysis The preparation of a formal safety plan is also advisable The following chemicals have the potential to be highly toxic or hazardous for detailed explanation consult the MSDS 5 3 1 Cadmium 5 3 2 Sulfuric Acid 5 3 3 Phosphoric acid 5 3 4 Potassium persulfate 6 EQUIPMENT AND SUPPLIES 6 1 6 2 6 3 6 4 Balance analytical capable of accurately weighing to the nearest 0 0001 g Glassware Class A volumetric flasks and pipettes or plastic containers as required Samples may be stored in plastic or glass Flow injection analysis equipment designed to deliver and react sample and reagents in the required order and ratios l i 6 3 1 Sampler 6 3 2 Multichannel proportioning pump 6 3 3 Reaction unit or manifold 6 3 4 Colorimetric detector 6 3 5 Data system Special Apparatus 6 4 1 Lachat Sample Preparation Module A30X11 X 1 for 110V x 2 for 220V with UV 254 lamp 6 4 2 PVC PUMP TUBES MUST BE USED FOR THIS METHOD 10 107 04 3 D l Page 3 T 2 Dec 2010 sat 7 REAGENTS AND STANDARDS 7 4 PREPARATION OF
213. g 3 Have the collector sign the C of C form in the Relinquished By column 4 Sign the form in the Accepted By column 5 Give the collector the pink copy of the C of C form If they also submitted a regular multi copy data sheet give them the pink copy of that as well 6 After the submitter has signed off custody and the samples are determined to be acceptable they may leave Once samples are in the possession of Sample R ceiving personnel they may not be left unattended It is permissible to ask another Public Health Laboratory employee to watch the samples for a brief period of time A sample is considered to be in a person s custody if e tis in a person s actual possession OR e tis in view after being in a person s physical possession OR e t was in a person s possession and that person locked the sample up in a secure e cabinet or other storage container facility 7 Write the appropriate Chain of Custody code 990 or 991 on the C of C form and any other forms submitted with the samples Depending on how the collector listed the samples the custody code may not need to beadded to each line of the form Instead it should be added only once per SAMPLING POINT For example If a submitter collected VOC and Metals samples from the same sampling point but listed them on separate lines on the form we would assign a separate sample number to each line but then assign the C of C code to only one of the sample numbers If
214. g Comments on the data sheet NUMBERING THE SAMPLE DATA SHEETS Use the Rapidprint Machine to number the samples On the MDH 1 data sheet there are 4 spaces across corresponding to 4 columns Make sure the numbers are stamped in corresponding fashion For example if samples are listed only in columns 3 amp 4 stamp numbers in spaces 3 amp 4 only On some types of data sheets we must also write the sample number s in designated places after stamping all of the numbers on the top This includes the C of C forms Radiation data sheets OSHA forms etc Some data sheets have columns or rows for 10 20 samples we cannot stamp all of the numbers across the top of this type of sheet 1 Stamp the first number write thru or through after it 2 Write the sample numbers in the designated spaces on the data sheet 3 Use scratch paper to punch off additional number 4 Stamp the last number of the sequence on the slab sheet Stamping the date time on Data Sheets Use the AMANO PIX 3000 Electronic Time Recorder Time Clock to stamp the date and time on the upper right corner of the data sheets Do not stamp over a sample number or other pertinent information Make sure that every sheet gets the Date Time stamp so we can prove when the samples were received Minnesota Department of Health Sampl Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date
215. g Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 10 of 57 REJECTION PENDING LIST PROCEDURE When the LIMS system calculates that a sample has passed the hold time it will place it in the Rejection Pending List and ask the user to fill out an email form The email will be automatically sent to the client s that are identified with the particular program code The client then needs to reply to confirm the rejection or ask that the sample be run anyways 1 From the main screen select Entry and pull down to select Reject Pending List 2 The screen will list all the samples that are pending Next to each sample there are two boxes labeled Run Anyway and Reject Based on the clients response check the appropriate box For samples that are rejected the database will then indicate that they were past the hold time For samples that are run the database will indicate that they were past but run anyways at the clients request i 3 Bacteriological An 327 samples that are between 30 and 48 hours will be put on the list even though we routinely run them anyways by a business rule with Environmental Health For these samples both boxes will be checked 4 After making changes click the Confirm Rejection box which will commit the changes and remove the samples from the list Minnesota Department of Health Sample Receiving Procedure Manual
216. g based on an experimental design described in this document The tasks described herein will examine depth and time dependent concentrations of sulfate sulfide and iron in two types of sediments and in two different temperature environments in a controlled laboratory setting This experimental design will generate results to a provide a basis for comparing results from hydroponic studies to container mesocosms and field sites b help identify the importance of oxygen release from wild rice roots and c quantify the rate of diffusive transport of environmentally important chemicals into and out of sediment As part of the larger Wild Rice Sulfate Standard Study the results of this experiment will inform and support the MPCAs decision as to whether or not a change to the existing sulfate standard is necessary to protect wild rice and if so what the revised standard should be Such a change if warranted would be proposed in accordance with the provisions and requirements of Minnesota s Administrative Procedures Act Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 6 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 14 of 44 Section A 6 Project Descriptions Section A 6 1 Objective The quality objectives will generally follow the guidance outlined on the Quality System webpage http www pca state mn us index php about mpca mpca overv
217. g step iii Click the optimize button the one on the smarttune window not the button on the main menu and wait for the system to complete the optimization 1 Theresults of the tuning procedure is stored and can be viewed at the default optimization file which is used in the process of running the sample later on 2 The result of daily performance check is reported as a picture file and required timely save we save them in My document Daily performance report put the date at the end of the report before saving your report so you can keep track of them later 3 The results of smart tune especially the process of the AutoLen may not pass and the daily performance check may indicate fail if the default parameters are used for the tuning procedure It is said that the default setting set by the manufacturer was pretty strict and after several years of running the system may not meet the criteria Making sure the X Y alignment has been done well and the system is running OK It is OK to adjust the parameter to an acceptable level or accept the results with a little bit lower performance Judge this by consulting the software manual and comparing your performance check result with the past performance check results stored it the computer and recorded in the log book iv Once the optimization is complete record the results of daily performance check and save a copy of the report to the Optimization records folder in My
218. g system the torch and coil with the sampling receiving system the skimming cones vi vii On main menu of ELAN6000 software click file Open workspace select x y wrk and open In sample tab click analyze sample or analyze blank Switch to real time tab select signal in the box from the dropdown menu Watch the change of the signals Flip open the main chamber cover adjust the X and Y spectrometer alignment knobs located right outside of the torch box adjust the rear knob first to maximize the signal If the maximizing process has not been completed by one run of analyze sample blank repeat steps 5b i v to complete the process Cover back the main chamber Tune the system The purpose of this step is to tune and optimize the instrument by automatically run a series of selected procedures Click on the SmartTune button on main interface of software Click file and open select the desired tuning files from the list of pop up window 1 If the ICPMS has not been used for some days use the full tuning procedure by selecting smart tune full UMD swz file if the system has been used normally daily it is not necessary to run the full tune procedure run smart tune daily for saving some time and tuning solution watch and be sure the centrifuge tube containing tuning solution is not empty while the tuning procedure is running refill if
219. ge 19 of 44 reviewed to determine if appropriate procedures were followed If the procedures as described in this QAPP were followed sample results are considered representative of the site Section A 7 6 3 Comparability Comparability is the degree of confidence that one data set can be compared to another data set and whether the data sets can be combined and used for decision making purposes The level of comparability between data sets is determined by reviewing sample collection and handling procedures sample preparation and analytical procedures holding times and quality assurance protocols When a large difference in one of the methods or procedures exists the comparability of the data is considered low If all of the procedures were followed data from the same site is considered comparable Section A 7 6 4 Completeness Completeness is measured by determining the ratio of valid sample results compared to the total number of samples for a specific matrix During data verification the data completeness is determined by the following equation 96Completeness Number of Valid Results 100 Number of Samples Tested A completeness of 9096 in a year must be obtained in order for a laboratory report to be considered acceptable If the data set does not meet at least 9096 completeness the data are rejected If the laboratory is at fault and they will be responsible for securing the re collection and re analysis of samples W
220. ghed a 3 time using an analytical balance and final weight is recorded on label of bottle All weights are recorded in Element bench sheet Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 11 of 31 https inside mn gov sites MDH bureaus hpb phlid env inorganics Gen Chem SOPs gen26 doc UA RR A Neh a SNE RR RR a a 8 3 Maximum holding time is 14 days when stored at 4 C 2 C 8 3 1 Holding time for Acid Volatiles is 6 months when preserved with Zinc Acetate and stored at 20 C 90 QUALITY CONTROL 9 1 Initial Demonstration of Capability IDC The analyst must be able to demonstrate that they can generate acceptable accuracy and precision data with this SOP by successful completion of the following 9 1 1 Initial Calibration The 1st order calibration range must be determined initially and whenever a significant change in instrument response is observed The initial demonstration of linearity must use a calibration blank and a minimum of 3 different calibration standards One of the standards is near but above the MDL If any portion of the range is shown to be nonlinear sufficient standards must be used to clearly define the nonlinear portion The standards must bracket the range of concentrations found in samples and should define the working range of the instrument
221. gulations or agreements established for particular projects When we are not certain of the category for acceptance CWA SDWA RCRA etc for a particular sample i e the collector did not provide the project identification or indicate specific tests we will use the most stringent criteria to assure that the data are usable For missing items not affecting the outcome of the analysis e g collector name collection year we will leave the information blank or in the case of the collection year we will document the sample was collected within the past twelve months a reasonable assumption We will retain records of these discrepancies but will not contact you so please be sure you maintain your sampling logbook should questions arise The following items will prevent us from analyzing your samples and supplying valid results The sample containers were broken in shipment or the containers are leaking The samples were preserved but they require no preservation for accurate testing The samples submitted for volatile organics analysis have headspace i e air bubbles larger than pea size We did not receive enough sample volume to perform the tests you requested The sample container cap is loose and allows extraneous water or materials to seep into the samples We consider the following items crucial to valid testing We may be able to test the samples after we obtain more information from you The samples will be placed on hold in our sample
222. h Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date ot last signature Page 28 of 57 TESTS WITH A 2 DAY 48 HOUR HOLD TIME 6 Solids settleable 11 Turbidity 12 Color 35 Surfactant 63 Orthophosphate total 67 Nitrite total 69 Nitrate UNPRESERVED w Yellow dot on cap 70 Orthophosphate dissolved 73 Nitrite dissolved 75 BOD Bacterial Oxygen Demand 20 day dissolved 76 BOD 5 day dissolved 80 CBOD 20 day NI Dissolved 81 CBOD 5 day NI Dissolved 82 CBOD 20 day NI 83 CBOD 5 day NI 92 CBOD 40 day NI 95 BOD 20 day 96 BOD 5 day 301 MPN total DW Coliform 315 Heterotrophic Plate gt e PP 320 General Micro 327 E H Community d HA PA Coliform 330 331 332 333 334 335 Various MPN Colilert tests 59 63 Combined in one 250 ml general bottle w yellow fill line Program code HZ Put the Total Phosphorus 59 label ON the bottle Peel back 1 3 of Ortho Phos 63 label and place on the cap TESTS WITH A 3 DAY HOLD TIME 327 PA Total Coliform DW Colilert All types except for E H Community HA Program 308 MF Total Coliform DW TESTS WITHA4DAY HOLD TIME 809 Radon TESTS WITH A 5 DAY HOLD TIME 807 Radium 226 228 formerly test codes 805 amp 806 816 Gross Alpha SDWA SDWA Radiation samples must be acidified within 5 days of collection Minnesota Department of Health Sample Receiving Procedure Manual P
223. h answer sheet for PT project The unapproved use or modification of an Standard Operating Procedure Mishaps with sample collection delivery receipt handling identification preservation and or storage __ Internal or external audit deficiencies Instrument or analytical procedure not within Quality Control parameters e g calibration records standard expiration dates and control limits Instrument and or software malfunction with integration or data transfer e g check QC parameters preventative maintenance records and instrument operations Proficiency Test PT parameter failed to be within provider s acceptable limits Other please explain Investigative Steps Taken see page 2 for possible investigative steps for unacceptable PT results Original Quality Assurance Officer Copy QA Records EnviCorrective Actions 2008 CAF Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division i Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 67 of 67 http fyi health state mn us phl environmental index htm CUCA Corrective Action Form Revision 3 Created on 04 16 08 Page 2 of 2 Proficiency Test PT Investigative Steps Taken check those that apply Re read the instruction sheets for the PT sample s to see if special instructions time handling temperature dilution etc were overlooked Check the QC values for previous runs
224. hat is certified through another agency appropriate to the testing requested For example the laboratory considers certification by the American Industrial Hygiene Association AIHA for analysis of metals in air samples The Operations Unit supervisor acts as the project manager and provides oversight to ensure that clients needs are met All subcontracted data are entered into the LIMS and the subcontracted data report generated by the subcontracting laboratory is attached to the MDH final laboratory report I Sample Storage Samples are stored in walk in coolers refrigerators shelving areas or temporarily on carts in the laboratory analytical areas Storage conditions comply with the preservation and holding time requirements specified in regulation or method More information on monitoring storage conditions is in Section 11 0 of this manual J Sample Disposal For routine non custody samples analysts in the Inorganic Chemistry Unit and the Organic Chemistry Unit monitor the received dates printed on the sample bottle labels Personnel authorized by the unit supervisor dispose of most samples between 30 and 60 days after receipt Water microbiology samples are discarded on the day of analysis Personnel in the Sample Receiving Unit dispose of samples when final reports have been issued and storage space is needed for incoming samples The laboratory staff queries the LIMS for samples to be disposed Custody samples are retained f
225. he IDC and any ongoing DL study The frequency of any required ongoing DL must also be stated in the SOP The Detection Level Study must include all of the steps in the analysis including sample preparation and processing For purposes of this policy and procedure an environmental matrix may include multiple matrices example drinking water and non potable water may be grouped together so long as each matrix is processed and analyzed in a similar manner as part of a single SOP The written SOP must list all of the matrices for which it is applicable Note The effective date of this document is the date of the last signature on this document On the effective date this document becomes an appendix to the Quality Assurance Manual for the Environmental Testing Units of the Public Health Laboratory Division Minnesota Department of Health Public Health Laboratory Division Environmental Laboratory http fy i health state mn us phl environmental index html Quality Assurance Manual Filename qa0001 Revision 9 Effective Date Date of last signature Page 53 of 67 Appendix 9 l Method Detection Limit MDL Single Analyte Worksheet and MDL Worksheet Instructions Minnesota Department of Health Environmental Laboratory Method Detection Limit MDL Single Analyte Worksheet Instrument ID Target Analyte MDH LIMS Code Date submitted MDL Study Analytical Method Prep Method Reported Units 1st 2nd 3rd MDL Std D
226. he balance Open the Acid Volatile dry weight spreadsheet template Enter dish numbers in spreadsheet Open balance data transfer program and select Acid Volatile method 11 8 3 Place dish on balance When balance stabilizes record weight in spreadsheet Data transfer program will insert weight in selected spreadsheet cell eliminating need for typing weight and the possibility of transcription errors Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 22 of 31 https inside mn gov sites MDH bureaus hpb phid env inorganics Gen Chem SOPs gen26 doc A A A A ETS CN IA LA A M 11 8 4 When preparing Acid Volatile solids it is essential that you mix the sample well Using an analytical balance weigh out 5 g of soil into When balance stabilizes record weight in spreadsheet Data transfer program will insert weight in selected spreadsheet cell eliminating need for typing weight and the possibility of transcription errors 11 8 5 Set up a Duplicate DUP and for every 10 samples 11 8 6 Place sample in 105 C for at least 12 hours Remove dishes from oven using heat resistant gloves and tongs allow dishes to cool on the bench top for no more than 10 minutes set timer Complete cooling to room temperature in desiccator 11 8 7 Record dish weights using an analytical bala
227. he normality of iodine and sodium thiosulfate has not changed 7 17 1 7 Using the found concentration of the stock standard determine the volume of stock standard needed to make the 10 mg L intermediate standard The formula used is CyVi Ca Va 7 17 2 Intermediate Stock Standard 10 mg L In an acid rinsed 500 mL volumetric flask add the volume of 100 mg L stock standard determined in 7 14 1 7 Dilute to volume with 0 025 M sodium hydroxide reagent and invert to mix Prepare fresh daily 7 17 3 Working Calibration Standards To prepare 200 mL quantities of calibration standards use acid rinsed 200 mL volumetric flasks Add 20 mL of alkaline antioxidant reagent to approximately 100 mL of 0 025 M sodium hydroxide reagent Use the table below to determine the correct amount of stock standard to pipette into each volumetric flask Dilute to volume with 0 025 M sodium hydroxide reagent and invert to mix Prepare fresh daily Calibration Standard Quantity of 10 mg L Intermediate Stock Standard 0 02 mg L Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 10 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc 8 0 7 18 The second source calibration verification SCV is purchased and prepared according t
228. her Lead Worker Sample Receiving Supervisor Laboratory Services Gary Jones Stephanie Drier Information Systems Manager QA Officer Environmental Laboratory Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 2 of 57 TABLE OF CONTENTS INTRODUCTION TO SAMPLE RECETV ING eee eene eene earn e nena etae tenen eene tata sensn 4 CLIENTELE Rc 4 PROGRAM CODES 5 DXVEIN DIST M 5 DI DEVE NI FSRR oros 6 COMPUTER OPERATIONS e eeeeeeee ee eee ee etna eset etes assess eosam Presa eee anna eese eaten sess eee t ease aen 7 OVERVIEW OF SAMPLE ENTRY SCREENS eese repeats tese ee testatattte rms 7 INITIAL DATA ENTRY PROCEDURE eee ec etlenaa eee se asses enenenesenes etit ib see eeseseseseseeseceses O REJECTION PENDING LIST PROCEDURE 4 eee eene eere eere eene ee to oath a se ona aane ee en aee tn natae 10 EDITING SAMPLE ENTRY INFORMA YTION eee eeea eene eese enata tnos tta aeneo ns nennen tn 11 USING THE VIEW SCREENS TO FIND SAMPLE RECORDS eere tette 13 USING LAB REVIEW TO FIND A PROGRAM CODBE eene ee eren netten tnnt 15 ADMINISTRATIVE CODES 2 4 44 ee ee eett tata aae a eee ee esaet e aatis osos
229. ible sources of ignition spark or flame Small Spill Dilute with water and mop up or absorb with an inert dry material and place in an appropriate waste disposal container Large Spill Flammable and poisonous liquid Keep away from heat or sources of ignition Adsorb with dry earth sand or other non combustible material Call for assistance with disposal Disposal Dispose of by means in compliance with all State Local and Federal Regulations Vanadium Pentoxide Acute Effects Very hazardous in case of ingestion or inhalation Hazardous in case of skin contact irritant or eye contact irritant Slightly hazardous in case of skin contact Chronic Effects The substance may be toxic to gastrointestinal tract upper respiratory tract and skin Repeated or prolonged exposure to the substance can produce target organ damage Repeated exposure to highly toxic material may produce general deterioration of health by an accumulation in one or many human organs Compound Specific PPE All sample prep work that involves vanadium penoxide should be conducted in a fume hood while wearing a lab coat face mask goggles and nitrile gloves Storage Store in a tightly closed container Store in a cool dry well ventilated area way from incompatible substances Small Spill Use appropriate tools to put the spilled solid in a convenient waste disposal container Large Spill Poisonous solid Do not touch spilled material Prevent entry into s
230. ibration to verify instrument performance The results of the SCV must be within the manufacturer s range of the target value otherwise corrective action is taken before analyzing samples If the SCV is out of control the run data can only be accepted by the Unit Supervisor 9 2 3 Demonstration of Low Background At the beginning of each run and with each batch analyze an initial calibration blank ICB or blank BLK to determine reagent or laboratory contamination The background level of the BLK or ICB must be below the report level otherwise the source of the contamination is investigated and corrected before samples are analyzed Analyze a continuing calibration blank CCB every 10 samples and at the end of the run The CCB must be less than the report level MRL If the CCB is above the Report Level the source of the deviation is investigated and corrected before the next batch of samples can be analyzed Samples must be bracketed by passing CCBs to be accepted Samples associated with failing CCBs are reanalyzed 9 2 4 Report Level Verification RLV Check A Report Level Verification CRL check must be performed each time the instrument is calibrated The CRE check is performed by Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 14 of 31 ni linside mn gov sites MDH bureaus h
231. ical Pipetas 34 Analytical Instrulients sieut oie pe deserti od i a dub aas dU cios 34 Quali Conttols coop tdo ota a dep lr sde 34 QC in the QA Manual and in SODBS ied mater tinere trio di 34 Detection EVE ls ads 34 Initial Demonstration of Capability esee T 35 Report Level Verla 35 Other QO C Dee oS liada 35 Data Reduction Verification Validation and Reporting sss 35 Reduction and Validation Process ccsssssssssssssseseessessssessecscsscssessesecssessesseceseateasseseas sud A E aA 37 SEM Audits nihoni n iod ay Sense aE E recul oiv A ad 37 Proficiency esti A a 37 Internal A Ulis a tia tdo o 38 EXE NS 38 Corrective Action Pol a atentado eger tione upra cas dod 39 A O uad oda tod enfer Didonis sat dedu uis R Ped esce 40 Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 5 of 67 http fyi health state mn us phl environmental index html Appendix 1 Appendix 2 Appendix 3 Appendix 4 Appendix 5 Appendix 6 Appendix 7 Appendix 8 Appendix 9 Appendix 10 Appendix 11 Appendix 12 Appendix 13 Appendices Table of Contents PHLD organizational chart focusing on the environmental testing units 42 Training record for an individual Standard ee Procedure i 43 Record of Personnel Education and Training 44 Sample analysis requ
232. icate Conc Precision can also be determined between the results of a laboratory control sample LCS laboratory control sample duplicate LCSD pair RPD results should be 2596 for water samples and 5096 for sediment samples for the data to be acceptable Section A 7 6 1 Accuracy The accuracy of the measurement is gauged through the analyses of surrogate spikes matrix spike MS and or laboratory control sample LCS laboratory control sample duplicate LCSD Surrogate compounds are spike into every sample prior to extraction and analysis Where possible a MS sample is collected If a MS cannot be analyzed an LCS LCSD pair may be used to measure accuracy The percent recovery is determined by comparing the spiked sample concentration to the environmental un spiked sample concentration The formula for determining percent recovery is as follows R Spiked Sample Conc Environmental Sample Conc 100 Spiked Concentration Added Section A 7 6 2 Representativeness Representativeness of the data set is the measure that expresses the degree to which the data accurately represents the population as a whole The methods for sample collection in the laboratory sample preservation and storage sample preparation and sample analysis are Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 7 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Pa
233. iew agency strategy mpca quality system html expandable 1 amp menuid amp redirect 1 The Quality System for MPCA s environmental data describes the agency s general policy for data quality assurance This QAPP falls under all requirements of the MPCA s Quality Management Plan QMP which is approved by U S Environmental Protection Agency EPA Region 5 The objective of this experiment is to measure interpret and then model sulfide sulfate oxygen and iron in the rooting environment of wild rice Section A 6 2 Scope Sediment will be collected from two wild rice environments with contrasting sediment quality and then incubated in laboratory microcosms 8 inch diameter at least 20 vertical cm of sediment Six microcosms will be incubated from each of two sites chosen in consultation with the MPCA Project Manager 12 microcosms total six microcosms from one site with higher organic sediment and six microcosms from a second site with coarser less organic sediment Half of each set three from each site will be incubated at room temperature approximately 21 degrees C and half at approximately 4 degrees C to investigate the effects of temperature on sulfate flux and conversion to sulfide Initially overlying water with relatively low sulfate similar to site water will be maintained over sediment microcosms Subsequently overlying water sulfate concentrations will be increased to a concentration of 300 mg L consistent with concentration
234. iew back how and which reprocess have been done otherwise leave it there The data can be reprocessed many times with various conditions If you want to save a report of the results differ from the report generated from previous reprocess go to 15 Method tab and click the Report and defile a different name otherwise the new results will overwrite or append at the end of the old one depending on the selection you have made before in Report tab Click Reprocess data the software will reprocess your data Save your new standard calibration with a new name with current date if you just have done a calibration by assigning the standard solutions This new calibration will be used to calculate the actually concentration of the samples that you will be reprocessing Be sure the currently opened method file is the same as the method file that you have defined on the Method file column on dataset window corresponding to the data that you are to reprocess The system read the method file that is currently open as the method to reprocess you data if your opened method file is no consistent with the method file you are suppose to use for reprocessing the data the results will be confusing 10 Viewing the result reports a b The result report can be viewed and converted to Excel file In Excel click Open look in C Elandata ReportOutput select your result file Open In Text Import Wiz
235. ike two additional sample aliquots with the spiking solution and analyze these aliquots to determine the concentration after spiking A Calculate the percent recovery P of the analyte in each aliquot using the following equation 10 115 01 3 E Post MUR p A B 100 T Page 9 l 3 December 2010 sat 9 4 9 5 9 6 9 3 4 9 3 5 Where A Measured concentration of analyte after spiking B measured background concentration of analyte T True concentration of the spike The percent recovery of the analyte should meet current laboratory acceptance criteria 9 3 4 1 If the results of the spike fail the acceptance criteria and the recovery of the QC standard in the ongoing precision and recovery test of the analytical batch is within the current laboratory acceptance criteria an interference is present In this case the results may not be reported for regulatory compliance purposes and the analyst must assess the potential _ cause for the interference If the interference is attributable to sampling the site or discharge should be re sampled If the interference is attributable to a method deficiency the analyst must modify the method repeat the test required in Section 9 1 2 and repeat the analysis of the sample and the matrix spike 9 3 42 If the results of both the spike and ongoing precision and recovery test fail the acceptance criteria the analytical system is judged to be out of control and the problem
236. ild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 8 and A 9 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 20 of 44 Section A 8 Specialized Training Certifications Section A 8 1 Laboratory Laboratory personnel have been trained in proper analytical techniques They also receive annual refresher training on such items as laboratory safety right to know and emergency procedures The documentation of this training is maintained in the Laboratory Manager s office or in the laboratory s QA Office Section A 9 Record Keeping The State of Minnesota has a structured record management retrieval system that allows for the efficient archive and retrieval of records All information considered as documentation and records will be retained for 10 years from the date of generation However if any litigation claim negotiation audit or other action involving the records has been started before the expiration of the 10 year period the records must be retained until completion of the action and resolution of all issues which arise from it or until the end of the regular 10 year period whichever is later The laboratory SOP for records retention indicates that all data documentation records protocols and final reports are stored either on site at the laboratory or off site in secure storage The records are retained for a period of not less than 10
237. important component of aquatic communities in parts of Minnesota particularly northern Minnesota It provides food for waterfowl and shelter for animals and fish Wild rice is also a very important cultural resource to many Minnesotans and is economically important to those who harvest and market wild rice Based on testimony presented at public hearings leading to the adoption of the sulfate standard it was intended to apply both to waters with natural wild rice stands and to waters used for paddy rice production The MPCA is presently undertaking a study to investigate the potential effects of elevated sulfate on the growth of wild rice One high priority hypothesis is that the conversion of sulfate to sulfide in anoxic subsurface sediment may harm the roots of wild rice either directly or indirectly Sulfide reacts with many metals including iron which may play a major role in controlling sulfide in the sediments of wild rice habitat The rate at which sulfate from overlying water diffuses into and is converted to sulfide within different types of sediments at high and low temperatures is presently unknown Additionally the feasibility of maintaining environmentally relevant sulfide concentrations in laboratory experiments is also unknown To address these issues sediment from two different sampling sites with different characteristics will be collected and incubated at two different environmentally relevant temperatures in a laboratory settin
238. in a solution of 70 alcohol 90 ethanol 5 propanol 5 methanol and stored at 4 C in glass or plastic bottles Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 2 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 25 of 44 that are labeled by treatment and replicate number to be analyzed by MPCA aquatic organism experts for identification and quantification The volume of sediment in each 2 diameter core will be recorded to calculate concentration of organisms per given volume of sediment In addition three or four 1 diameter sediment cores will be taken and composited per treatment replicate for analysis of total sulfur AVS total carbon and nitrogen and solids Samples will be preserved based on the QA QC requirements of the lab contracted to conduct the analyses This information can be found in Table 3 of this document Timing The final microcosm coring for sediment collection and characterization will take place during the 2 to 3 days of the deconstruction phase of the experiment Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 2 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 26 of 44 Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 3 Revision No
239. index html 5 Minimum Reporting Level A minimum reporting level MRL also known as Reporting Limit or Report Level must be established 6 Method Detection Limit MDL Study A minimum of 7 replicate laboratory fortified blanks LFB are spiked at a value 1 to 5 times the estimated detection limit The MDL is determined using the procedure in 40 CFR Part 136 Appendix B and following the current guidelines in MDH Environmental Laboratory Detection Level Policy and Procedure This can be completed in one analytical run when performing an MDL study as part of an IDC The Quality Assurance Officer may specify a time frame for completion of the MDL study Documentation and other requirements The acceptance criteria for each element of the IDC and corrective actions that the analyst must take if the acceptance criteria are not met must be described in the SOP The frequency with which an IDC is conducted must also be included in the SOP The IDC must include all of the steps in the analysis including sample preparation and processing For purposes of this policy and procedure an environmental matrix may include multiple matrices example drinking water and non potable water may be grouped together so long as each matrix is processed and analyzed in a similar manner as part of a single SOP The written SOP must list all of the matrices for which it is applicable Every analyte or analysis for which an IDC is required must have an IDC on file
240. ing exposure to sampling site conditions equipment storage preservation if necessary and all analytical procedures The purpose of the field blank is to determine if the field procedures or sample transporting procedures and environments could have contaminated the samples Field Duplicates FD1 and FD2 Two separate samples collected in separate sample containers at the same time and place under identical circumstances and treated exactly the same throughout field and laboratory procedures Analyses of FD1 and FD2 give a measure of the precision associated with sample collection preservation and storage as well as with laboratory procedures Filter Blank FB For each batch of lab filtered or field filtered samples reagent water is passed through one or more unused 0 45 um filter s and the filtrate from each is collected The filtrate is treated like all other dissolved samples in the batch Analysis of the filter blank will reveal contamination from the filter or filtration process Holding Time Maximum Allowable Holding Time The maximum time that a sample may be held prior to preparation and or analysis and still be considered valid or not compromised Initial Demonstration of Capability IDC A procedure by which an analytical team must demonstrate acceptable precision accuracy sensitivity and specificity for the analysis prior to its initial use For additional information see the Policy and Procedure for Initial Demonstra
241. ion Laboratory Approval Manual version 2 0 October 2006 One Minimum Reporting Level Verification MRLV sample must be analyzed daily to demonstrate that for each analyte near the MRL the measured recovery for each analysis or analyte is within limits established by the Quality Assurance Officer Note UCMR2 states recovery must be within 50 to 150 inclusive The MRLV sample is a Laboratory Fortified Blank LFB that must contain all method preservatives described in the method contain each analyte of interest at concentrations at or below the MRL and be processed through the entire method procedure i e including extraction where applicable Remedial action Ifthe percent recovery of the Report Level Verification standard is outside the acceptance criteria the analyst must either 1 repeat the verification check or 2 recalibrate and then perform the Report Level Verification check If the repeat RLV is within acceptance criteria or if the instrument recalibration results in a Report Level Verification check that is within acceptance criteria the analyst may proceed with the analytical run If the second verification check is not within acceptance Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 60 of 67 http fyi health state mn us phl environmental index html criteria the analy
242. ion response data by the Omnion 3 0 Software Attach a pdf of the curve to the sequence in Element to document the initial calibration The calibration standard curve is accepted if a correlation coefficient of at least 0 9990 is achieved Also the concentration of the standards must be within 10 of their true value except the lowest standard which can be 20 of its true value 10 5 After the calibration has been established it must be verified by the analysis of the ICV ICB SCV CRL CCV and CCB 10 5 1 If measurements exceed 10 of the established ICV value 0 5 mg L the analysis should be terminated and the instrument recalibrated The new calibration curve must be verified before continuing analysis 10 5 2 The background level of the analyte in the ICB must be at or below the MDL otherwise the source of the contamination is investigated and corrected before samples are analyzed 10 5 3 The results of the CRL must be within 40 of the true value 0 01 mg L in order to proceed If it is not follow the procedure outlined in Section 9 2 4 10 5 4 If measurements exceed the range of the established SCV value the analysis should be terminated and the instrument recalibrated The new calibration curve must be verified before continuing analysis 10 5 5 A continuing calibration verification standard CCV and a continuing calibration blank CCB must be run every 10 samples and at the end of each run The results f
243. is point if the coulometer isn t titrating delicately adjust the electrodes until they begin to titrate 6 Blank Runs a Use an empty ceramic boat filled with a small amount vanadium pentoxide as much as you would put on a regular sample b Put the ceramic boat with vanadium pentoxide in combustion tube and push into the combustion furnace using the medal sample rod Close combustion tube as quickly as possible to reduce the loss of combusted sulfur c Press the reset button on the sulfur coulometer d Wait 10 minutes and record the ug S in the Sulfur Coulometry Template Blanks will range from 5 to 40 ug S 7 Sample Runs a Weigh sample out on a clean ceramic boat 50 to 150 mg depending on sulfur content b Cover sample completely with vanadium pentoxide i To reduce the likelihood of spilling vanadium pre weigh all the samples you plan to run and place them in order make sure to write down the order in secondary containment ii Place pre weighed samples in the fume hood iii Put a lab coat nitrile gloves and lab goggles on before handling vanadium iv Cover each pre weighed sample completely with vanadium pentoxide v Bring the samples back into the coulometry room in the secondary containment c Put your first ceramic boat with sample and vanadium pentoxide in combustion tube and push into the combustion furnace using the medal sample rod Close combustion tube as quickly as possible to reduce the loss of combusted
244. ite their analysis requests on the bottom of the form instead Solvent samples are for the Organics Lab Bactichem and Radiation rarely receive OSHA samples Metals The Periodic Table of Elements Chemical Symbol of each Metal is listed after the name because OSHA collectors often request metals tests this way Metals Analysis Codes Metals Digest Prep Codes 653 Aluminum A 682 Miscellaneous 654 Antimony Sb 683 Filters 655 Arsenic AS 684 Wipes 656 Barium Ba 685 Bulks 657 Beryllium Be 686 Dust Minnesota Department of Health Public Health Laboratory Division Environmental Laboratory 658 659 660 661 662 663 664 665 666 667 668 669 670 671 672 673 674 675 676 677 678 679 680 688 981 Boron B Cadmium Cd Calcium Ca Chromium Cr Chromium Hexavalent Cr 6 Cobalt Co Copper Cu Iron Fe Lead Pb Magnesium Mg Manganese Mn Mercury Hg Molybdenum Mo Nickel Ni Potassium K Selenium Se Silver Ag Sodium Na Thallium TI Tin Sn Titanium Ti Vanadium V Zinc Zn Bismuth Bi Sample Receiving Procedure Manual Revision Effective Date Date of last signature Page 56 of 57 687 Paint One Digest Prep Code must be assigned to each OSHA Metals sample along with the Analysis Codes If Metals Group 1 is requested it consists of the following codes 661 Chromium Insol Salts 664 Copper fume as Cu 665 Tron oxide fume 668 Manganese fume as Mn 671 Nickel Insol Comp 680 Zinc
245. ive portion of a sample taken for sample preparation and or analysis and assumed to have been taken with negligible sampling error Analyte The element ion compound or other substance that an analytical procedure determines Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 7 of 67 http fyi health state mn us phl environmental index html Analytical Run The continuous analysis of one or more analytical batches using the same calibration Batch Field and QC samples that are prepared and or analyzed together A preparation batch is a group of field and QC samples of the same matrix prepared with the same process and personnel using the same lot s of reagents An analytical batch is composed of field and QC samples that are analyzed together as a group An analytical batch can include prepared samples originating from various matrices provided that the matrices do not adversely affect other matrices such as by carrying over to another sample matrix Bias The systematic or persistent deviation of a measurement process which causes errors in one direction Blank Filter BF This applies to analyses where a filter is used to collect and retain the sample The filter is processed and analyzed for the target analyte s Blank filters should be taken from the same lot as the sample filters and
246. iver them to MDH for testing We also provide sample bottles for these collectors We have standing routine bottle orders set up for some of the landfills that have a regular sampling schedule The order information is in a yellow folder that is stored in a rack on the counter The parameter test code lists for these standing orders aren the desk file drawer each in their own labeled folder The parameter lists should be brought with the lab sheet every time Interpoll Labs faxes their bottle orders to us as needed Their bottle orders list the parameters that will be run on the samples and we must determine the necessary bottles from this list The parameter list is in alphabetical order rather than by bottle type or numerical order This makes it difficult to figure out the type of bottles needed when a person is new to sample receiving Listed on the next page are the codes in the parameter list order with the bottle type listed by each code A list of codes in numerical order follows and finally a list of codes taken from each bottle type are listed Alphabetical List Test Code Bottle type Alkalinity 22 General 1 liter Ammonia Nitrogen 64 Nutrient Arsenic 108 109 Metals Barium 113 114 Metals BOD bacti oxygen demand 96 General 2 liter Bromide rarely ordered 455 two 40 ml vials ask organics Cadmium 122 123 Metals Calcium 694 695 Metals CBOD 83 General 2 liter Chloride 23 General 1liter Chromium 129 130 Metals Co
247. lding during regular business hours 3 Contractor badges provide access to all of the general lab spaces throughout our building and general spaces in the Freeman Building The Contractor badges also provide access to the engineering spaces in both buildings Visitors must be escorted by an authorized employee while in the laboratory facility SECTION 4 0 POLICIES Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 20 of 67 http fyi health state mn us phl environmental index html D E Quality Assurance Policy Laboratory staff members provide quality data and services to clients according to their needs The laboratory management team considers quality to be an ongoing process of improvement and an integral part of the laboratory s testing and support operations To support the quality goals the laboratory management team ensures that adequate facilities supplies staffing and supervision are available to perform the testing required The laboratory s management team ensures that quality measures are documented and data are stored and disseminated in a manner that allows access to public data while protecting client confidentiality This manual and its related procedures specify the activities performed to achieve the quality goals of the laboratory and its clients Ethics Policy
248. le from the American Chemical Society s Department of Government Regulations and Science Policy 1155 16th Street N W NES D C 20036 202 872 4477 15 WASTE MANAGEMENT 15 1 15 2 It is the laboratory s responsibility to comply with all federal state and local regulations governing waste management particularly the hazardous waste identification rules and land disposal restrictions and to protect the air water and land by minimizing and controlling all releases from fume hoods and bench operation Compliance with all sewage discharge permits and regulations is also required For further information on waste management consult the Waste Management Manual for Laboratory Personnel available from the American Chemical Society s Department of Government Regulations and Science Policy 1155 16th Street N W Washington D C 20036 202 872 4477 16 REFERENCES 16 1 U S Environmental Protection Agency Methods for Chemical Analysis of Water and Wastes EPA 600 R 93 100 Revised August 1993 Method 353 2 10 107 04 3 D Page 14 2 Dec 2010 sat 16 2 Determination of Nitrogen in Water Comparison of a Continuous flow method with on line UV Digestion with the original Kjeldahl method Hennie Kroon Analytica Chemica Acta 276 1993 287 293 16 3 Lachat Instruments Inc ukhen Method 10 107 04 3 P 10 107 04 3 D Page 15 l 2 Dec 2010 sat graphical events programming Sample throughput Pump Speed Cycl
249. len screw in the center of the block The expired membrane is removed and a replacement centered If the replacement membrane has any text on it the membrane should be placed so that the text side faces the bottom of the unit The part numbers for this are as follows 85362 BUBBLE TRAP QC8000 8500 Not salable 85363 BUBBLE TRAP SPARE MEMBRANES PK 5 85364 TUBING SET BUBBLE TRAP QC8000 QC8500 85361 KIT BUBBLE TRAP QC8000 QC8500 10 107 04 3 D Page 28 2 Dec 2010 sat 17 5 MEASURING NITRATE NITRITE UTILIZING TN MANIFOLD 17 5 1 DATA SYSTEM PARAMETERS FOR NITRATE NITRITE The timing values listed below are approximate and will need to be optimized using graphical events programming Low Range f Sample throughput 60 samples h 60 s sample Pump Speed 35 CyclePeriod 60 Analyte Data Concentration Units mgN L Peak Base Width 67 6 s Inject to Peak Start 28 9 s Chemistry Direct Bipolar Calibration Data 7 8 9 Concentration mg N L _ 2 00 1 00 0 40 0 20 0 10 0 04 0 02 0 01 0 00 Calibration Fit Type 2 Order Polynomial Weighting Method 1 x Force through zero No Sampler Timing Min Probe in Wash Period 15s Sample Period 20s Valve Timing l Load Period 15s Inject Period 45s 10 107 04 3 D l Page 29 l 2 Dec 2010 sat High Range Sample throughput Pump Speed Cycle Period Analyte Data Concentration Units Peak Base Width Inject to Peak Start
250. licy and Procedure for Report Level Verification in the Appendices to the QA Manual Requirement Denotes a mandatory specification often designated by the terms shall or must Resource Conservation and Recovery Act RCRA The enabling legislation under 42 USC 321 et seq 1976 that gives USEPA the authority to control hazardous waste from the cradle to grave including its generation transportation treatment storage and disposal Run See analytical run Safe Drinking Water Act SDWA The enabling legislation 42 USC 300f et seq 1974 Public Law 93 523 that requires the USEPA to protect the quality of drinking water in the U S by setting maximum allowable contaminant levels monitoring and enforcing violations Sample A representative portion of material water soil etc collected for analysis in the laboratory A sample must be uniquely identified When the sample is further prepared by subdividing mixing or grinding or a combination of these operations the result is a test sample Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 17 of 67 http fyi health state mn us phlVenvironmental index html When no preparation of the sample is required the sample is the test sample An aliquot is removed from the test sample for the performance of the test or for
251. lient The laboratory maintains complete copies of all laboratory records Sample Custodians A member of the Environmental Laboratory Management Team is designated as the custody coordinator The custody coordinator maintains a list of sample custodians and ensures proper training and appropriate access to custody areas The following positions are designated sample custodians for the laboratory sample receiving personnel quality assurance officer and unit supervisors or their designees Additional Instruction Additional guidelines for sample collection storage and delivery for civil or criminal chain of custody samples are available on the department s intranet site http fyi health state mn us phl environmental handbook intranet custodyprocedures pdf Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 29 of 67 http fyi health state mn us phl environmental index html G Sample Tracking All samples that are analyzed in the laboratory follow a standardized tracking process A sample analysis request form accompanies each sample when it arrives at the laboratory The collector enters information about the sample on this form A one page set of instructions about completing the sample analysis request forms is provided to the collectors in the MDH Environmental Laborator
252. lity System A set of policies objectives principles organizational authority responsibilities accountability and implementation plan of an organization for ensuring quality in its work processes products items and services The quality system provides the framework for planning implementing and assessing work performed by the organization and for carrying out required QA and QC Raw Data Describes any original factual information from a measurement activity or study recorded in laboratory notebooks worksheets records memoranda notes or photo copies thereof that are necessary for the reconstruction and evaluation of the report of the activity or study Raw data may include photography computer printouts magnetic media and recorded data from automated instruments After processing some raw data are passed to the laboratory s database Laboratory Information Management System or LIMS which enables the data to become compiled into reports or to become accessible for further analysis or processing Reagent Blank RB See Method Blank Reagent Water Water known to be free of interfering amounts of target analytes or other interferences Individual SOPs may have additional requirements Reference Method A test method issued by a nationally recognized organization from which the laboratory s analytical Standard Operating Procedure SOP is derived Relative Percent Difference RPD A measure of precision between two values
253. ll maintain it powered and should be ready to use If the system is shut down consult Bryan to power it up Monitor the Argon pressure and be sure the tank is not empty if the gage show less than one quarter of argon left inform Bryan for new order A full small tank of argon can last 8 hours and a big tank of argon can last about 40 hours for normal operation However the process of igniting plasma can consume extra amount of argon especially when you have to try many times for ignition process Make sure the valves of argon flowing system are opened all the way Check for green signs on Instrument front panel on software interface Replace the tubing the small one of clamped by peristaltic pump with new tubing daily or every 8 hours of running remember to stretch it when you release the tubing from peristaltic pump Replace the drain pump tubing The large one weekly Install sampling and draining tubing on peristaltic pump Connect sampling tip to sampling tube submerse sampling tip in Milli Q water and turn on peristaltic pump to make sure the flowing directions are correct and they drain If needed consult manual P4 13 for detail of reconnecting the Peristaltic Pump Check and make sure the tubing at the back side of autosampler works well otherwise replace it d Cleaning skimmer cones and torch vi vii Flip open the cover of main chamber carefully slide the vacuum chamber and main interface to the left
254. llowed by th three blanks Carryover Passed File Name 12 2 cal support Acq Date 2 Dec 2010 i Page 34 2 Dec 2010 sat 10 107 04 3 D Calibration Data for Nitrate Nitrite High Range 7 o o x gaa d 400 9100 melo 409 ma L o 290 mon EM mg L S 8132 7 UN zs gt ex 586 8 Time s File Name 11 12 cal HR omn Acq Date 12 Nov 2009 Calibration Graph and Statistics 19 8i 202 nn mE 11 12 2808 9 95 9 0779 11 12 2003 11 12 2008 3 8 L0 00 mall 0f 0 ieget 1 60 3 11 12 2009 11 12 2009 11 12 2009 11 12 2009 0 0759 0 0389 0 0386 11 12 2009 11 12 2008 11 12 2009j 1310 AME 8 14 39 AME fe 315e 3 Conc 1276 4 Area 0 186 Area 3096 4 Carreletion Coefficient r 1 00000 1 Weighting 1 x 10 107 04 3 D Page 35 31 42 2009 2 Dec 2010 sat Volts 2 4e 3 0 137 PAN i Lil i 18e43 Time s Method Detection Limit for Nitrate Nitrite using a 0 05 mg N L standard MDL 0 012 mg N L Standard Deviation s 0 004 mg N L Mean x 0 052 mg N L Known Value 0 05 mg N L File Name 11 12 support HR omn Acq Date 12 Nov 2009 438 r 10 ppm 10 ppm mg L 10 ppm s mgit o o o Lj 83 mg L Volts
255. lorophyll filters wrapped in tinfoil in this freezer labels go in the field filtered chlorophyll basket on the general counter 6 e 8 Put chlorophyll bottles in the walk in cooler Line them up on the shelves in the back left corner Labels go in the lab filtered chlorophyll basket on the general counter 6 Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 42 of 57 9 Cryptosporidium filters or water jugs go on the middle shelf just inside the cooler door 10 Bromate Chlorite samples should be collected in 250ml unpreserved plastic bottles wrapped in tinfoil Place them on the middle shelf in the cooler 11 AII bacteriological samples are placed on this counter Line up samples in groups of five front to back and right to left For non routine bacti analyses put copies Of the lab sheets on top of the samples for the lab analysts 12 Put copies of cryptosporidium lab sheets on this counter Refer to the Labs Map North for the following sample delivery locations 1 Most non volatile organics samples PFOS SOC PCB S VOG etc are placed in this refrigerator This cooler is often quite full but try to follow the shelf labels for the correct placement of samples For PFOS samples put a copy of the lab sheets on Julia s desk For other non routine samples leave a copy of the lab sheet
256. lso allows you to find the name and address information for a given PWS 1 From the main screen use the mouse to select View and pull down to select PWS Table Review 2 Hit F7 or click on the Enter Query button to put it in query mode Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 14 of 57 e 3 To find the PWS for a sample you can use the name and or address fields to search for it Enter the known information using the symbol to search for all systems with that word in their name For example querying BAY will bring up all systems with the word BAY in the name Advance through the list using the arrow keys to find the right system The other fields can also be used to search using the same method 4 To find the address information enter the PWS and click on the Execute Query button This will bring up the complete record for that system Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 15 of 57 USING LAB REVIEW TO FIND A PROGRAM CODE If samples are received with no program code indicated the Lab review options can be used to figure out what the code should be This method will only work for facilities that have a PWS ID
257. lved and documented according to QA procedures B Training 1 General Employee Training for all staff New employees are asked to participate in a six hour New Employee Orientation training hosted by the department training coordinator within the first three months of their employment This training provides information about functions and policies of MDH and the State of Minnesota All employees in the environmental testing units are required to read understand and agree to comply with the contents of the laboratory s Quality Assurance Manual and the specific referenced policies and procedures that are pertinent to the individual analyst These include pertinent sections of the references listed in Section 16 0 References pp 36 37 pertinent appendices included in this Quality Assurance Manual and pertinent Standard Operating Procedures SOPs Copies of the completed Quality Assurance Manual Agreement Form are kept in the training files for all employees The text of the agreement is as follows Quality Assurance Manual Agreement As an employee in an environmental testing unit of the MDH Public Health Laboratory Division I have read and understood the contents of the currently approved Quality Assurance Manual I have also read and Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page
258. ly Bottle Orders Periodically Sandy Bissonette and Beth Endersbe send us their standing bottle order Generally Lab Services Shipping personnel fill these orders on a monthly basis The MPCA courier picks up the orders and delivers them to the MPCA warehouse Specialized Bottle Orders Local MPCA collectors frequently place more complicated and specialized bottle orders directly with us Many of these orders are for emergencies and we try to fill them as needed Most organic bottle orders are placed this way If you are unsure what type of bottle the collector needs refer them to the appropriate Unit Leader or other laboratory personnel for assistance Out state Bottle Orders Occasionally out state MPCA collectors place orders that they want shipped directly to them and we try to accommodate them However it the order is fora large number of routine bottles general nutrient metal cyanide bacteriology etc refer them to Ed Norwig in the MPCA warehouse LS ee ee a Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 51 of 57 MPCA CLOSED LANDFILL PROGRAM The Minnesota Pollution Control Agency MPCA administers this program in order to monitor the groundwater quality of sanitary landfills that are no longer in active use The MPCA subcontracts with various private labs to collect the samples and del
259. lyze process then to define calibration standards and blanks when come back to reprocess the data after a run has completed tried to define the blanks and calibration solutions beforehand the analysis process it turned out repeat running the sample three times and need to use three times of the sample volume of a single run and the results were confusing to me as well The process of one time run and reprocess at the end seemed work and plain to me so prefer to use this method In Method column select your predefined method file Fill down and copy to each sample unless you are intend to use different method for various samples In Sample Type column select sample for each sample unless you want to use auto QC QA function you may want to select various sample type i e QC spike QC dilution etc to have the system automatically calculate QC for you but then you need to enable QC function when you define your method file have not tried that Information in columns of Aliquot volume and Dilution to Volume are very useful when you have to dilute your samples found it very helpful when I viii c Auto Sampler vi vii reprocess my data as these values are always there and in the report of results this function save me quite some time in calculating back the original concentration of the samples So use it with care as needed On the upper part of the sampling window click button of Summary you
260. m a narrative of the analysis which notes items that are outside the laboratory QC limits and the analytical results for the collected sample In addition to the analytical results the reports include the per cent recoveries R of laboratory control sample laboratory control sample duplicates matrix spikes and standard reference material and the relative per cent differences RPD between duplicates Laboratory analytical QC acceptance criteria are detailed in Tables 4 5 and 6 Section A 7 1 1 Research Directions and Decisions The construct and need for these temperature dependent tests are based on a desire to better understand the potential seasonal variation in susceptibility of wild rice to sulfate exposure Section A 7 1 2 Inputs to the Decision The project management team Shannon Lotthammer Edward Swain and Patricia Engelking along with the Work Order Coordinator Nathan Johnson Ph D and Principal Investigator John Pastor PhD will be responsible for final decisions on the project These decisions will be informed by input from MPCA permitting personnel scientific technical expertise outputs from other investigations associated with this study such as the field studies comments from the Wild Rice Standards Study Advisory Committee and other sources of technical information Section A 7 1 3 Laboratory Analysis Due to the small volumes associated with many of the porewater samples collected in these experiments most po
261. m Method 10 MDH Appendix C Dissolved Nit 0 05 N L Modi OBEN mg N 107 04 3 D Environmental Table 2 Experimental Target Analytes in Porewater Analytical Method Location of Target Analyte Report Level RL Reference Laboratory Method Dissolved Oxygen Oto 50 mg L with 0 01 mg L Hydrolab Multiparameter UMD Civil Appendix D resolution Sonde Engineering Conductivity 0 to 100 mS cm with 0 0001 Hydrolab Multiparameter UMD Civil Appendix D unit resolution Sonde Engineering O to 14 units with 0 001 unit Hydrolab Multiparameter UMD Civil pH ye Appendix D resolution Sonde Engineering 5 to 50 C with 0 01 C Hydrolab Multiparameter UMD Civil Temperature j Appendix D resolution Sonde Engineering Ferrous Iron 0 75 mg L SM3500 Fe UMD EMI Appendix D Engineering Sulfate 0 05 mg L Modified EPA 300 1 UMD Civil Appendix D Engineering Chloride 0 05 mg L Modified EPA 300 1 UMD Civil a pp ndix D Engineering UMD Civil Bromide 0 05 mg L Modified EPA 300 1 add Appendix D Engineering Fluoride 0 05 mg L Modified EPA 300 1 UMD Civil Appendix D Engineering Sulfide 0 15 mg L SM4500 S D UMD Civil Appendix D Engineering Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 6 and A 7 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 16 of 44 Table 3 Experimental Target Analytes in Sediment Repo
262. maintenance contract with Specialty Underwriters for major analytical equipment e g the mass spectrometry instruments the ion chromatography the alpha beta radiation chemistry instruments and others The contract is managed by the State of Minnesota Department of Administration and reviewed internally by the individual testing unit supervisor Other instrumentation is maintained and repaired by the unit supervisor or experienced analyst Appendix 7 pp 49 50 contains examples of equipment maintenance logs to show representative items recorded in the LIMS B Monitoring Conditions Where required or needed for internal quality control temperatures for walk in coolers refrigerators ovens and water baths are electronically monitored and logged using an Isensix system The system operates through a series of remote radio controlled sensors with uniquely identified thermocouples at each monitoring location Acceptance ranges for each monitored area are programmed into the system to activate various alarm categories ranging from an audible alarm to a phoned alert message sent to an individual or group of individuals responsible for monitoring the storage or analytical conditions When alarms are Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 33 of 67 http fyi health state mn us phl environmental i
263. metal sulfides and is considered to be the key binding phase for controlling bioavailability of toxic metals in anoxic sediments This Standard Operating Procedure SOP is applicable to the measurement of sulfide in drinking ground and surface waters and domestic and industrial wastes This SOP can be used for sample analysis under the Clean Water Act CWA The working range is 0 01 to 2 0 mg L Dilutions are prepared for concentrations greater than 2 0 mg L The working range of the reference method is 0 01 to 2 0 mg L This SOP is compliant with the requirements of SM4500 S2 E using the Lachat QuikChem Method 10 116 29 3 A Approval letters Appendices I and II 2 0 SUMMARY OF METHOD 2 1 2 2 The method is based on the methylene blue reaction Hydrogen sulfide H2S is released by means of in line distillation under acidic conditions The gaseous H3S is separated by a diffusion cell and then absorbed by a sodium hydroxide solution The method does not recover sulfide from insoluble matter such as CuS or suspended solids Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 3 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc X M AAD EEE EQ 2
264. mgyL den 5 maL i 8 gt i i fi i 0 5359 1 i 1533 0 0 5 Time s Method Detection Limit for Nitrate Nitrite using a 0 005 mg N L standard MDL 0 0005 mg N L Standard Deviation s 0 0002 mg N L Mean x 0 054 mg N L Known Value 0 005 mg N L File Name 12 2 mdl 21 Acq Date 2 Dec 2010 2 986 E E E g E amp amp A E B a a a e 3 e 2 E 2 03 0 9980 mg L 1 002 mg L 0 9997 mg L 0 9965 mg L Volts i 19540 Time s Precision Data for Nitrate Nitrite u using a 1 0 mg N L standard RSD 0 40 Standard Deviation s 0 004 mg N L Mean x 1 00 mg N L Known Value 1 00 mg N L File Name 12 2 cal support Acq Date 2 Dec 2010 10 107 04 3 D Page 33 2 Dec 2010 sat dio ia 0 4 ppm 1534 E E E E E amp amp amp amp amp amp amp al Yr ME Ss hd S a S S S i 0 4022 0 4026 0 398 0 3981 03993 0 400 0 3931 0 398 0 3303 2 0 5408 Time s ae 2 mri eer Precision Data for Nitrate Nitrite using a 0 4 mg N L standard RSD 0 90 Standard Deviation s 0 0036 mg N L Mean x 0 40 mg N L Known Value 0 40 mg N L File Name 12 2 cal support Acq Date 2 Dec 2010 j i i 0 002269 mg L 4 001072 mof 38364 mafl m Time s 2980 0 Carryover Study Two 2 0 mg N L standards fo
265. mm test tubes use once and discard Disposable 5ml safety lock syringe and needles use once and discard Vortex mixer Acid Volatile 6 8 1 60 mL Teflon vials 6 8 2 33 mL Teflon transfer caps 6 8 3 0 125 OD x 062 Teflon tubing 6 8 4 Flow meters 6 8 5 Multi position Stir Plate 6 8 6 High purity nitrogen 6 8 7 50 mL plastic digestion tubes and caps 6 8 8 Drying oven equipped with digital thermometer for operation at 95 C and 180 C 6 89 Desiccating cabinet 6 8 10 Moisture indicating desiccant Drierite 97 CaSO4 CASH 778 18 9 and 3 CoCl CAS 7646 79 9 6 8 11 Heat resistant trays 6 8 12 57 mm Aluminum weighing dishes or equivalent Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 6 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc 6 8 13 Forceps 6 8 14 Stir plate 6 8 15 Balance data transfer software i e Collect 6 1 6 8 16 Excel spreadsheet template with proper calculations 7 0 REAGENTS AND STANDARDS 7 1 7 2 7 3 7 4 7 5 7 6 7 7 7 8 19 7 10 Reagent Water ASTM Type I or equivalent with resistivity gt 16 mega ohm cm at 25 C and free of the analyte sulfide Only Analytical Reagent AR grade or American Chemical Society ACS grade chemicals should b
266. mple type and reactivity of reduced sulfur compounds present in the sample AVS acid volatile sulfur CRS chromium reducible sulfur Safety The following section regards sound laboratory techniques safety practices and manners You are responsible for following these procedures The chemicals glassware and equipment are potentially hazardous Lab staff must specifically train you before beginning the procedure Required personal protective gear gloves and safety glasses must be worn at all times You must wear closed toe shoes and long pants If you have long hair make sure to tie it back If you are found without any of these required personal safety devices you will relieved of duties All sample prep work that involves vanadium penoxide should be conducted in a fume hood while wearing a lab coat goggles and nitrile gloves Anode Solution 30 Pyridine Acute and Chronic Effects POISON Irritation to contact area drowsiness headache unconsciousness anorexia fatigue muscle cramps or incoordination nausea vomiting dizziness diarrhea sweating CNS depression impaired vision blindness difficult breathing cardiac depression liver and kidney damage dermatitis Inhalation Irritant narcotic Skin Absorption Irritant sensitizer narcotic Eye Contact Irritant Ingestion Narcotic toxic Signs and Symptoms of Exposure Nasal and throat irritation with unpleasant taste in mouth Diziness drowsiness and headache
267. mpling oiu cede poc och RR eie cute iam EEA E E E pU aurum lotes E Bou ftos 24 Sample Custody Handling and Tracking esee eene 25 Re cerving HOUrS 3 coo tdi diem pads 25 Sample Acceptance Rejectionr Criterio poco poa ee NIE 25 Civil or Criminal Chain of Custody Procedures eese 26 Data Records for Custody Samples sete terit desc re Rte ba gn 28 Sample Cus tO tas six scu cor ridi aont soe EU eae di tomb UP D REORUM E E De NUS Cs 28 Additional Instruction id etie beer retenue Ia da REF PRO a dH SE RR VAT Fe PER 28 Sample rc ido 29 Subcontracting of Analytical Services eese nnns 29 Sample Storage cuit tatio A A T 30 Sample Disposal ii ad 30 Re cords RetentloDsais onsec id E ae naaa 31 Data Qualty ODIe eH V Sereni a tc 31 Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 4 of 67 http fyi health state mn us phl environmental index html 10 0 11 0 12 0 13 0 14 0 15 0 16 0 17 0 Analytical PEOCE MIES di AA a 31 Equipmentand SUDD IGS cari a etnies Ml Dae used at 32 Manten edo ge tat tas dedita onion 32 Monitoring Conditoris eem iode is ii 32 Procurementof Supl lo e o dr 33 Calor MERE i 34 Analytical Balances rin di tii 34 A ma ease scour lv M MUSAE estu Ma lacs tei su tt E ues ue ote sen 34 Mechan
268. n Should be in correct position for TN Please note that there may condensation at the outlet of the alternate debubbler A true leak occurs around the edge of the disc with this debubbler 7 3 9 5 Check that the cadmium column is in good condition by looking at the color The color of cadmium should be black or dark gray If white precipitated material is seen in the column replacement is necessary 11 3 9 6 If acceptable duplicate peaks are produced real samples can be run Otherwise adjust the timing and troubleshoot or perform maintainence on the system until it is in good condition 12 DATA ANALYSIS AND CALCULATIONS 12 1 Calibration is done by injecting standards The data system will then prepare a calibration curve by plotting response versus standard concentration Sample concentration is calculated from the regression equation 12 2 Report only those values that fall between the lowest and highest calibration standards Samples exceeding the highest standard should be diluted and reanalyzed 12 3 Report results in mg N L 10 107 04 3 D Page 13 2 Dec 2010 sat 13 METHOD PERFORMANCE 13 1 13 2 The method support data are presented in Section 11 This data was generated according to a Lachat Work Instruction during development of the method Although Lachat Instrument publishes method performance data including MDL precision accuracy and carryover studies we cannot guarantee that each laboratory will
269. n A 7 6 Definitions of Precision Accuracy Representativeness Comparability and Completeness 18 Section A 8 Specialized Training Certifications ooooocnncnnccnooncoonconoconoconcco nono nonononn nono conc n non nnnn nano nennen nennen 20 Section A 8S 1 ds A 20 Section A 9 Record Kepa ini 20 Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 2 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 6 of 44 Section B Data Generation and ACQUISItION ooooocononoconononocononononnnonnnonnnonn nennen eene emet tne tene tene neee 21 Section B 1 Experimental Design and Sampling Process Design sene 21 Section B 2 Sampling Methods otitis 24 Section B 3 Sample Custody diante nie o e Ede eot Re dedo eves herbae tede en 27 Section B 3 1 OYerview eiii pie 27 Section B 3 2 Microcosm Sampling Custody Procedures esee 27 Section B 3 3 Laboratory Custody nene teet penetret o tpe neret eR dadas 27 Section BA Analytical Methods eR ERR ec eaoten gem en oS 28 section B5 Quality Control ie REESE pili 29 section B5 ALOE Types it 29 Section B 6 Instrument Equipment Testing Inspection and Maintenance see 32 Section B 6 1 Laboratory Equipment eet peser ter pe e eH qge feries 32 Sec
270. n Experiment Ouality Assurance Project Plan Section No A 7 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 18 of 44 Section A 7 4 Matrix Spike and Laboratory Control Samples A laboratory may use Matrix Spike MS and duplicate MSD or Laboratory Control Sample LCS and duplicate LCSD recoveries to measure accuracy in the analyses depending on their laboratories QA CQ procedures Laboratory generated limits for spike recoveries are used in validation of data when required Refer to the laboratory s Quality Assurance Manual QAM if available or specific analytical method located in the appendix of this QAPP for details of this QC activity Section A 7 5 Laboratory Activities The quality assurance objectives for accuracy precision completeness representativeness reporting limits and comparability to be met by the laboratory are described in the laboratory s OAM if available Section A 7 6 Definitions of Precision Accuracy Representativeness Comparability and Completeness Where possible laboratory precision is measured through the collection and analysis of duplicate samples The result for the duplicate sample is compared to the result of the known sample The relative percent difference RPD between the known sample result and the duplicate sample result is calculated according to the following formula RPD Sample Conc Duplicate Conc 200 Sample Conc Dupl
271. n No B 1 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 23 of 44 Initial Characterization Subsamples of sediment for the characterization of initial conditions will be collected after the first initial equilibration phase of the experiment from sacrificial microcosms using 1 2 diameter polycarbonate tubes Sacrificial microcosms were treated identically to experimental microcosms during Phase but not sampled for pore water chemicals Sediment samples will be sectioned analyzed for the same parameters as previously collected field cores SO4 pH iron sulfide DOC AVS Microcosm Experiment Design Experimental treatments The experimental treatments will consist of incubating replicate 3 microcosms from each site at 21 degrees C and 4 degrees C with overlying water amended with sulfate and a tracer An overlying water depth of 10 cm will be carefully monitored and recorded in order to facilitate accurate flux measurements An initial 1 month laboratory equilibration phase will take place with site water maintained at in situ sulfate concentrations and chloride as a tracer The second phase will be a 2 month sulfate dosing phase with overlying water amended and maintained with 300 mg L sulfate plus bromide as a tracer The third experimental phase will involve a 2 month return and maintenance of in situ sulfate concentrations in the overlying water and fluoride as a tracer Figure 5 includes a s
272. n a 1 L volumetric flask containing approximately 900 mL water add 49 g potdsstiim persulfat K25203 Add 10 g disodium tetraborate decahydrate Ne7B70 10H20 Add a magnetic stir bar dissolve and dilute to the mark with DI Na ul water Invert to mix Gentle heating or a warm water bath is required for complete oe Y dissolution M By Weight To a tared 1 L container add 975 g DI water and 49 g potassium y Td persulfate K25203 Add 10 g disodium tetraborate decahydrate Na2B407 10H20 Add a magnetic stir bar sir until dissolved Gentle heating or a warm water bath is v required for complete dissolution Potassium persulfate is known to have nitrogen contamination There are two suggest this contamination 1 re crystallize the potassium persulfate or 2 use cadum persulfate If you choose to use sodium persulfate use 43 g of Na2S20s instea g of K28205 Potassium persulfate re crystallization procedure 1 Dissolve 100 g of potassium persulfate in approximately 600 ml of Milli Q previously heated to 60 C Use a medium sized stir bar and a 1000 mL flask 2 Filter the solution rapidly through a sintered glass funnel 10 107 04 3 D Page 4 2 Dec 2010 sat 10 11 12 Rinse the 1000 mL flask Poor filtrate back into the flask used to heat the potassium persulfate solution Cool solution to about 4 C by placing the flask in ice water Whirl the flask continuously to prevent the solution from freezing Filter
273. n button on interface of Elan6000 Switch to the Service tab and click plasma tab located at the bottom of the interface Closely watch the plate voltage and when it jumps to 3899 V this takes about 60 s from the time the start button is pressed press the grill ignitor button i If everything works well the plasma will pup on when the igniter button is clicked and you can see the bright blue plasma from the viewing window If the plasma is not on wait till this ignition sequence end by observing the values on plasma tab turn back to normal this process normally takes about 1 2 minutes switch back to front panel tab and check everything is green Repeat steps d f to ignite the plasma if fail more than 5 times consult Bryan for help If Bryan is not here run trouble shutting according to manual P6 3 g Once the plasma is started allow the instrument to warm up for 30 45 min normal use this time to prepare for standard solutions 4 Optimizing and Tuning the system a C After system warm up place the end of the sampling tube into the tuning solution Don t put the sampling tip into the whole bottle of tuning solution as it will contaminate it but to pour some out into a second container such as a 50 ml centrifuge tube and put sampling tip in it X y alignment The target of this step is to find the strongest signal that the system can produce by alighting the position of sampling introducin
274. n external vendor to ensure accurate and precise delivery of measured volumes of standards The Quality Assurance Officer is responsible for contracting a qualified vendor to calibrate pipettes to specified ranges determined by individual manufacturers The QA Officer also is responsible for tracking verifying calibration results and maintaining accurate records of determined calibrations D Analytical Instruments Calibration procedures for analytical instruments are specified in the laboratory s standard operating procedures At a minimum the calibration procedures meet the requirements of the approved method SECTION 13 0 QUALITY CONTROL A QC in the QA Manual and in SOPs The QC policies and procedures listed herein are standardized for use in this laboratory Employees in this laboratory recognize that in some cases a particular USEPA approved method and in turn a particular Standard Operating Procedure SOP may describe different QC policies and procedures In those situations the QC policies and procedures in the SOP supersede those in this Quality Assurance Manual B Detection Level Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory i Revision 9 Effective Date Date of last signature Page 35 of 67 http fyi health state mn us phl environmental index html The policy and procedure for conducting a Detection Level Study are described in Ap
275. n of the method Current control limits for precision are on file in the laboratory If either the difference or the RPD for a set of duplicates falls outside of the applicable control limits the reason for the out of control condition is investigated and the duplicate analyses are repeated 9 2 10 1 Calculate the relative percent difference of the duplicates using the following formula S D x 100 S Dy2 Where S 7 concentration of sample D concentration of duplicate sample 92 10 2 Duplicate acceptance criteria None RPD lt 10 Concentration Range RL to 10xRL 10xRL to highest calibration std 9 2 10 3 If the duplicate concentration is between the RL and 10xRL and the RPD is greater than 10 the qualifier QH is added to the duplicate RPD between sample duplicates not within acceptance limits Analyte concentration in the samples too low for proper evaluation 9 2 10 4 Ifthe duplicate fails to meet the above criteria the samples should be reanalyzed to verify poor duplicate analysis RPD If the repeated duplicate is still not within acceptable limits the samples must be reported with a qualifier identifying the sample analysis result as yielding poor duplicate analysis RPD Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 17 of 31
276. n should be taken 9 6 Reagent and Standard Verification All reagents and standards are verified prior to sample analysis by the analysis of ICV ICB SCV CRL CCV and CCB Acceptable QC results along with an acceptable calibration curve demonstrate that all reagents and standards are verified for use 10 0 CALIBRATION AND STANDARDIZATION 10 1 Prepare a series of 7 calibration standards and a calibration blank by diluting suitable volumes of calibration standard solution as described in Section 7 16 10 2 Setup the manifold as shown in Section 17 If necessary refer to the Lachat manual for instrument operation 10 3 Process calibration standards and calibration blank and calibrate the instrument as described in Section 11 Read calibration standards and calibration blank in descending concentration on the Lachat 10 4 Prepare calibration standard curve by plotting instrument response against concentration value The curve used must be 2 order polynomial and not Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 18 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc M M HLA forced through zero The calibration standard curve will be fitted to the calibration standard solutions concentrat
277. nalysts and refilled weekly Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 34 of 67 http fyi health state mn us phl environmental index htmi SECTION 12 0 CALIBRATION A Analytical Balances Laboratory staff members maintain the analytical balances Staff checks the calibration daily by analyzing weights that are near the approximate weight of material that will be determined An external vendor calibrates the analytical balances annually to NIST traceable standards The Quality Assurance Officer is responsible for contracting a qualified vendor to calibrate the analytical balances to specified ranges determined by individual manufacturers The QA Officer also is responsible for tracking verifying calibration results and maintaining accurate records of calibration data sheets B Weight Sets The weight sets for each analytical unit are calibrated every five years by an external vendor The vendor is responsible for calibrating the weight sets and supplying MDH with a Certificate of Calibration The Quality Assurance Officer is responsible for tracking sending out verifying weights are returned within acceptable limits and maintaining accurate records of Certification of Calibration certificates for each weight C Mechanical Pipettes The mechanical pipettes are calibrated semi annually by a
278. nce computer software and Excel spreadsheet enter dry weight in Element 12 0 DATA ANALYSIS AND CALCULATIONS 12 1 12 2 12 3 12 4 12 5 12 6 12 7 Calibration is accomplished by injection of standards The data system will then prepare a calibration curve by plotting instrument response versus standard concentration Sample concentration is calculated from the regression equation Multiply results by appropriate dilution factor The method detection limit MDL is calculated as described in Section 9 4 The current MDL value is on file in the QA Office The minimum report level is 0 01 mg L Results are reported in mg L to three significant figures Sample results and quality control data are transferred electronically to the Element Database for review by the analyst Report only those values that fall between the lowest and highest calibration standard Samples exceeding 2 0 mg L are diluted and reanalyzed Results reports are reviewed by Unit Supervisor or designee according to established procedure prior to transmittal to client Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 230131 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc Ha 13 0 PERFORMANCE 13 1 Information pertinent to our laboratory s performanc
279. nce Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 11 of 67 http fyi health state mn us phl environmental index html volumes of the samples or sample extracts The internal standard s is added to all samples blanks and standards at a constant amount should not be present in the original test samples in interfering amounts and should behave similarly to the target analyte Laboratory Control Sample LCS An aliquot of reagent water or other blank matrix known to be free of interfering amounts of target analytes or other interferences to which known quantities of the target analytes are added in the laboratory The spiking solution for the LCS should be prepared from the same source as the calibration standards It is prepared and analyzed exactly like a sample Its purpose is to verify that the procedure is in control and that the laboratory is capable of making accurate measurements A LCS is also known as a Laboratory Fortified Blank LFB Laboratory Control Sample Duplicate LCSD A second aliquot of reagent water or other blank matrix known to be free of interfering amounts of target analytes or other interferences to which known quantities of the target analytes are added in the laboratory The LCSD is prepared the same as the LCS The LCS and LCSD are treated exactly as samples throughout the laboratory procedure The percent recoveri
280. nce Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 23 of 67 http tyi health state mn us phl environmental index html Training is presented through lectures demonstrations and self directed media Participants are required to sign an attendance log or a statement acknowledging that they have completed the training requirement Training records are maintained by the Radiation Safety Officer The laboratory s Radiation Emergency Plan is available to all employees on the PHLD Safety website http fyi health state mn us phl safety index html 3 Initial Demonstration of Capability for laboratory analysts Analysts who are learning analytical standard operating procedures SOPs receive technical training from the supervisor the lead worker or an experienced analyst for all assigned procedures Initially the trainer demonstrates and explains the process to the trainee After observing the trainer the trainee performs the analysis while the trainer observes The analyst trainee experienced analyst trainer and supervisor document the demonstration of capability and submit a completed training record to the Quality Assurance Officer Appendix 2 p 43 displays the Training Record for an Individual Standard Operating Procedure Note Section 13 0 Quality Control pp 32 33 describes the policies procedures and worksheets germane to the
281. nd allow the system to equilibrate until a stable baseline is achieved Place samples and or standards in the sampler Input the information required by the data system such as concentration replicates and QuikChem scheme See Section 17 Calibrate the instrument by injecting the standards The data system will then associate the concentrations with the instrument responses for each standard 11 3 SYSTEM NOTES 11 3 1 11 3 2 11 3 3 11 3 4 11 3 5 For information on system maintenance and troubleshooting refer to the Troubleshooting Guide in the System Operation Manual This guide is also available on request from Lachat Allow more than 20 minutes for the heating unit in the sample prep module to warm to 105 C Tubing crimp formation has been observed in the past with the PTFE manifold tubing when no liquid is running through heater tubing and the tubing is allowed to bake Running liquid through the heater whenever the temperature is above 80 C is necessary Since the digestion occurs prior to injecting the sample and since there is an air segment between the sample and the sampler wash solution the valve and sample timing parameters are critical It is important to verify that the center of the sample zone is injected Because the blank peak in this method is due to nitrogen in the buffer and persulfate solid reagents it is important to use the best purity available Digestion efficiency should be v
282. nd the instrument response to a single analyte Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 8 of 67 http fyi health state mn us phl environmental index html Calibration Range The working range between and including the lowest and highest calibration standards from which the value of unknown samples can be determined Calibration Standard A substance or reference material used to calibrate an instrument Calibration Verification Standard CVS A standard analyzed with an analysis batch that verifies the previously established calibration curve and confirms accurate analyte quantitation for all samples The concentration of the CVS should be near the mid point of the calibration curve Also known as a Continuing Calibration Verification CCV Certified Reference Material CRM A reference material one or more of whose property values are certified by a technically valid procedure accompanied by or traceable to a certificate or other documentation and which is issued by a certifying body Chain of Custody C of C The procedures and records that document the possession and handling of samples from collection through disposal See Section 8 0 of the Quality Assurance Manual for more details Chain of Custody Form A record that documents the possession of the samples from the time
283. nd the refrigerator in room L100 for samples that may have arrived after hours Tasks to be performed throughout the day Check email and voicemail as needed Process and deliver samples to the labs Bring data sheets and log lists to clerical tios so they receive a steady flow of work Tasks to be performed first thing in the morning on the first workday after any day s off The weekend analysts leave the data sheets on the counter in Sample Receiving Print a log list for the samples that were processed on the weekend or day s off Compare the data sheets with the log Make corrections to data sheets or initial entry data as needed If any samples were past hold time check email for responses from clients Check rejection pending list and make appropriate changes Tasks to perform at the End of Each Month Prepare monthly report using sample receiving counts from Ed Add up bottle orders for the month and send report to Ron Tasks to Perform at the Beginning of Each Calendar Year Reset the Rapidprint numbering machine to Y Y Y00000 so the first number to print is YYY00001 The Y s represent the last three numerals of the current year Example For 2006 the machine was set at 00600000 so the first number to print was 00600001 Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 7 of 57 COMPUTER OPERA
284. ndex html silenced either locally or remotely the system requires documentation of the user identification and a comment This information is stored in the Isensix database along with the system s automatic log of the resulting action Pre programmed actions are in place to allow the system to auto correct when warming or cooling is required Data can be retrieved from the database either in tabular or graphic form Thermocouples are calibrated on site by an Isensix Inc technician once a year In instances where monitoring or control is specified in a test method or by regulation the laboratory shall meet and document adherence to those monitoring requirements C Procurement of Supplies Procedures for the procurement of chemicals and supplies and information on safety and proper handling of chemicals are documented in the Public Health Laboratory Division PHLD Chemical Hygiene Plan as posted on the division s intranet site http fyi health state mn us phl safety chemhygieneplan pdf For high turnover consumable laboratory supplies the purchasing system automatically re stocks the item at a pre set interval or to maintain stock levels For specialty items such as gas chromatography columns the unit supervisors or their designees submit requests to purchasing personnel as needed Each unit monitors its own stock of supplies and orders more when needed Shared gases which are piped through the laboratory from the loading d
285. ndium of Chemical Terminology 2nd ed the Gold Book Compiled by A D McNaught and A Wilkinson Blackwell Scientific Publications Oxford 1997 XML on line corrected version http goldbook iupac org 2006 created by M Nic J Jirat B Kosata updates compiled by A Jenkins ISBN 0 9678550 9 8 doi 10 1351 goldbook Last update 2009 02 17 version 2 0 3 Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 41 of 67 http fyi health state mn us phl environmental index html SECTION 17 0 APPENDICES The Table of Contents for the Appendices is presented on p 5 of this Quality Assurance Manual The appendices are on pp 38 63 Minnesota Department of Health Public Health Laboratory Division Environmental Laboratory Quality Assurance Manual Filename qao001 Revision 9 Effective Date Date of last signature Page 42 of 67 http fyi health state mn us phl environmental index html Appendix 1 PHLD organizational chart focusing on the environmental testing units Division Director pL i id Assistant Division Director Technical Services Unit Clerical Services Unit JL LLL Environmental Lab Accreditation Program F7 E I ML Newborn Screening Section Environmental Laboratory Section 2 22 o 4 Environmental Laborator
286. ne anode solution phosphoric acid and vanadium pentoxide neat solid All reagents are pre made by manufacturer which requires no reagent preparation by lab technicians Equipment List All necessary equipment is listed in the catalog with the exception of stainless steel spatulas and a squeeze bottles for methanol Procedure Instrument Set Up 1 Open the left furnace and check on the status of the reduced copper It should appear shiny and bright Blackened copper has been consumed Either replace the copper with fresh reduced copper or reduce the existing copper with the procedure detailed below Close the furnace 2 Turn on the left and right furnaces Resting temperature is 5000C Heat the furnaces slowly Increment in 100PIC steps to set point temperatures The right furnace setpoint is 10500 the left furnace set point is 825PIC 3 Connect gas lines Nitrogen Ultra High Purity should be delivered at a pressure of 7 10 psi and then further adjusted to a flow of 100ml min using the right hand regulator on the front of the combustion furnace Oxygen Ultra High Purity should be delivered at a pressure of 7 10 psi and further adjusted to a flow of 100 ml min using the left hand regulator on the front of the combustion furnace Hold the reset button in for three seconds while adjusting the oxygen flow a After setting the flow the instrument will periodically admit oxygen to the combustion tube you ll hear a clicking sound
287. nen 36 Section C 2 1 MPCA Corrective Actions eese nne nennen tenete tren tnnt nennen enne enne 36 Section C 2 2 Laboratory Corrective Actions ern siani sisp aee e noc nonn nono nono n ran cnn ono EEA EEEN eA 36 Section C 2 3 Laboratory Reports nono no eene nono nono enne tete eoori nE oae tren trennen 37 Section C 2 4 Reports to Management eene eene eene neente tree teee trennen trennen 37 Section D Data Validation and Usability eese eene eren rennen eene nete tenerent 38 Section D 1 Data Reduction Verification and Validation occconooonoonconnnnnnnononnnnnccnononnnnononcnnonnnnonanoncnnnn 38 Section Ll Data Reduction RE rupe uota m n tct 38 Section D 1 2 Data Verification Methods sssesssssseseeseeeeen enne eene nennen rennes 38 Section D 1 3 Data Validation Methods sees enne rennen nennen enne 39 Section D 2 Reconciliation with User Requirements sess rennen eene nennen 39 Section D 3 References eue he Dn emet te ten e ei t i RR RO RH ente 39 Appendix A Table OL Acronyms An 40 Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No A 2 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 7 of 44 Appendix B MDH Environmental Laboratory QA Manuals eese nennen nennen 41 Appendix C MDH Environmental Laboratory St
288. nesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 9 of 67 http fyi health state mn us phl environmental index html special causes of variation must be suspected Control limits are usually defined as three standard deviations either side of the mean Corrective Action The action taken to eliminate the causes of an existing nonconformity defect or other undesirable situation in order to prevent recurrence Daily Applies to the days during which the analytical process including preparation of samples is performed Data Quality Objectives DQO A statement of the appropriate type of data and overall level of uncertainty that a decision maker is willing to accept in results derived from analytical data DQOs are often expressed in terms of precision accuracy reliability representativeness and comparability Data Reduction The process of transforming raw data by arithmetic or statistical calculations standard curves concentration factors etc and collation into a more useable form Data Validation A process used to determine if data are accurate complete or meet specified criteria Detection Level or Detection Limit DL The lowest concentration or amount of the target analyte that can be identified measured and documented with confidence that the analyte concentration is not a false po
289. ng Standard Operating Procedure for using ICP MS ELAN6000 Contents A let ilec d DINEILDE D EIL E A E D De OD Before turning on the system here is the system checkup list Turning on Plasma itecto at Optimizing and Tuning the system tre tte een Ren E ER Ran EE ERE SERERE TER RE ERA RUE Defining Method files Consult EIAN6000 Software Guide P47 62 ooocccococonocococanocooannononanononnnnnns 2 3 4 5 6 Deftinirig sample ile rte toten dote cedente aoc estates R E E REEE LM A O ci 8 Preparing standard solutions and samples esses eene nnne nnn nnns nnn an 9 Data processing inerte D E Em iret eee tee doe et eee ieee 10 VIEWING ThE result reports eicere ettet ineo eet evene catena eee eee xtd eaae eso d desean sioe tco do deta 1 A basic mindset An appropriate mindset of using the Elan6000 ICP MS in the Research Instrumentation Laboratory of MWAH at UMD include a Plan several days in advance and contact Bryan Bandli at MWAH 55 to ensure argon is present and equipment is functioning normally Plan at least 2 hours to starting and warming up the ICP MS system Make a clear plan on how many samples to run and an estimation of the range of concentration of your samples including dilutions if necessary 2 Before turning on the system here is the system checkup list a Power i ii b Argon i ii c Tubing If the system has been used normally the lab manager Bryan Bandli wi
290. ng any areas in which corrective action is needed After correction of any deficiencies the laboratory will respond to the USEPA to document the corrective actions taken Certification for analyses in drinking water is issued by the USEPA Region 5 Office of Water A copy of the current drinking water certification is included in Appendix 12 pp 61 64 The document is entitled Enclosure A Laboratory Certification Summary Minnesota Department of Health May 5 7 2008 D Corrective Action Policy A corrective action form is required when departures from the established quality assurance and quality control policies and procedures occur or in the event of a proficiency test PT failure Appendix 13 pp 65 66 contains a corrective action form for use with a non conformance of work or a failed PT sample All non conformance activities and PT failures require an investigation and documentation of potential causes and corrective actions Corrective actions are initiated when the Quality Assurance Officer assigns a corrective action form to an occurrence of non conforming work after notification of the event by an analyst or Supervisor The Quality Assurance Officer may assign an investigator who is independent of the analyst or Unit Supervisor The laboratory analyst or designated investigator completes and signs the Corrective Action Form submits it to the Unit Supervisor for review and signature and returns it to the Quality Assurance Office
291. ngs Provide direction for analytical requirements Perform final review of analytical data reports to ensure requirements are met Review and approve the QAPP including subsequent revisions Section A 4 8 MDH Public Health Laboratory Manager Paul Moyer The MDH Public Health Laboratory Manager will Provide administrative direction to assigned staff and to the MDH QA Officer as needed Implement the elements of the Project as well as any required quality control measures Manage the budget to assure that goals are met and funds and resources are responsibly allocated Review the QAPP including subsequent revisions Section A 4 9 MDH QA Officer Shane Olund The MDH QA Officer will Monitor and evaluate laboratory analytical activities as they pertain to this QAPP Conduct and document internal audits of laboratory procedures Review laboratory SOPs Schedule and document pertinent Method Detection Limit studies Maintain staff training records Maintain the laboratory corrective action program Review the laboratory elements of the QAPP Section A 4 10 MDH Laboratory Staff The MDH Laboratory Staff will Ensure analytical procedures are followed Document the analysis and observations Identify and report analytical problems to the Unit Supervisor and QA Officer Manage the budget to assure that goals are met and funds and resources are responsibly allocated Provide direction for the daily work activities Provi
292. nity bacteriology samples HB community fluorides l HC community code used for most other types samples Non community PWS ID s begin with a 5 Codes used are HD HU and HW Some non community facilities use more than one code Contact the EH Rep for assistance in such cases as code assignment is not determined by sample type but rather by facility type HD non community licensed facilities HU non community non licensed HW non community non transient Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 16 of 57 ADMINISTRATIVE CODES Administrative codes are used in the LIMS system to indicate various unusual changes to samples The administrative codes that are used by Sample receiving are 981 993 994 995 997 and 999 Codes 981 and 995 Samples Sent Out These codes are added to samples when all or some of the requested analyses will be sub contracted to another lab They canbe added during the initial data entry or after the fact through the editing screens Code 993 Analysis Canceled This code is used when some or all of the requested analyses need to be canceled after they have already been logged in This may happen if the submitter asks that some analyses be canceled or if a problem is n ticed in the lab that precludes testing e From the editing screen add the code 993 to the s
293. ntal Laboratory Handbook The handbook is posted at both the internal website Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 25 of 67 http fyi health state mn us phl environmental index html http fyi health state mn us phl environmental index html and the external website http www health state mn us divs phl environmental handbook internet envhandbook html SECTION 8 0 SAMPLE CUSTODY HANDLING AND TRACKING A Receiving Hours The laboratory accepts samples at the loading dock area between the hours of 7 a m and 6 p m or from 8 a m to 4 30 p m for civil or criminal chain of custody samples Monday through Friday The laboratory recommends pre arranged drop off schedules for all samples requiring special receiving conditions e g civil or criminal chain of custody samples and sample deliveries outside regular hours B Sample Acceptance Rejection Criteria For all samples the person delivering the samples submits the appropriate sample analysis request forms a k a chain of custody forms Information to be included on the form includes the appropriate analysis and project codes the sample collection dates and times the date of delivery to the laboratory the field numbers the name or identification number of the site from which the samples were collected and whether the
294. ny data issues identified by the laboratory or the MPCA The report points out any limitations on the use of the data to decision makers Section D 3 References 1 U S Environmental Protection Agency 2001 EPA Requirements for Quality Assurance Project Plans QA R 5 EPA 240 B 01 003 Office of Environmental Information 2 U S Environmental Protection Agency 2002 Guidance for Quality Assurance Project Plans QA G 5 EPA 240 R 02 009 Office of Environmental Information 3 USEPA Contract Laboratory Project January 2010 National Functional Guidelines for Inorganic Superfund Data Review USEPA 540 R 10 011 OSWER 9240 1 51 Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No Appendix A Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 40 of 44 Appendix A Table of Acronyms AVS CA COC CFR 96D DQO EPA FOC LacCore LRC LIMS MDH MPCA MS PE PM QAC QAO QAM QAPP QA QC QMP RSD RPD SAP SOP SRF UMD UMN Acid Volatile Sulfide Corrective Action Chain of Custody Code of Federal Register Percent Difference Data Quality Objectives Environmental Protection Agency Field Operations Center National Lacustrine Core Facility Limnological Research Center Laboratory Information Management System Minnesota Department of Health Minnesota Pollution Control Agency Matrix Spike Performance Evaluation sample Proj
295. ny required quality control measures Review and approve the QAPP including subsequent revisions Manage the budget to assure that goals are met and funds and resources are responsibly allocated Oversee the preparation of all Project reports to include measurable benchmarks problems encountered regarding QA QC and recommended changes in procedures Review all project deliverables and strategies Provide direct supervision and project assignment to assigned staff Provide technical direction for the preparation of work plans and the tasks to be performed Review invoices to ensure proper billing for services provided by the contractor s Interpret analytical data generated for the project Represent the data using modeling procedures approved for use in the project Represent the MPCA in meetings Publish the results from the project in peer reviewed journals Review and approve the Quality Assurance Project Plan QAPP including subsequent revisions Section A 4 6 The MPCA Contract Manager Patricia Engelking The MPCA Contract Manager will Implement the elements of the Project as well as any required quality control measures Manage the budget to assure that goals are met and funds and resources are responsibly allocated Review the QAPP including subsequent revisions Provide technical direction for the preparation of work plans and the tasks to be performed Review invoices to ensure proper billing for services provided by
296. o instructions provided by the manufacture Use 0 025 M sodium hydroxide reagent as diluent and add alkaline antioxidant reagent at 1096 of final volume 7 19 1 1 Hydrochloric Acid Add an equal volume of concentrated HCl 37 to reagent water This reagent is prepared by designated laboratory personnel and used to acid rinse glassware 7 20 Allreagents should be discarded if precipitate or growth appears 7 21 All reagents and standards are verified as described in Section 9 6 SAMPLE COLLECTION PRESERVATION SHIPMENT AND STORAGE 8 1 Samples are collected in 125 mL glass serum bottles and stored at 4 C 2 C prior to analysis 8 2 Bottle preservation and preparation 8 2 1 8 2 2 8 23 8 24 8 2 5 8 2 6 8 2 7 8 2 8 0 2 mL Zinc Acetate preservative 0 5 mL sodium hydroxide NaOH preservative and magnetic stir bar are added to each serum bottle Each bottle is purged with high purity nitrogen gas for 30 seconds and capped with a 20 mm septum stopper and a 20 mm tear off seal Each bottle is then weighed using an analytical balance and initial weight is recorded on label of bottle After samples are collected bottles are weighed using an analytical balance and weight is recorded on label of bottle Using a Safety Lok syringe 5 6 mL of Alkaline Antioxidant Reagent is injected into each bottle Bottles are placed on stir plate for at least 1 hour to dissolve any particulate Each bottle is wei
297. ocation with access restricted to a smaller number of authorized personnel l Additional information entered into the chain of custody logbook includes chain of custody record number site or I D number matrix sample collector all types of bottles received and whether the samples are involved in a civil or criminal investigation For the analysis of samples associated with criminal investigations only designated analysts receive the samples thereby limiting the number of people handling the samples The analysts are responsible for the care and custody of the samples once they are in their possession Analysts should be prepared to testify that the samples were in their possession and view or locked in a secure area from the time they received the samples until they returned the samples to be placed in the appropriate secured storage area Aliquots of the original samples undergoing analysis remain within the secured areas of the laboratory at all Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 28 of 67 http fyi health state mn us phl environmental index html times Upon completion of the analytical work the samples are returned to the secured storage area The date and time of the return are recorded in the chain of custody log along with the initials of the analyst In the event
298. ock area have re stocking procedures pre arranged with the vendor The laboratory has the ability to request emergency purchases which can be delivered overnight Specialty gases are categorized as bulk gases piped from the loading dock area through the building manifold gases piped from the gas manifold storerooms through the building and point of use gases Argon and nitrogen are supplied as bulk gases The argon tanks are assembled into a primary and a backup bank of tanks When the primary tanks are emptied the manifold automatically switches to the backup tanks New argon tanks are delivered every two weeks or as needed The liquid nitrogen supply is monitored remotely by the vendor When the tank level falls below a pre set mark the vendor is automatically notified via phone that re stocking is needed The gas manifold room has both a primary and a backup bank of helium gas cylinders When the primary tanks are emptied the manifold automatically switches to the backup tanks and a light indicates that the backup tanks are in use The laboratory routinely monitors the gas usage rate and takes corrective action if any possible overuse could be attributed to a leak in the system The normal turnover rate is 1 1 Y weeks per bank For selected specialty gases the cylinders are kept at the instruments and monitored regularly by the analysts For radiation chemistry the liquid nitrogen used in the gamma instruments is monitored by the a
299. od Hydrogen sulfide and acid soluble metal sulfides react with N N dimethyl p phenylenediamine sulfate to form methylene blue The intensity of the blue color is proportional to the sulfide concentration High sulfide levels in oil field waters may be determined after proper dilution Test results are measured at 665 nm Sulfide Page 3 of 4 Sulfide Consumables and replacement items Required reagents Catalog number Description Quantity Test Unit Sulfide Reagent Set includes Sulfide 1 Reagent 1mL 100 mL MDB Sulfide 2 Reagent 1 mL 100 mL MDB Water deionized 10 mL 4 liters 2244500 181632 181732 27256 Required apparatus Description Quantity Unit Catalog number Pipet serological 10 mL 1 each 53238 Pipet Filler safety bulb 1 each 1465100 Stopper for 18 mm Tube 2 6 pkg 173106 Optional reagents and apparatus Description Unit Catalog number Bromine Water 30 g L 29 mL 221120 Phenol Solution 30 g L 29 mL 211220 Stopper for 18 mm Tube 25 pkg 173125 Flask Erlenmeyer 50 mL each 50541 FOR TECHNICAL ASSISTANCE PRICE INFORMATION AND ORDERING HACH COMPANY 9 In the U S A Call toll free 800 227 4224 WORLD HEADQUARTERS Outside the U S A Contact the HACH office or distributor serving you Telephone 970 669 3050 On the Worldwide Web www hach com E mail techhelp hach com FAX 970 669 2932 Hach Company 2007 2010 2012 All rights reserved Printe
300. ode on the upper part of the bottle or vial Most organic analyses will have their own bottle so the lab doesn t need the rest of the labels Radiation samples Place one small label with just the sample number onthe samples and save the rest of the label for delivery to the lab For samples that have a paper tag put the label on the tag Duplicate sample containers Sometimes collectors will submit more than one of the same type of container for a sample In these cases write 1 of 2 or 2 of 2 on a single label and put it on each container Attach the rest of the labels to one of the containers or deliver them to the lab separately as needed OSHA samples Do not remove the samples from their bags the labs will do this Just clip the labels and paperwork to the bag containing the samples People in the labs will deal with labeling themselves PRINTING SAMPLE ENTRY LOG AND COMPARING TO DATA SHEETS After samples have been delivered to the lab print a Daily Entry Log and compare it to the data sheets 1 From the main screen select Log lists and pull down to select Daily Entry log 2 Type in the beginning and ending sample numbers for the lab sheets 3 Select the printer Labserv 2 to print the log list 4 The log will list all the sample numbers with some basic information about each one The information we are checking for is Program Code Analysis Codes Priority and Field Trip Blank As you are checking the sampl
301. ods are acceptable for NPDES compliance monitoring A good example of this is Lachat method 10 107 04 1 C Lachat Applications submitted the method for review to the USEPA requesting a letter stating that the method was acceptable for use in both NPDWR and NPDES compliance monitoring The modifications in this method allow samples to be analyzed without pH adjustment due to the high flow rate of the buffer reagent which allows the method to compensate for high or low pH samples This method adjustment falls within the flexibility allowed at 40 CFR Part 136 6 of the MUR Therefore this method is acceptable for use in NPDES compliance monitoring and no letter is required or will be issued by the EPA The EPA states that The absence of a letter does not preclude use of Equivalent Lachat methods for NPDES compliance monitoring purposes The modifications that fall within the allowed flexibility of the MUR do not require review as a Clean Water Act ATP The USEPA sent Lachat and all Regional ATP Coordinators this statement regarding this issue Due to increased inquiries on method flexibility we would like to stress ek dt tk P RII HII HUI PO FO HP HUGE B G GR EUR RU RE REGE RU VY A B EU HE Urn n n n n an n rr Rr m Regions States and permitting authorities should not expect a letter from the EPA s Office of Science and Technology OST stating that a modification that falls within the flexibility allowed under 40 CFR Part 136 6 which was added a
302. of last signature Page 24 of 57 e SAMPLE RECEIVING EQUIPMENT LABEL PRINTER We use an Epson LQ 870 printer to print sample bottle labels This printer is set up to print on 1 x 7 16 piggyback labels in rows of 3 across The labels are called piggyback because they have 2 layers of self adhesive backing A supply of these labels is kept in the MDH Stockroom item 375 0503 There are 30 000 labels box and we order 4 5 boxes at a time The correct ribbon for this printer is Nu kote BM203 Epson LQ800 A supply of these ribbons is kept in the MDH Stockroom item 375 0716 We order 2 3 boxes at a time Installing labels in the printer 1 Open the paper guides and slid the strip of labels up from underneath the printer head 2 Turn the manual feed wheel to move the labels up 3 Fit the labels over the paper guide grips and close the paper guides 4 Line up the labels by carefully turning the manual feed wheel The top of the clear plastic guard should line up between 2dabels at the perforation Installing a new ribbon 1 Make note of how the current ribbon is installed before removing it 2 Put on a pair of disposable gloves to keep ink from staining fingers 3 Remove the ribbon cartridge by pulling it out and then gently pull the ribbon from the guide 4 Lower the new cartridge into place and guide the ribbon between the printhead and the guide 5 Turn the knob in the direction of the arrow to remove
303. ompleting an internal audit the Quality Assurance Officer supplies a copy of the completed checklists which serves as the report to laboratory management and unit supervisors of any deviations from approved procedures or policies The unit supervisor or designated laboratory staff members prepare a response and corrective action plan which includes any recommendations to management that might assist in improving the quality of the data being generated If the proposed actions are acceptable the Quality Assurance Officer files a copy of the report the laboratory s response and any follow up documentation indicated in the corrective action plan Follow up audit activities are employed to verify and document the implementation of the corrective action plan The complete audit record is available for review by the USEPA Region 5 certification officer C External Audits External laboratory audits can determine adherence to established and documented sample collecting handling and documentation procedures Audits are performed at the discretion of Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 39 of 67 http fyi health state mn us phl environmental index htm the Certification Officer from the USEPA Region 5 Office of Water Results of the audits are reported by the USEPA to the laboratory identifyi
304. on 9 Effective Date Date of last signature Page 3 of 67 http fyi health state mn us phl environmental index html 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 Table of Contents Eist Of ACTODJHIS i 6 Definitions OL QC Vern a oec roe dae trol quio ies NUR a ip e NNI IER USs 6 General Lab Information and Policies eese 18 LBS VATI LY NEED E ET a santa e echec tu Susie aa 18 Facility Description and Location eter tha eret er dido 19 Building SecUbity dise tscticaccena ees phi eb Mad eae satu ett DD eam d Mie E ies 19 PONSA da 19 Quality Assurance POlicy siisa ace daa 20 Ethics POUCW ET 20 Data Practices Polla a ass 20 Computer Security Pole ara da dut idu 20 Corrective Action Policy ERE 20 PERSON MeL ia A a 20 Positions and Responsibilities 5 is pi di 20 PANNING on 21 General Employee Training for all staff sese 21 Radiation Safety Training for selected staff sese 22 Initial Demonstration of Capability for laboratory analysts sess 23 Ongoing Demonstration of Capability for laboratory analysts sss 23 Information Technology O m 23 Specifications for the Laboratory Information Management System LIMS 23 Computer Security usi die oot E hase bae utei eae eae ur ta NEP ter pere eu ooi 24 Additional Software susct A ia 24 Sa
305. on of Method Detection Limit Revision 1 11 Federal Register Vol 49 No 209 Friday October 26 1984 pp 198 204 17 0 TABLES FIGURES VALIDATION DATA 17 1 The Initial Demonstration of Capability data are on file in the QA Office the most current MDL precision and accuracy data are on file in the Environmental Laboratory 17 2 Sulfide Manifold Diagram Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 25 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc Pap fiov Probe Kio Pirevalvo distillation LLL oriugsPubile Hate Flow celi ye ES Hote 2 To waste To waste n mt 75 ei x 5 nua Ed Hote 5 Carrier 0 025 M NaOH Reagent 5 Manifold Tubing 0 8 mm 0 032 in i d This is 5 2 uL cm AE Sample Loop 150 em x 0 5 mm 0 022 in i d QC8000 Sample Loop 150 cm x 0 5 mm 0 022 in i d Interference Filter 660 nm Apparatus An injection valve a 10 mm path length flow cell and a colorimetric detector module is required The La shows tubing wrapped around the heater block at the specified temperature see manifold notes for the length of tubing used 8 168 cm of tubing on a 8 cm coil support Note PVC PUMP TUBES
306. onally the laboratory s standard operating procedures SOPs present the specific protocols to be followed as part of the analysis for the program Preventative maintenance steps employed by the laboratory are described in the laboratory OAM if available In general the preventative maintenance is performed on a scheduled basis on all instruments in the laboratory The preventive maintenance performed is documented in the instrument maintenance logbooks kept at the instrument Irregularities noted during operations are traced through the maintenance logbook to allow for efficient corrective action to solve problems Analysts are trained in preventive maintenance of their assigned instruments The laboratory utilizes in house service technicians in the event of instrument failures Contracts are maintained on the computer hardware and software Backup instrumentation is generally available if a specific analytical system becomes unavailable Section B 7 Instrument Equipment Calibration and Frequency Section B 7 1 Overview This section discusses calibration of laboratory instruments to be used for the Project All laboratory equipment used for analytical determinations is subject to periodic inspection and calibration Frequency of calibration is based on the type of equipment inherent stability manufacturer recommendations and intended use Section B 7 2 Laboratory Procedures The calibration procedures followed by the laboratory are outlined
307. ontainer is opened and the assigned expiration date of the chemical or standard The procedures are documented in the individual laboratory s QAM if available Section B 9 Data Management Internally each agency will store all data in their own specific StarLIMS database Laboratory Information Management system Data will be transferred from the laboratories to the MPCA Data will be stored in a Microsoft Access database at MPCA for data processing and analysis Section B 9 1 Data Recording Data and information collected in the lab will be recorded in dedicated notebooks and forms Data recording procedures to be followed by the laboratory are discussed in individual laboratory s QAM if available Section B 9 2 Data transformation Data and laboratory information is transformed in the MPCA offices Procedures for data transformation by the laboratory are discussed in the laboratory QAM if available Data are input into various computer Projects for storage The Projects utilized include Microsoft Access Excel and Word Section B 9 3 Data Transmittal Data and laboratory information are delivered to the MPCA using raw data notebooks and forms Analytical data are submitted to the MPCA as final analytical reports These reports have been reviewed and approved by the laboratory s technical QA QC and project management staff Data are then entered into a database by MPCA staff A report of Project activities is prepared by the MPC
308. optimized using graphical events programming Sample throughput 45 samples h 80 s sample Pump Speed 35 Cycle Period 80 Analyte Data Concentration Units ug P L Chemistry Direct Bipolar Expected Inject to Peak Start 21 58 Expected Peak Base Width 95s Calibration Data lea 313 2 as 4 s se 7 Concentration ug P L 500 250 100 so 25 10 0 Calibration Fit Type 1 Order Polynomial Weighting Method o 1 x Force through zero No l Sampler Timing Min Probe in Wash Period 5s Sample Period 30 s Valve Timing Load Period 25s Inject Period 55 s 10 1 15 01 3 E Post MUR Page 24 3 December 2010 sat Ortho Phosphate manifold Probe Wash orange Molybdate CR Ascorbic Acid Carrier 5 Note 10 mb waste Sample Carrier DI water Manifold Tubing 0 5mm 0 022 in i d This is 2 5 pL em QC8000 8500 Sample Loop 200 cm 0 032 i d Interference Filter 880 nm Apparatus A sample prep module with heater and UV lamp an injection valve a 10 mm path length flow cell a heater TO and a colorimetric detector module are required 4 5 70 cm of tubing on a 4 5 cm coil support 7 135 cm of tubing on a 7 cm coil support 12 255 cm of tubing on a 12 cm alternating coil support Note 8 The LSB shows 175 cm of 0 8 mm i d on the heater is used at the temperature shown Note 9 200 cm back pressure loop is 0 5 mm 0 022 in i d tubing
309. or at least 90 days after the report issue date or a date specified by the client during the project set up For custody samples the Operations Unit will notify the client prior to disposal The laboratory staff scans the sample barcode to record which sample containers the staff included in the disposal batch The LIMS records the disposal and the date of the disposal for each scanned container All aqueous samples that are non hazardous are neutralized if needed and enter the laboratory s general waste stream The building contains a neutralization flow through system in the basement area to filter and neutralize laboratory waste prior to entering the City of St Paul sewer The neutralization tanks are monitored at least annually for volatile and semivolatile organics radiation metals including mercury and pH The laboratory Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 31 of 67 http fyi health state mn us phl environmental index html monitors the tank contents to determine point source pollution and to take corrective action to avoid disposing of waste above regulatory limits All soil sludge samples that are non hazardous are discarded as trash Any hazardous samples are disposed according to the guidelines in the PHLD Chemical Hygiene Plan and the PHLD Hazardous Waste Manual Both of these
310. or the CCB must be less than the report limit of 0 01 mg L The results for the calibration verification standard CCV must be within 10 of the true value 0 5 mg L If analytical results do not meet the above criteria the analysis is terminated the instrument is checked and then re calibrated All samples following the last passing blank and standard are reanalyzed Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 19 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc 11 0 PROCEDURE 11 1 System Start up 11 1 1 Set up manifold as shown in Section 17 2 and inspect manifold for proper connections 11 1 2 Turn on power strip Allow at least 15 minutes for the heating unit to warm up to 65 C Do not pump reagents or water into the flow system until the temperature has reached 65 C 11 1 3 Raise tension levers on pump tube cassettes Place reagent lines into reagent water and check for leaks and smooth flow Allow about 20 minutes for heater to reach equilibrium 11 1 4 Transfer lines to designated reagent Allow system to equilibrate unti a stable baseline is achieved 11 2 Prepare a BS and MS for each batch by adding 100 uL of Intermediate Stock Standard 10 mg L into a 10 mL borosilicate test tube Add 5 0 mL of 0 0 mg L blank solution or
311. ork lists for analyses as needed The printed sample numbers from the labels are used to identify their sub samples A variety of queries to track progress and to generate workload summaries are used by the analysts supervisors and management team H Subcontracting of Analytical Services When the laboratory is requested to analyze samples for tests it is not able to perform either because the technology is not available or the capacity is not sufficient the samples may be subcontracted to another laboratory Subcontracting processes depend on the dollar amount of the work to be performed If the project is gt 25 000 and is performed over an extended period of time then the laboratory must issue a formal Request for Proposals through the Minnesota Department of Administration and receive bids from other laboratories interested in performing the work Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 30 of 67 http fyi health state mn us phl environmental index html For projects lt 25 000 the laboratory may choose from a qualified list of laboratories capable of performing the tests For Safe Drinking Water Act compliance a laboratory is chosen based on its certification status and approval through the state For tests not certified by the state the laboratory may choose a subcontractor t
312. other copy of the data sheet to the copy of the C of C form for clerical 13 If they submitted a multi copy data sheet e Separate the copies and make a photocopy if necessary to equal three copies e Then follow step 12 14 Deliver the samples to the locked cooler in room L250 The key for this cooler is kept in the top left drawer by the numbering machine 15 Place the original form s into the binder 16 Carefully enter the samples into the Custody Logbook in room L250 Refer to previous entries if necessary for examples Be sure to sign off custody when completed 17 Let the appropriate laboratory units know that they received Chain of Custody samples When Analysts are ready to perform the requested tests they must sign the samples out through the Custody Logbook 18 Print a daily entry log for the samples verify all information was entered correctly and deliver appropriate copies to clerical 19 Deliver copies to the submitting agency For the MPCA samples place the sheets in the box on the counter for their courier to pick up Minnesota Department of Health l Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 21 of 57 PRIORITY LEVELS Priority levels determine the length of time the laboratory has to analyze samples from the time of receipt until results are available on the computer Assigning the more urgent priority l
313. ottom of the handheld screen stating Calibration successful if this message does not display or if the message reads Calibration Failed recheck the calibration fluid make sure the standard was properly entered or obtain fresh calibration fluid e Dissolved Oxygen Calibration Rinse the probes and plastic tubing with DI water Fill the plastic case 1 3 full with DI water replace the black plug loosely screw the calibration tube into place on the end of the sonde and turn the sonde upright case down o The probes need not and should not be submerged during oxygen calibration Wait 5 min or until condensation begins to appear on the probes and tubing Navigate to the LDO on the sonde calibration menu and press Select Enter the current barometric pressure typically near 760 mmHg and press Done Calibration successful should appear across the bottom of the screen on the handheld if not recheck the current barometric pressure and attempt to recalibrate if the problem persists contact Dr Nathan Johnson for assistance NOTE A simple method of submerging the probes of the sonde is to simply pour the calibration fluid into the clear plastic tubing and hold the sonde upside down so the corded end of the sonde is facing the ground By using this method approximately 50 mL of fluid is required to submerge the probes excluding turbidity and perform the calibration University of Minnesota Duluth Civil Engineeri
314. ou may need to use a retractable blade Exacto knife to cut through the sealing tape It is advisable to wear safety glasses while using a knife Make sure that data sheets were included with the samples Collectors usually put data sheets in plastic bags to protect them from moisture and they sometimes tape the bag to the lid of the cooler Ifthere are no data sheets a very rare occurrence refer to the return address to help you track down the collector At the very least you would then be able to contact the MPCA office that the samples were shipped from RECEIVING SAMPLES AND DAIA SHEETS VIA IN PERSON DELIVERY When the MPCA courier Ed KORIE delivers samples he will arrange them in order on the counter He never delivers samples without data sheets When other MPCA collectors bring in their samples ask them to arrange them in order on the counter Make sure they filled out their data sheets completely and correctly Do not allow Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 47 of 57 them to leave until the data sheet is complete and you have had a chance to compare the sample containers to the data sheets In other words go through steps 4 5 6 7 amp 8 before the collector leaves CHECKING THE TEMPERATURE OF SAMPLES UPON ARRIVAL We normally check the sample temperature by using a temp
315. ount of analyte is spiked into a blank matrix similar to the initial sample This spike is then taken through all extraction dilution etc steps and analyzed like a sample MS MSD Matrix Spike duplicate min once per matrix o Asample which was analyzed alone should be split and prepared in exactly the same way A known amount of analyte is then spiked into the duplicate sample The original replicate will have a known amount of the analyte and can be subtracted from the spiked replicate to ensure recovery and or linearity of instrument response o Many times a sample is split into three replicates and two are spiked to check precision reproducibility and recovery at the same time Detection limit once for the method o Established by analyzing many samples 2 7 at a concentration expected to be near the detection limit the standard deviation of these analyses is used to establish a method detection that is known to be above zero with confidence according to a standard procedure Typical analytical sequence As a result of the need for these quality assurance checks a typical analytical sequence for 30 samples in a new matrix might involve the following An analytical blank Two to five non zero calibration standards spanning the range of expected sample concentrations Ongoing Precision Recovery sample Quality Control or reference sample An analytical blank Seven samples A method blank Ongoing precision R
316. overwrite the report file that you have defined before and you will lose the previous results if you select overwrite the result under file write option 4 If you select the Append under the file write option you will have new results append at the end of previous defined file resulting a long files but maybe useful if you split a batch of sample into several parts and run in different times 5 Under report format select all options of use titles use delimiter and use separator they are important for viewing the result later in Excel 6 Defining sample file a Asample file has to be defined before a sample or a batch of samples can be analyzed b Switch to Sample Tab by clicking Sample on main menu vi vii Select batch tab unless you are to measure only one or two samples or bear to switch the sampling tip every 4 minutes for a batch of samples Under Batch put all of your standard solutions samples spike samples replicates in auto sampler Clearly label and define the sample IDs and record the location A S Loc this information will be detailed in the following auto sampler section for each sample fill this information in the sampling table or you can use sample template to build the sample file In column of measuring action select run sample for all samples listed under A S Loc including blanks standard solutions spikes and replicates for the ana
317. ox will appear next to the AN code column e Double click on the box and enter the list of analysis sodes that are to be rejected separated by commas e This will bring up the rejection email screen which is the sample screen used for samples that are past the hold time To the lower left of the sample section is the Rejection Reason field Several common sample problems are available as pull down menus or other information can be typed in e Continue with entry as described in the Initial Entry Procedure section Minnesota Department of Health i Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 17 of 57 NUMBERING ERROR CORRECTION PROCEDURES Numbers on a data sheet must be in sequential order so if a number is stamped by mistake or missed we try to shift the numbers around to keep everything in order e Iftoo many numbers were stamped on a data sheet try to move the extra number s to another sheet Check to see if there are any unnumbered data sheets thatthe extra number s can be moved too For example if two extra numbers were stamped off and you find an unnumbered data sheet with exactly two samples listed on it write the extra numbers on this data sheet e If not enough sample numbers were stamped on a data sheet it may be possible to add sequential numbers from the next data sheet For example if two more numbers are needed
318. pare weekly 72 PREPARATION OF DIGESTION REAGENTS l Reagent 6 Digestion Reagent 1 By Volume To a 1 L volumetric flask add 500 mL DI water and then add 106 5 mL sulfuric acid H2504 CAUTION this solution will become very hot Dilute to the mark and stir to mix Allow to cool to room temperature prior to use Prepare weekly By Weight To a tared 1 L container add 893 5 g DI water and then add 196 0 g sulfuric acid H5SO4 CAUTION this solution will become very hot Stir to mix Allow to come to room temperature before use Prepare weekly Reagent 7 Digestion Reagent 2 By Volume To a 1 L volumetric flask add 800 ml DI water and then add 26 g potassium persulfate K2S20s Mix with a magnetic stirrer until dissolved Dilute to the mark Prepare weekly Degas before using i By Weight To a tared 1 L container add 990 g DI water and then add 26 g potassium persulfate K2S208 Mix with a magnetic stirrer until dissolved Prepare weekly Degas before using Potassium persulfate from EM Science catalog number PX1560 1 has been shown to give good results with this method 10 115 01 3 E Post MUR l Page 5 3 December 2010 sat 73 PREPARATION OF STANDARDS NOTE Standards are prepared in a matrix of 1 5 mL L sulfuric acid This is assumed to match the sulfuric acid added to the samples for preservation If samples are not preserved the matrix for the standards is DI water If a different amount of acid is used for preser
319. pared the elemental peak to a known standard material after calibration and generated a report for each element on a weight basis Each sample chromatogram was visually inspected Manual integration was performed as necessary to use only the area of the element of interest in calculations Results were manually transferred to the spreadsheet provided by Amy Myrbo and reported via email STANDARD OPERATING PROCEDURE TOTAL SULFUR TS Purpose and Analysis Overview after S Grosshuesch The analysis of total sulfur is accomplished by combustion using two furnaces aligned in sequence A sample is weighed into a ceramic combustion boat and covered with V20s The boat is pushed inside the first furnace where sample ignition occurs at 1050 C In the presence of Oz sulfur is converted to SO2 and SO These gas products are carried through to the second furnace set at 825 C where they react with a mixture of granular copper oxide and reduced copper filings to ensure that all sulfur is converted to SOz The SOzis purged into the sulfur coulometer cell where it is absorbed and titrated The coulometer titration cell contains an anode and cathode compartment The anode compartment contains platinum detector and generating electrodes The cathode compartment contains a single platinum cathode The anode compartment is filled with a solution containing methanol pyridine water and tetrabutylammonium iodide the cathode cell compartment contains a
320. pb phId env inorganics Gen Chem SOPs gen26 doc analyzing a calibration standard at or below the report level 0 01 mg L The CRL check sample is not required to be processed through the entire SOP The percent recovery of the CRL must be within 40 9 2 4 1 If the percent recovery of the CRL is outside the acceptance criteria the analyst must either 1 repeat the CRL or 2 recalibrate and then perform the CRL If the repeat CRL is within acceptance criteria or if the instrument recalibration results in a CRL that is within acceptance criteria the analyst may proceed with the analytical run If the CRL is not within acceptance criteria the analyst must either 1 recalibrate the instrument and then perform the CRL once again or 2 perform the CRL at a higher concentration level 9 2 4 2 If an acceptable percent recovery can only be achieved at a higher concentration level the analyst must elevate the Report Level for the associated samples to the concentration of the lowest point that meets the acceptance criteria The analyst must report all samples analyzed after the failed CRL using the elevated Report Level until a new calibration curve and CRL meet the acceptance criteria 9 2 5 Continuing Verification of Calibration Analyze a continuing calibration verification standard CCV after every 10th sample and at the end of the sample run Each analyte must fall within 10 of its expected value If an analyte is outside the interv
321. pendix 8 pp 51 52 The worksheet for determining the Method Detection Limit MDL for analyses involving single analytes is provided in Appendix 9 p 53 Instructions for completing this worksheet are provided in Appendix 9 pp 54 56 C Initial Demonstration of Capability The policy and procedure for conducting an Initial Demonstration of Capability Study are described in Appendix 10 pp 57 58 D Report Level Verification The policy and procedure for conducting a Report Level Verification are described in Appendix 11 pp 59 60 E Other QC Checks The analytical Standard Operating Procedures SOPs for each field of testing list the quality control procedures that are required for laboratory staff At a minimum the SOPs include the following For chemistry and radiochemistry the quality control included or referenced instrument performance check standards frequency and acceptability of method detection limit MDL calculations frequency and acceptability of demonstration of low level capability calibration internal and surrogate standards laboratory reagent blank field reagent blank and trip blank field and laboratory matrix replicates quality control and proficiency testing samples laboratory control sample and matrix spike replicates initial demonstration of method capability use of control charts qualitative identification confirmation of contaminants VVVVVVVVVVV For microbiology the quality control incl
322. phosphoric acid solution Inert carrier gas Nz containing sample sulfur as SO2 or H2S is delivered to the anode cell compartment Free iodine is electrochemically produced in the anode cell and reacts with the sulfur gas as illustrated in the following reactions Anode reactions S02 l2 2H20 e H2S04 21 2H H2S I2 6 2H 21 SO 2I o I2 2e Cathode reaction 2H20 2e o H2 20H The decrease in free iodine proportionally decreases the sulfur detector current automatically activating the titration current and generating I2 stoichiometrically Hydrogen gas is produced in the cathode cell at a rate equivalent to that of iodine generation After the majority of the analyte is titrated an increase in the detector current and free Iz occurs ultimately stopping the titration when the initial iodine concentration is reached The titration current is continuously monitored integrated and used to calculate the quantity of sulfur delivered to the anode cell The significant advantage associated with the coulometric titration of sulfur is that the current is the titrant and as a result there is no need for generating and applying standard calibration curves Most sample analyses for total sulfur can be completed within 10 min Longer analysis times result if the sample contains more than about 3000 ug of sulfur or if sulfur bearing compounds in the sample resist oxidation Analysis times for AVS and CRS measurements are highly dependent on the sa
323. pied and the fourth level houses the air handling systems Approximately 60 of the building s space is utilized by the PHLD The building ventilation system includes a state of the art heat recovery wheel to save on long term energy costs and air filtration The building has 10096 outside air running through the labs with no recirculation In addition the air in the metals clean room area is HEPA filtered The metals clean room the routine metals area and the radiation chemistry area are equipped with polypropylene hoods to protect the integrity of the hood surfaces and reduce risk of contamination from corrosion Ventilation hoods have digital sensors monitoring for image detection as well as movement to automatically adjust for appropriate airflow The automated system reduces the amount of heat loss through the hoods while protecting the health and safety of the workers C Building Security The MDA MDH Laboratory building is a locked secure area and it is not open to the public Visitors must register at the Orville Freeman Office Building reception desk and receive one of three types of security badges 1 Lab Visitor badges provide access to the front door and the atrium s turnstiles during regular business hours These visitors then have access to the elevators and conference rooms on the 2nd and 3rd floors 2 Lab Staff badges provide access to the general lab spaces throughout our building and general spaces in the Freeman Bui
324. point only 10 115 01 3 E Post MUR Page 15 3 December 2010 sat 17 2 SUPPORT DATA FOR QUIKCHEM 8000 8500 Calibration Data for Total Phosphorus Time 1840 94 Seconds Amp 134151 Volts A M A AAA i v v e H o I t t s i H i 1 04 as T T T T T T H E A E T 7 7 a 7 7 j 4 lt lt Ki X 4 1 u o o 3 E i Ss S M p y 4 e E T id a o 9 n 10 M KS KS lt lt 4 y y p i o IN N o d IM 3 ri md ie S he 2 o ip D T o a r N c o M lt 4 o 0 3 o N M a r D N a ak 0 9 Q D T o Q 9 N o 3 a N T 0 N N p o 0 a o s T 0 m o a r r 0 T c e o is o s o o o a o o o o m m ye T M LU le o 0 0 o o o o 9 0 o o 3 T he D ha N N Li T D D a N E T o Ok i i i D i i 500 1000 3 Data Filename 042502E f t dii Acq Date 25 April 2002 Calibration Graph and Statistics Leve i RSD jue 1 mese 1i mma s 3 ET 1 393 Bl oq Rp Scaling None Weighting 144 1st Order Poly Conc 8 241e 005 rea 3 682e 000 r 1 0000 X 2 10 115 01 3 E Post MUR Page 16 3 December 2010 sat Time 5515 63 Seconds Amp 194457 Volta vu v Y i 133 i 1 9 152 d d d d d d 3 J Fi d J Fi d q z 2 d J 3 d 3 3 i 0 I o m g E of a C o o o iu o o o 3 o D 5 o 3 o 3 a D o o o Dp 3 3 5 3 3 5 5 m 5 5 M 5 3 a 3 5 5 5 5 3 4 a B 8 g UP i 8 3 8 5 8 f
325. port A12 The inlet of the A12 is connected to outlet of tee 2 and the outlet is connected to a union i then to UV lamp Cooling fins are used to keep the coil from becoming too hot This coil is wrapped with 150 cm of 0 032 i d 0 8mm tubing This coil can be placed on top of the in line module if this is convenient The outlet of the tubular membrane debubbler is connected to port 6 of the valve using a 39 cm length of 0 5 mm 0 022 in i d Teflon tubing l l The Debubbler is mounted on the manifold board near the valve Replacement membranes are part number 85363 To install unit Cut tubing with 2 nuts in half Screw half into each port on the PEEK body These are the inlet and outlet of the unit If needed 50 or 100 cm of 0 022 i d tubing can be added at the outlet of the debubbler connected to Port 6 of the valve The TA Va shows 175 em of 0 8 mm i d on the heater is used at the temperature shown 200 cm back pressure loop is 0 5 mm 0 022 in i d tubing The 100 cm back pressure loop is 0 5 mm 0 022 in i d tubing 10 115 01 3 E Post MUR Page 22 3 December 2010 sat 174 DEBUBBLER MEM S S A and outlet i i 1 Membrane M This debubbler h s holes in the bottom anda circular membrane sandwiched between two round pieces of tan PEEK Typically it does not require a backpressure loop on the outlet When a liquid other than water is passed through this debubbling unit it is ve
326. preserved with sulfuric acid maximum of 2 mL concentrated H SO per liter and refrigerated CAUTION Samples must not be preserved with mercuric chloride or thiosulfate because this will degrade the cadmium column Samples should be collected in plastic or glass bottles All bottles must be thoroughly cleaned and rinsed with reagent water The volume collected should be sufficient to insure a representative sample allow for replicate analysis if required and minimize waste disposal 9 QUALITY CONTROL 9d Each laboratory using this method is required to operate a formal quality control QC program The minimum requirements of this program consist of an initial demonstration of laboratory capability and the periodic analysis of laboratory reagent blanks fortified blanks and other laboratory solutions as a continuing check on performance The laboratory is required to maintain performance records that define the quality of the data that are generated 9 1 1 Analyses of matrix spike and matrix spike duplicate samples are required to demonstrate method accuracy and precision and to monitor matrix interferences interferences caused by the sample matrix The procedure and QC criteria for spiking are described in section 9 3 9 1 2 Analyses of laboratory blanks are required to demonstrate freedom from contamination 10 107 04 3 D Page 8 2 Dec 2010 sat 9 2 9 3 9 1 3 The laboratory shall on an ongoing basis
327. projects the client s project manager has pre approved the laboratory to take specific actions These exemptions from the notification process are programmed in the LIMS as business rules When samples are received and do not meet the laboratory s Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 26 of 67 http fyi health state mn us phl environmental index html acceptance criteria the LIMS determines whether a business rule applies If a business rule applies the LIMS will allow the sample receipt custodian to accept or reject the samples and generate an electronic message with no need for a response Approval for these conditions has already been given by the client In those instances the LIMS will qualify the data on the final report without further interaction from the operations unit or laboratory staff If the custodian determines that samples do not meet receipt requirements sample receiving personnel enter into the LIMS the condition of the samples or sample containers and the reason for rejection The most common errors in submission or reasons for rejection of samples are available as drop down options in the LIMS nonetheless the sample receiving staff has the option to enter free text for particular conditions not otherwise identified When problems are identified by the sample
328. r and Program PWSN Collected Date etc 3 Sample refers to the MDH number we assigned atlogin Enter the number at the prompt and press the enter key to retrieve additional information If the sample is known this is the quickest way to pull up the record Once a sample record is retrieved you can check other samples in the sequence by clicking the Prev Samp and or Next Samp buttons at the top of the screen 4 PWS His the Public Water Supply assigned by Environmental Health Enter the at the prompt and press the enter key to retrieve dditional information 5 To use the Collection Date and Collector option you must know the collector s ID This is a four digit number that is assigned to each EH collector Enter the ID and press enter tab to retrieve all sample records from that collector A collection date can also be entered to narrow the search 6 The final option Program PWSN Collected Date etc allows you to search for samples using multiple criteria This is the screen we use when searching for specific samples with little information to go on Enter what information you have and leave the other fields blank Click _ on Fetch Data or hit enter tab from the last field to retrieve samples This method can be useful when searching for samples for which we know the program and or analysis codes PWS Table Review This option is allows you to find a PWS number using the name or return address information It a
329. r within two weeks The completed Corrective Action Form and copies of all documentation of corrective actions are maintained by the Quality Assurance Officer Upon completion a copy of the Corrective Action Form is forwarded to the Environmental Laboratory Section Manager for review The Quality Assurance Officer reviews the proposed plan and verifies the corrective action progress and effectiveness Problems arising during or after analysis of samples may also require corrective actions however the investigation of such problems is carried out by the analyst generating the data or by the designated reviewer or Unit Supervisor reviewing the data Corrective actions are described in standard operating procedures for the test methods used in the laboratory If an analyst determines that corrective actions have not resolved the problem or that a data set is compromised the analyst must notify their Supervisor immediately The Unit Supervisor must assess the data and determine if and how the data may be qualified This process may require contact with the client and written instructions on how to proceed The Unit Supervisor may conclude that the effectiveness of the corrective actions should be investigated further and requests a corrective action form from the Quality Assurance Officer l Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effe
330. ration curve Verify calibration using a midrange calibration standard every ten samples or every analytical batch Compute the percent recovery using the following equation l D recovery x100 K Where D Determined concentration of analyte in the calibration standard K Actual concentration of the analyte in the calibration standard If recovery exceeds 10 the analytical system is judged to be out of control and the problem must be immediately identified and corrected and the analytical batch reanalyzed 10 107 04 3 D Page 11 2 Dec 2010 sat 11 PROCEDURE 11 1 SAMPLE PRETREATMENT PROCEDURE 11 1 1 Samples may be determined without preservation or preserved with sulfuric acid as directed above 11 1 2 Both standards and samples should be carried through this procedure If samples 11 1 3 have been preserved with sulfuric acid standards should be preserved in the same manner Samples may be homogenized i in a device designed for this purpose However turbid samples should be filtered since the digestion effectiveness on nitrogen containing particles is unknown 11 2 CALIBRATION PROCEDURE 11 2 1 11 2 2 11 2 3 11 2 4 11 2 5 11 2 6 Prepare reagent and standards as described in Section 7 Set up manifold as shown in Section 17 Input data system parameters as shown in Section 17 Pump DI water through all reagent lines and check for leaks and smooth flow Switch to reagents a
331. ratory at the time of the analysis The PT samples are managed analyzed and reported in the same manner as routine samples Additional measures to demonstrate proficiency may be required for individual projects The scope and requirements of the proficiency program are generally presented to the laboratory in specific quality assurance project plans QAPPs Proficiency testing results are reviewed by the Laboratory Quality Assurance Officer and the reports are distributed to the Laboratory Supervisors The unit supervisors are responsible for distributing the individual results to each staff member who participated in the PT studies Acceptable performance on PT samples is required to establish and demonstrate ongoing capability for the various analytical systems methods and matrices In the event of Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 38 of 67 http fyi health state mn us phl environmental index html unacceptable proficiency testing results the federal or state regulatory agency is notified within 30 days of corrective action including documentation stating the purchase of a remedial PT sample Additionally the laboratory authorizes the approved PT vendor to electronically supply results directly to the regulatory agency B Internal Audits The Quality Assurance Officer
332. rea For custody samples the samples and submission forms are hand delivered or sent in a sealed shipment container and are received at the laboratory by a designated sample receipt custodian If a tag was used to seal the shipment container the custodian examines the seal tag to check for tampering The custodian breaks the intact seal and opens the container to verify that the tag number written on the custody form matches the number on the container seal If the samples are being hand delivered by someone other than the person who signed for custody of the samples on the chain of custody form or the tag on the sealed shipment Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 27 of 67 http fyi health state mn us phl environmental index html container is not intact the sample receipt custodian does not accept the samples The sample receipt custodian records the information in the comments section on the chain of custody form and notifies the Quality Assurance Officer or a unit supervisor The sample receipt custodian notifies the client of the discrepancies and obtains further instructions The custodian examines the samples to determine that they meet laboratory requirements that no damage to the sample bottles has occurred and that the sample seal tape if used on the bottles is still intac
333. receiving staff and entered into the LIMS the sample receiving personnel initiate requests for resolution of discrepancies according to a procedure similar to those for messages sent for holding time issues as explained above Civil or Criminal Chain of Custody Procedures Due to the evidentiary nature of samples collected during enforcement investigations sample possession must be traceable from the time samples are collected until they are disposed and until their derived data are used for enforcement purposes or are introduced as evidence in legal proceedings The laboratory uses civil or criminal chain of custody procedures to maintain a record that tracks each sample and each individual responsible for sample collection receipt analysis and disposal An example of a chain of custody form associated with receipt of samples involved in enforcement actions is provided in Appendix 5 p 47 The laboratory maintains a bound civil or criminal chain of custody logbook to internally track samples that are associated with enforcement activities A page from the civil or criminal chain of custody logbook is contained in Appendix 6 p 48 The laboratory s civil or criminal chain of custody procedure is described below The laboratory considers a sample in custody if the sample is in a person s actual possession in view after being in a person s physical possession or in a person s possession and that person placed the sample in a secured a
334. recision One pair should be extracted and analyzed per ten samples or less The RPD should be less than or equal to the values listed in Tables 4 5 and 6 Section B 5 1 5 Out of Control Situations When the out of control situations listed in Sections B 5 1 3 through B 5 1 5 occur the failing analysis should be repeated If the re analysis meets QC criteria report the second analysis If the re analysis still does not meet criteria the affected samples should be re prepared and re analyzed If the results of the re analysis of the MS still fail to meet criteria and the result of the LCS is acceptable then the problem is related to matrix and the QC batch requirements are considered to have been met Report the results of the batch and qualify the result of the environmental sample chosen for QC purposes as estimated If the results for the LCS fail again instrument maintenance is required After the maintenance has been completed another initial calibration must be performed Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 6 and B 7 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 32 of 44 Section B 6 Instrument Equipment Testing Inspection and Maintenance Section B 6 1 Laboratory Equipment The protocols for testing inspection and maintenance of laboratory equipment are addressed in the laboratory QAM s if available Additi
335. results will match the manual off line digestion If samples are not filtered in line results will be 1 15 low compared with off line digestion Surface water samples may not require filtration but this should be verified with a sample containing high levels of solids After digestion nitrate is quantitatively reduced to nitrite by passage of the sample through a copperized cadmium column The nitrite reduced nitrate plus original nitrite is then determined by diazotization with sulfanilamide under acidic conditions to form a diazonium ion The diazonium ion is coupled with N 1 naphthyl ethylenediamine dihydrochloride The resulting pink dye absorbs at 540 nm and is proportional to total nitrogen The method will recover nearly all forms of nitrogen Nitrate and nitrite are recovered in this method They are not recovered in the conventional Kjeldahl nitrogen method Thus the resultant concentration for this method is termed total nitrogen and not Kjeldahl nitrogen The applicable range is 0 05 to 5 0 mg N L for the low range and 0 2 to 20 0 mg N L for the high range The method detection limit is 0 003 mg N L for the low range and 0 008 mg N L for the high range The method throughput is 45 injections per hour SUMMARY OF METHOD 2 1 Nitrogen compounds are oxidized in line to nitrate using alkaline persulfate UV digestion Oxidation of nitrogen containing compounds to nitrate is achieved at 105 C with additional energy supplied by expo
336. rewater and overlying water analyses will take place in the UMD Civil Engineering Laboratory in the labs of Drs Johnson and Pastor Quality assurance guidelines and SOPs for the Johnson lab are included in Appendix C The analytes of concern from an aqueous and sedimentary medium with Report levels and analytical methodologies are detailed in tables 1 2 and 3 above Due to the constraints presented by low sample volume the MDH Inorganic Environmental laboratory will not be the lab of primary analysis although cross checks of results between the U of M Duluth Civil Engineering lab and MDH Inorganic Environmental lab are done frequently as a quality control activity Section A 7 2 Blanks The laboratory uses method blanks to verify the extraction procedures glassware and instrument conditions have background below the laboratory reporting limits The method blanks are reported with MPCA samples to allow the project manager to determine that laboratory contamination or analytical error could cause a false positive The laboratory performs method blanks at a rate of one for each analytical batch of twenty samples 5 or less to ensure a contaminant free environment Section A 7 3 Duplicate Samples The laboratory also prepares and analyzes duplicate samples to gain a measure of reproducibility MPCA has a relative percent difference RPD goal for duplicates of 25 in waters and 50 in sediments Wild Rice Sulfate Standard Sediment Incubatio
337. rganic chemical analyses and radiological analyses it is not applicable to microbiological analyses An Initial Demonstration of Capability IDC Study must be performed for each new method for each new environmental matrix for each new analyte for each new instrument and for each new analyst For new analysts an IDC must as a minimum include steps 1 4 below All other situations would require that items 41 6 be performed An IDC may also be required whenever there is a significant change in the SOP matrix or instrument that could affect the precision accuracy or sensitivity of the analysis The Quality Assurance Officer QAO in consultation with the analyst and Unit supervisor would make this determination The Quality Assurance Officer may waive or modify the IDC requirement when it is not feasible to conduct an Initial Demonstration of Capability Study Requirements The analyst must follow requirements for the performance of an Initial Demonstration of Capability Study cited in the reference method or applicable regulatory program for which the data are to be used A project or client may also specify additional IDC requirements If no such requirements exist the analyst shall utilize the IDC procedure described below For analyses that are part of the UCMR2 Unregulated Contaminant Monitoring Regulation the analyst must follow the procedure outlined in Section 6 of UCMR2 Laboratory Approval Manual version 2 0 October 2006 The elem
338. row keys until pH Units is highlighted and press the Select Button Enter the target pH of the calibration fluid by navigating with the left and right arrow keys to highlight different numbers Press Select to enter that number within the new standard Once the new standard value is entered press Done and wait for several seconds A message should come across the bottom of the handheld screen stating Calibration successful if this message does not display or if the message reads Calibration Failed recheck the calibration fluid make sure the standard was properly entered or obtain fresh calibration fluid Repeat this process for calibration fluid at pH 4 7 and 10 d Conductivity Calibration Thoroughly rinse the probes and plastic tubing with DI water Make a Calibration solution using the solution within the sonde case 2000 uS cm o e g Typical values of conductivity for the WD Wild rice Sulfate Project 2013 fall between 300 and 500 uS cm so a 400uS cm calibration is appropriate To make this 5 0mL is required mix 10 mL of the 2000u S cm solution from the case and combine it with 40 mL of DI water Navigate to the SpCond uS cm item on the calibration menu Using the left and right keys enter the concentration of the calibration fluid that you made Submerge the Sonde probes in the calibration fluid that you made and press Done on the handheld device A message should come across the b
339. rrer for at least four hours The solution can be stored in plastic for up to two months if refrigerated Reagent 2 Stock Antimony Potassium Tartrate Solution By Volume In a 1 L volumetric flask dissolve 3 22 g antimony potassium tartrate potassium antimonyl tartrate trihydrate CgH4OiK58b 3H2O or dissolve 3 0 g antimony potassium tartrate potassium antimonyl tartrate hemihydrate K SbO C H 05 1 2H20 in approximately 800 mL DI water Dilute to the mark and mix with a magnetic stirrer until dissolved The solution can be stored in dark plastic for up to two months if refrigerated By Weight To a 1 L dark tared container add 3 22 g antimony potassium tartrate potassium antimony tartrate trihydrate CaH4O K Sb 3H20 or dissolve 3 0 g antimony potassium tartrate potassium antimonyl tartrate hemihydrate K SbO C4H4061 2H O0 and 995 g DI water Mix with a magnetic stirrer until dissolved The solution can be stored in dark plastic for up to two months if refrigerated Reagent 3 Molybdate Color Reagent By Volume To a 1 L volumetric flask add about 500 mL DI water and then add 25 mL Sulfuric Acid H2504 Stir or swirl to mix Then add 213 mL Ammonium Molybdate Solution Reagent 1 and 72 mL Antimony Potassium Tartrate Solution Reagent 2 Dilute to the mark and stir to mix Degas with helium Prepare weekly or if blue color or yellow precipitate develops By Weight To a tared 1 L container add 690g DI water and 47 8 g
340. rt Level Analytical Method Target Analyte RL Reference Laboratory Location of Methods Sediment Acid Volatile Sulfide AVS 0 01 mg kg SM4500 S2 J MDH Environmental Appendix C ICP MS for Extractable 03 ug L EPA 6020 A UMD Civil Engineering Appendix D Metals Total Sulfur TBD TBD LacCore LRC Appendix E Total Carbon TBD TBD LacCore LRC Appendix E Total Nitrogen TBD TBD LacCore LRC Appendix E Percent Solids 0 01 mg kg SM4500 S2 J MDH Environmental Appendix C Section A 6 4 Intended Data Usage Data will be interpreted based upon the data produced geochemical calculations and computer modeling From this data a simple reactive transport model will be created and calibrated to model the rate of sulfate diffusion and transformation in sediment as constrained by observed changes in the concentrations of sulfate and inert tracers in overlying water porewater sulfide AVS and other supporting analyses To the extent scientifically defensible the effects of oxygen release by roots on concentrations of sulfide in sediment may be modeled Section A 6 5 Technical Reports The Work Order Coordinator will provide updates to the MPCA Wild Rice Sulfate Standard Study staff summarizing the experiment progress and analytical data during weekly phone conversations or meetings The Work Order Coordinator will provide a technical report to the MPCA providing and interpreting all data as well as creating a reactive transfer model for
341. ry between instruments To use this table select an instrument then read across to find the corresponding information required to perform this test Table 393 Instrument specific information Instrument Sample volume Sample cell Cell orientation DR 6000 10 mL 2495402 Fill line faces right DR 5000 10 mL 2495402 Fill line faces user DR 3900 10 mL 2495402 Fill line faces user DR 3800 DR 2800 DR 2700 10 mL 2495402 Fill line faces right Before starting the test Analyze samples immediately Do not preserve for later analysis Avoid excessive agitation of samples to minimize sulfide loss Some sulfide loss may occur if dilution is necessary Sulfide 2 reagent contains potassium dichromate The final solution will contain hexavalent chromium D007 at a concentration that is regulated as a hazardous waste by Federal RCRA Refer to the current MSDS for safe handling and disposal instructions Collect the following items Description Quantity Sulfide 1 Reagent 1 2mL Sulfide 2 Reagent 1 2mL Water deionized 10 25 mL Pipet serological 10 mL 1 Pipet Filler safety bulb q Sample Cells see Instrument specific information 2 Stoppers 2 See Consumables and replacement items for reorder information Sulfide Page 1 of 4 Sulfide Methylene Blue Method Stored Programs 690 Sulfide Start 1 Select the test Insert an adapter if required see nstrument 2 Blank Preparation Measure 10 m
342. ry important that Di water be pumped through it for 5 10 minutes followed by pumping air for another 5 10 minutes at the end of each days run This aids in removing salts acids and bases that could reduce the lifetime of the membrane and at least partially dries the hydrophobic membrane material Membranes typically last 1 3 weeks or even longer with fastidious care If the solution passing through the unit is very hot it is not unusual to see water droplets on the outside l if bubbles are still entering in the fluid stream but not exiting at the outlet the unit is still property functioning despite this condensation Membranes are replaced by removal of the Allen screw in the center of the block The expired membrane is removed and a replacement centered If the replacement membrane has any text on it the membrane should be placed so that the text side faces the bottom of the unit The part numbers for this are as follows 85362 BUBBLE TRAP QC8000 8500 Not salable 85363 BUBBLE TRAP SPARE MEMBRANES PK5 85364 TUBING SET BUBBLE TRAP QC8000 QC8500 85361 KIT BUBBLE TRAP QC 009 QC8509 The Kit contains the PEEK Bubble trap 3 membranes and the tubing and nuts needed for connections 10 115 01 3 E Post MUR Page 23 3 3 December 2010 sat 17 5 MEASURING ORTHO PHOSPHATE UTILIZING TP MANIFOLD 17 5 1 DATA SYSTEM PARAMETERS FOR ORTHO PHOSPHATE The timing values listed below are approximate and will need to be
343. s Medical Conditions Aggravated by exposure Liver kidney or central nervous system disorders Compound Specific PPE Wear nitrile gloves safety goggles or face mask and lab coat when pouring anode solution in calibration cell While coulometer being used vent coulometer anode half cell to fume hood Storage Store in tightly closed container away from heat or flame Storage area should be well ventilated Store away from oxidizers strong acids and perchlorates Disposal Dispose of by means in compliance with all State Local and Federal Regulations Cathode Solution Phosphoric Acid Inhalation Corrosive causes irritation with coughing choking and burns of mucous membranes Symptoms include dizziness headache nausea weakness and pulmonary edema Repeated exposure can cause inflammation and ulcerative changes in the mouth and bronchial pneumonia Skin Absorption Corrosive causes pain or burns Repeated exposure may cause dermatitis Studies show that skin adsorption may occur Eye Contact Eye burns pain lacrimation photophobia from corrosiveness Injury ranges from irritation to conjunctivitis to blindness depending on the concentration and duration of exposure Ingestion Corrosive causes burns of mucous membranes of the mouth throat and esophagus Symptoms range from inflammation of respiratory distress to death depending on the concentration and duration of exposure Symptoms may be immediate or delay
344. s Standard 1 Stock Standard 1000 mg N L In a 1 L volumetric flask dissolve 7 221 g potassium nitrate KNO3 pre dried 60 C for 1 hour or 4 93 g sodium nitrite NaNOz2 in about 800 mL DI water Dilute to the mark with DI water and invert to mix When refrigerated the nitrate standard may be stored for up to three months Standards prepared as nitrate are more stable than those prepared as nitrite Standard 2 100 0 mg N L By Volume Inal L volumetric flask add 100 mL of Standard 1 1000 mg N L Dilute to the mark with DI water invert to mix Prepare fresh weekly 10 107 04 3 D Page 5 i 2 Dec 2010 sat Standard 3 10 0 mg N L By Volume In a 1 L volumetric flask add 10 mL of Standard 1 1000 mg N L Dilute to the mark with DI water invert to mix Prepare fresh weekly Low Range Standards Working Standards Prepare Daily Concentration mg N L By Volume Volume mL of standard 3 diluted to 250 mL with DI water By Weight Weight g of standard 3 A diluted to final weight 250 g divide by factor below with DI water Division Factor Divide exact weight of the standard by this factor to give final weight 10 107 04 3 D Page 6 2 Dec 2010 sat High Range Standards Working Standards Prepare Daily Concentration mg N L By Volume Volume mL of standard 2 diluted to 250 mL with DI water Volume mL of standard 3 diluted to 250 mL with DI water By Weight
345. s or other perishable samples into the fridge 2a 3 Place all metals samples on this counter Put samples in order left to right and front to back Line up Metals samples and Mercury samples separately Put any non water samples just to the right e 4 This is the preserved samples bench There are trays for three different sample bottles cyanide nutrient and nitrate All bactichem samples should be lined up in order left to right and back to front exceptas noted When a tray is full or the tray is missing more can be found in the cabinet just below the counter 5 There are two trays on this counter Nitrite samples go on the tray to the right fluoride samples go on the tray to the left The lab only runs fluorides every few weeks so the samples tend to accumulate When a tray is full put a new tray on top and continue to line up samples as before 6 This is the general unpreserved samples counter There are not specific trays since many different types of samples and bottles are placed here Try to keep similar samples grouped together as much as possible In addition to samples collected in general bottles any sample that is unpreserved should go on this counter BOD CBOD samples are placed on this counter with the printed labels paper clipped together and sitting on top of the bottles for the lab analysts The baskets for chlorophyll labels are located on this counter just to the right of where the samples are put 7 Put ch
346. s are expected to be in excess of 200uM a smaller sample volume is added and diluted to the expected sample volume with DI water The vial is then capped and gently mixed Absorbance is read at 510nM within 30 minutes and compared to absorbance of blanks and standards For low concentrations blanks and standards are prepared in deoxygenated but formerly oxidized matrix water UMD Civil Engineering Standard Operating Procedures Standard Operating Procedure for Hydrolab Sonde Calibration Johnson Research Group UMD Civil Engineering Updated 4 1 2013 Sonde calibration is to be conducted at the beginning of each use and the calibration status is to be checked whenever conditions change e g going from the warm storage into the cooled storage rooms a Charge sonde overnight The evening prior to use remove the handheld part of the sonde and plug into the RS232 charger which is located in the case The handheld unit needs to be turned on for charging to commence b Unplug the handheld from the charger and plug the sonde into the handheld using the same RS232 port on the back which the charger was plugged into c pH Calibration Rinse the probes with DI water Submerge the probes within the proper pH calibration fluid Press the Setup Cal button on the handheld then press Calibrate and press Sonde and wait for several seconds until the calibration menu appears Navigate the menu on the handheld using the up and down ar
347. s discussed by permitting personnel at the MPCA for a period of about two months Finally overlying water sulfate concentrations will be reduced back to ambient concentrations for a period of about two months during which time the temperature of the 4 C treatments may be increased to 21 C Flux of sulfate into and out of sediment will be quantified by carefully monitoring concentrations of sulfate and an inert tracer in the overlying water sulfate and by extracting sub cores from microcosms and or porewater with Rhizon filters at key time points when treatments are altered Geochemical calculations will be made to test assumptions about the chemical speciation of sulfur iron and other metals The project timeline schedule is from March 25 2013 to December 23 2013 Section A 6 3 Analytical Samples Samples that are to be sent to the MDH Environmental Inorganic Laboratory are brought under chain of custody procedures The samples are labeled to allow identification of each sample specific to the site where the sample was taken Samples are labeled and identified by the type of analyses being requested This information allows the laboratory to use the proper method when analyzing these samples and to produce identifiable records of results Specific instructions on sampling procedures including collection preservation and transportation are provided in Section B 1 The lists of target analytes are provided below in Tables 1 2 and 3 All analyti
348. s part of the Methods Update Final Rule published in the Federal Register on March 12 2007 Such modifications are acceptable for use in CWA monitoring Letters for modified methods that fall within the scope of Part 136 6 will no longer be issued and the use of these methods are acceptable provided that they meet the performance requirements specified in the method Minnesota Department of Health SOP Name Sulfide FIA water Environmental Laboratory File name gen026 Revision Date 07 02 2013 Revision 0 Effective Date Date of last signature Page 30 of 31 https inside mn gov sites MDH bureaus hpb phld env inorganics Gen Chem SOPs gen26 doc Secondly the flexibility allowed at Part 136 6 may be used to modify any method approved at Part 136 for compliance monitoring under the CWA including methods developed by VCSBs such as Standard Methods and ASTM International If you choose to modify an approved method in addition to documenting that the modification works to be fully transparent the user also discloses that a Modified Method X not just Method X is being used This annotation is especially important when modifying a method published by a standards organization such as Standard Methods ASTM International or AOAC International This is further clarified in the attached memo from Richard Reding Ph D Chief EASB to Regional ATP Coordinators and Alternates titled Citing Clean Water Act Limited Use ATP Methods as Modifications
349. s will be analyzed automatically You can also use schedule function by click schedule on main menu to define and schedule auto analysis wash and shutdown procedures So you can be sure the plasma will be shut down after the bath measurement is done However it is crucial for occasional check and to be sure the sequences are running appropriately when one or more batches of measurement are scheduled If a response to the system is asked for by the software during a run the system will stop the analyzing process until the respond has been received while the pumps and plasma are still running 7 Shutdown a At the end of sample runs place the end of the sample pump tubing in milli Q water and allow to run for 10 min Stop the plasma by clicking on the stop button in the plasma section of the instrument front panel window The instrument will go through an internal shutdown procedure and continue making noises for about a minute Stop the peristaltic pump Release the pump clamps and remove the pump tubing Open the cover of the auto sampler to allow the acid gas to release 8 Preparing standard solutions and samples a Standard solution i Never insert a pipette tip directly into the bottle containing original stock solution always use a second contained to hold a small amount of stock solution and work with it ii Standard calibration need to be made every day Typically when you restart the plasma and retune th
350. sample preparation The surrogate is added at a known concentration and is used to determine the efficiency of the sample preparation process Surrogates should possess chemical properties similar to those of the target analytes but should not be present in the original test sample Target Analyte The analyte in a given matrix that is determined by an analytical procedure Test Sample The prepared sample from which test portions are removed for analysis Trip Blank An aliquot of reagent water or other appropriate blank matrix taken from the laboratory to the sampling site and returned to the laboratory unopened A trip blank is used to Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 18 of 67 http fyi health state mn us phl environmental index html document contamination attributable to shipping and field handling procedures This type of blank is useful in documenting contamination of volatile organics samples Unregulated Contaminants Contaminants that require monitoring under the National Primary Drinking Water Regulations but have no MCL Weekly Applies to the weeks during which the analytical process including preparation of samples is performed SECTION 3 0 GENERAL LABORATORY INFORMATION AND POLICIES A Organization The Environmental Laboratory is located within the
351. se aspects of the analysts training 4 Ongoing Demonstration of Capability for laboratory analysts On an annual basis laboratory analysts must demonstrate their continued capability to perform the assigned procedures Acceptable demonstrations of capability may include any of the following successful analysis of a series of laboratory control samples with results statistically comparable to those of a trained analyst successful completion of a proficiency testing study or successful repetition of the initial demonstration of capability The laboratory staff must verify the demonstration of capability option selected meets method specific or client requirements Training of employees in the technical areas may require participation at conferences workshops and courses Subscriptions to scientific journals and participation in analytical laboratory organizations assist analysts in maintaining knowledge of the latest technology On site training conducted by manufacturers on the operation of their instruments is common Appendix 3 p 44 contains a copy of the Record of Personnel Education and Training which is completed by each analyst and filed in the Quality Assurance Office SECTION 6 0 INFORMATION TECHNOLOGY A Specifications for the Laboratory Information Management System LIMS The PHLD uses the Promium LIMS product Element which is a Client Server Application running against Oracle Database 10 2 0 4 Backup of data is ac
352. sign develop and implement the sediment incubation experiment maintaining project notebooks and recording data in an appropriate database Provide administrative direction to assigned staff as needed Critically examine all data generated for the project and annotate the data with any concerns Transfer all final data including annotations to the MPCA Project Manager Make preliminary interpretations of the data Prepare reports to the MPCA that summarize the experiments results preliminary interpretations and include an attachment of all final data in electronic database format At their discretion publish results from the project in a peer reviewed journal Section A 4 2 Graduate Researcher Will Derocher Review the Quality Assurance Project Plan QAPP including subsequent revisions With guidance from the MPCA Project Manager Work Order Coordinator and Principle Investigator design develop and implement the sediment incubation experiment maintaining project notebooks and recording data in an appropriate database Critically examine all data generated for the project and annotate the data with any concerns Make preliminary interpretations of the data Assist the Work Order Coordinator in preparing data and reports to the MPCA that summarize the experiments results preliminary interpretations and include an attachment of all final data in electronic database format In coordination with the Work Order Coordinator an
353. sign off authority on issues dealing with Project samples Section C 2 2 Laboratory Corrective Actions Laboratories have a corrective actions system that is described in the laboratory QAM if available Generally an individual involved in the analysis of the samples or review of the data discovers the problem The problem is identified and documented The documentation is important to allow tracking of the problem and ensure a proper solution is implemented All analysts OA staff and managers supervisors must agree to the solution to the problem The QA staff will go back and verify that the solution corrected the problem The documentation is archived with the client project folder Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No C 2 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 37 of 44 Section C 2 3 Laboratory Reports The laboratory sends a complete report to the MPCA that includes the following information a Anarrative discussing overall issues with the data e g calibration holding times internal QC etc Extraction date Sampling date Analysis date Alphabetical list of compounds Reporting limits Method of analysis and extraction Signature of a laboratory officer Chain of custody Results of spike Spike duplicates Results of surrogate samples Blanks and Concentrations found of each analyte 23 7m 7
354. sing the procedure described in Section 11 9 6 1 Compare the results with the current laboratory acceptance criteria If the criteria are not met the analytical system is judged to be out of control and the problem must be immediately identified and corrected and the analytical batch reanalyzed Quality Control Samples QCS It is suggested that the laboratory obtain and or prepare a quality control sample using a source different from the source routinely used in Section 7 The QCS is used to verify the concentrations of the calibration standards Depending on the specific program requirements field replicates and field spikes of the analytes of interest into samples may be required to assess the precision and accuracy of the sampling and sample transporting techniques 10 CALIBRATION AND STANDARDIZATION 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 Prepare reagents and standards as described in Section 7 Set up manifold as shown in Section 17 Input data system parameters as shown in Section 17 Pump DI water through all reagent lines and check for leaks and smooth flow Switch to reagents and allow the system to equilibrate until a stable baseline 1s achieved Place standards in the sampler Input the information required by the data system Calibrate the instrument by injecting the standards The data system will then associate the concentrations with the peak area for each standard to determine the calib
355. sitive value Detection Level Study DLS The broad term for any study that determines the detection level for a given analyte or analysis An MDL Study is one type of DLS Dissolved Analyte The analyte in an aqueous sample that will pass through a 0 45 um membrane filter prior to any sample preservation Duplicate See field duplicates or laboratory duplicates Equipment Blank A sample of analyte free media which has been poured over or through the sampling equipment It is collected after completion of decontamination and prior to sampling This blank is useful in documenting adequate decontamination of sampling equipment External Standard Calibration The process of creating a mathematical relationship by directly comparing the concentrations of target analytes to their instrument responses in calibration standards Samples are quantitated by using this mathematical relationship to calculate the concentrations of target analytes from the instrument responses to the same target analytes in samples Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 10 of 67 http fyi health state mn us phl environmental index html Field Blank An aliquot of reagent water or other appropriate blank matrix that is placed in a sample container in the field and treated as a sample in all respects includ
356. sks and pipettes or plastic containers as required Samples may be stored in plastic or glass Flow injection analysis equipment designed to deliver and react sample and reagents in the required order and ratios 6 3 1 Sampler 6 3 2 Multichannel proportioning pump 6 3 3 Reaction unit or manifold 6 3 4 Colorimetric detector 6 3 5 Data system Special Apparatus 6 4 1 In line TN TP sample prep module with 254 nm lamp 6 4 2 PVC PUMP TUBES MUST BE USED FOR THIS METHOD 6 4 3 Glass standard and sample vials must be used with this method 10 115 01 3 E Post MUR Page 3 3 December 2010 sat 7 REAGENTS AND STANDARDS 7 1 PREPARATION OF REAGENTS Use deionized water 10 megohm for all solutions Degassing with helium To prevent bubble formation degas all solutions except the standards with helium Use He at 140kPa 20 Ib in through a helium degassing tube Lachat Part No 50100 Bubble He through the solution for one minute Reagent 1 Stock Ammonium Molybdate Solution By Volume In a 1 L volumetric flask dissolve 40 0 g ammonium molybdate tetrahydrate NH Mo O 4H 0 in approximately 800 mL DI water Dilute to the mark and mix with a magnetic stirrer for at least four hours The solution can be stored in plastic for up to two months if refrigerated By Weight To a tared 1 L container add 40 0 g ammonium molybdate tetrahydrate NH Mo O 4H 0 and 983 g DI water Mix with a magnetic sti
357. ssa e sues sess esee eate eee etn nana eee 16 NUMBERING ERROR CORRECTION PROCEDURES eee eee eene entente nennen 17 CHAIN OF CUSTODY EE 18 CUSTODY FORMS dM MO REL oot tore 18 C of C SAMPLE PROCESSING PROCEDURE sssosssssssssssrseseseenenenensssssenanenocssonsncassrsescsees 18 PRIORITY AS BALDI 21 PRIORITY SAMPLE PROCEDURE eee eee eese ense eene otn etta aatia ae ease etn sheets ase a seen neto tenue 21 Maximum Analytical Times Priority Options Chart eene eee eene eene tenente ennt 22 SPECIAL SAMPLE HANDLING o occcoconononacoconncnonononananonnononanococacononaconanananacanananonorananrcrcnncncnnos 23 SAMPLE RECEIVING EQUIPMENT ooocccocccnociooonnncocannananoconnnancanccnnccncanonranccnnoconananonccnnacrnrccnos 24 SAMPLE RECEIVING MONTHLY REPORTS e eee eren ettet 26 HOLD TIMES LIST TEMERE ERE 27 ENVIRONMENTAL HEALTH SAMPLES eee eee ene eene sete en ases ass tetas aset enses state tno 31 ENVIRONMENTAL HEALTH DATA SHEETS ccccccccoononccoonananacaranconaronacananacococanaconconaenasanoss 33 MDH DATA SHEET RR 33 EH SAMPLES FROM NON MDH COLLECTORS onuccsionosmmossiessincscaccorconeonecannaconaconacccnonosono 34 SAMPLE PROCESSING PROCEDURE occcccccccoononconcaosonncnccccanacnnncncononananococanananconanoncccononanoroos 35 SAMPLE DELIVERY SCHEDULE vnmiccioccononcccnncannnaonncoronaranccnnccncacnanan conca nacoo nooo aestas corn esent ano 35 CHECKIN
358. st must either 1 recalibrate the instrument and then perform the Report Level Verification check once again or 2 perform the RLV at a higher concentration level If an acceptable percent recovery can only be achieved at a higher concentration level the analyst must elevate the report level for the associated samples to the concentration of the lowest point that meets the acceptance criteria The analyst must report all samples analyzed after the failed report level check using the elevated report level until a new calibration curve and report level verification standard meet the acceptance criteria Analysts using the MRLV procedure must follow the remedial actions described in the UCMR2 Laboratory Approval Manual Documentation and other requirements The Report Level Verification procedure RLV or MRLV including the acceptance criteria must be described in the SOP The frequency of any RLV or MRLV must also be stated in the SOP along with action the analyst must take if the acceptance criteria are not met Results of the RLV or MRLV check shall be recorded as directed by the Unit Supervisor or Quality Assurance Officer Documentation and other requirements for modified RLV MRLV or alternative QC procedures If the QAO has determined that an analysis should use either a modified RLV MRLV procedure or an alternative QC procedure in lieu of an RLV MRLV this must be described in the SOP The SOP must state the frequency of such procedures the ac
359. sure to UN light The digestion occurs prior to the injection valve Results for wastewater influent may be up to 3096 low when compared with a rigorous TKN digestion because of sediment in the sample test tube If effluent samples are preserved and filtered in line digestion results will match the manual off line digestion If samples are not filtered in line results will be 1 1596 low compared with off line digestion Surface water samples may not require filtration but this should be verified with a sample containing high levels of solids After digestion nitrate is quantitatively reduced to nitrite by passage of the sample through a copperized cadmium column The nitrite reduced nitrate plus original nitrite is then determined by diazotization with sulfanilamide under acidic conditions to form a 10 107 04 3 D Page 1 2 Dec 2010 sat diazonium ion The diazonium ion is coupled with N 1 naphthyl ethylenediamine dihydrochloride The resulting pink dye absorbs at 540 nm and is proportional to total nitrogen A 3 DEFINITIONS The definitions and purposes below are specific to this method but have been conformed to common usage as much as possible 3 1 3 3 3 3 3 4 3 5 3 6 3 7 3 8 3 9 3 10 ANALYTICAL BATCH The set of samples extracted distilled or digested at the same time to a maximum of 10 samples l CALIBRATION BLANK CB A volume of reagent water in the same matrix as the
360. t The custodian compares the field numbers assigned to the samples by the sampling team leader to those recorded on the custody form If anything is not in order the custodian records information in the comments section on the chain of custody form and notifies the client Entries into all records must be written legibly and erasures or marking shall not obliterate entries in records All corrections must be made by one line marked through the error leaving the original record visible The individual making the correction must sign or initial and date the correction The chain of custody form which is completed in triplicate is distributed as follows the original is kept by the laboratory in a three ring binder the yellow copy is attached to the sample analysis request form and returned to the client upon completion of the analytical work and the pink copy is given to the sampler upon relinquishing custody of the samples When the samples have been properly accepted and logged into the LIMS the sample receipt custodian delivers the samples and any chain of custody forms to the laboratory Information concerning the identification and transfer of civil or criminal chain of custody samples is recorded in a bound log book and the samples are placed in a designated secure storage area While access to general laboratory areas is restricted to authorized personnel the civil or criminal chain of custody samples are further protected in a secure l
361. ta quality objectives of specific projects The laboratory works closely with its clients to develop Quality Assurance Project Plans QAPPs for specific studies These QAPPs define the general problems that are being addressed as well as outlining the boundaries of the investigations including the quality assurance activities conducted by the laboratory to ensure that the needs of the study are met SECTION 10 0 ANALYTICAL PROCEDURES The laboratory analyzes samples from a wide range of matrices drinking water ground water surface water air soils sediments tissue and wastes The Laboratory s internal Standard Operating Procedures SOPs are based on reference methods developed or approved by various state and federal agencies The analytical procedures and reference methods used by the Environmental Laboratory Section for various state and federal programs are listed in the Environmental Laboratory Handbook The handbook does not list sensitive information such as the procedures and methods for chemical terrorism response Minnesota Department of Health Quality ee Manual Public Health Laboratory Division Filename qao0 ironmental Laborato Revision 9 did Effective Date Date of last signature i Page 32 of 67 http fyi health state mn us phl environmental index html A E The handbook is posted at both the internal website http fyi health state mn us phl environmental index html and the external website http
362. tandard by this factor to give final weight 10 115 01 3 E Post MUR Page 6 3 December 2010 sat 7 4 PREPARATION OF DIGESTION CHECK STANDARDS Stock Standard 1 1000 mg P L as pheny phosphate PP By Volume In a 1 L volumetric flask add 8 20 g phenyl phosphate C HsOP ON ONa 2H20 FW 254 09 in about 800 mL DI water Dilute to the mark with DI water and invert to mix Prepare fresh monthly Stock Standard 2 1000 mg P L for trimethyl phosphate TMP By Volume Ina 1 L volumetric flask add 4 5 g trimethyl phosphate CH30 3P O FW 140 08 in about 800 mL DI water Dilute to the mark with DI water and invert _ to mix Prepare fresh monthly Stock Standard 3 1000 mg P L for sodium pyrophosphate 2P v By Volume Ina1L volumetric flask add 4 292 g sodium pyrophosphate Na4P207 Fw 265 90 in about 800 mL DI water Dilute to the mark with DI water and invert to mix Prepare fresh monthly l Za Stock Standard 4 1000 mg P L for sodium tripolyphosphate 3P By Volume In a 1 L volumetric flask add 4 66 g sodium tripolyphosphate 85 NasP3010 FW 367 86 in about 800 mL DI water Dilute to the mark with DI water and invert to mix Prepare fresh monthly Working Stock Standard Solution 10 0 mg P L By Volume In a 1 L volumetric flask about 550 mL Solution 1 1 5 mL H SO4L and 10 0 mL Stock Standard 1 2 3 or 4 Dilute to the mark with Solution 1 Invert to mix By Weight To a tared 1 L container add abo
363. te List We use four of the selections under this heading Once a list is selected it will print automatically Bottle Type List List of all bottle types and all of the analysis codes that are run from each type Assoc An List List of all analysis codes that are associated with other analysis codes When the listed code is assigned the other code will automatically default in Def An by Prog Lists by number all the default analysis lists that have been created for each program code View Lab Review This is used to look up data including results via the Sample PWS ID Collection Date Collector Program Code or AN Code PWS Table View This is used to find PWS ID numbers PWS names and addresses via the facility name city zip code etc Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 8 of 57 e INITIAL DATA ENTRY PROCEDURE Most computer functions can be performed by using the keyboard or mouse or a combination of both The Enter or Tab keys are used interchangeably to move from one field to the next 1 From the main screen select Entry and pull down to select Initial Entry 2 The cursor will be on the Beginning Sample on the Initial Entry Screen 3 Type in the 9 digit sample number beginning with the year and then press Enter Tab to go to the next field Example 200
364. th every analytical batch of no more than twenty samples a midrange standard must be prepared using the procedure described in Section 11 10 115 01 3 E Post MUR Page 10 3 December 2010 sat 9 7 9 8 9 6 1 Compare the results with the current laboratory acceptance criteria If the criteria are not met the analytical system is judged to be out of control and the problem must be immediately identified and corrected and the analytical batch reanalyzed Quality Control Samples QCS It is suggested that the laboratory obtain and or prepare a quality control sample using a source different from the source routinely used in section 9 7 1 The QCS is used to verify the concentrations of the calibration standards Depending on the specific program requirements field replicates and field spikes of the analytes of interest into samples may be required to assess the precision and accuracy of the sampling and sample transporting techniques 10 CALIBRATION AND STANDARDIZATION 10 1 10 2 Prepare a series of at least 3 standards covering the desired range and a blank by diluting suitable volumes of standard solution See section 7 2 Set up the manifold as shown in Section 17 Calibrate the instrument as described in section 11 10 3 10 4 Prepare standard curve by plotting instrument response against concentration values A calibration curve may be fitted to the calibration solution concentration response dat
365. that the entire sample was used for the analysis the empty sample container is returned to the secured storage area and the date and time of the return are recorded with the initials of the analyst Once all analyses are completed the original sample containers are stored in the secured storage area until the disposal of the samples has been approved by the client The laboratory provides the client with a list of chain of custody samples which are ready for disposal on a quarterly basis Upon client approval the laboratory properly discards the samples The dates of disposal of such samples are recorded in the chain of custody log book Data Records for Custody Samples Upon the completion of the analytical work and computation of the data a report is generated The analytical results are reviewed by appropriate laboratory staff Once the data have been reviewed and approved for release to the client the data packages are prepared Data generated from the analysis of any sample collected by the client shall not be released to any outside interested party unless the client has provided the laboratory with prior written approval The data package is sent to the client s designated staff person for review The data package includes the original sample analysis request form final results recorded on the form or supplied on attachments the yellow copy of the chain of custody form and any corresponding quality control data requested by the c
366. the Report Level Verification procedure If no such requirements exist the analyst shall utilize the Report Level Verification RLV procedure outlined in 1 below The analyst with the approval of the QAO and the Supervisor may choose the Minimum Reporting Level Verification MRLV procedure outlined in 2 as an alternative Report Level Verification when they have determined that it is more appropriate 1 Report Level Verification RLV Check MN Rules 4740 2100 Subp 8 C One RLV check must be performed each time the instrument is calibrated if the instrument is not calibrated with each use then the RLV shall be performed monthly The RLV can be performed one of two ways 1 by analyzing a standard at or below the reporting level or 2 by recalculating the standard at the report level that was used to determine the calibration curve for the instrument The analyst must choose which of these two RLV procedures will be used for a given SOP The RLV check sample is not required to be processed through the entire SOP preparation steps such as digestion extraction etc can be omitted The percent recovery of the standard must be within limits established for each analysis or analyte by the Quality Assurance Officer Note MN Rules state that the percent recovery of the standard must fall within 40 of the true value 2 Minimum Reporting Level Verification MRLV The MRLV is described in the UCMR2 Unregulated Contaminant Monitoring Regulat
367. the contractor s Represent the MPCA in meetings Section A 4 6 MPCA QA Coordinator William Scruton The MPCA QA Coordinator will Represent the MPCA with the contractor s ensuring adequate exchange of information regarding Project responsibilities and effective functioning of the analytical Project Coordinate analytical needs and projections analytical data reports from the contractor and resolution of problems arising from contract provisions with the analytical laboratory and MPCA staff Review and approve the QAPP including subsequent revisions Notify the contractor of updates and changes in analytical techniques or requirements of federal and state regulatory Projects Update and distribute the Sulfate and Wild Rice QAPP when deemed necessary Wild Rice Sulfate Standard Sediment Incubation Experiment Ouality Assurance Project Plan Section No A 4 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 11 of 44 Provide an overview to the Project Manager of analytical results and quality control data to ensure the laboratory has met Project requirements Section A 4 7 MDH Inorganic Unit Supervisor Jeff Brenner The MDH Inorganic Unit Supervisor will Ensure that the analytical requirements of the QAPP are implemented Provide direct supervision and project assignment to assigned staff Provide direction for the daily work activities Provide technical representation at meeti
368. the custody code were assigned to both sample numbers the submitter would be charged the custody fee twice for the same sampling point Most collectors now list all bottles from a single sampling point on one line so this does not occur often but it is still something we must watch for 8 Write the C of C Unique Form Number found on the upper right corner of the form on all other forms submitted with the C of C form 9 Follow basic sample processing procedures to number the samples date time stamp the data sheet and enter initial entry data in the computer Be sure to enter the C of C code along with the test codes where appropriate see step 8 o 10 Attach the labels to the samples Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature i Page 20 of 57 11 Separate the carbon copies of the C of C form and make a photocopy e The original white form will go in the C of C binder in room L250 e The yellow copy will go to the submitting agency usually the MPCA e The photocopy will go to clerical 12 If they also submitted a single copy data sheet make two photocopies of the data sheet e Staple the original data sheet to the original C of C form for the C of C binder in L250 e Staple one copy of the data sheet to the yellow copy of the C of C form for the X submitting agency usually the MPCA e Staple the
369. the instrument is functioning accurately and consistently and that there are no abnormal matrix effects that may compromise the analytical results At least four or five types of QA QC checks should be performed MB Method Blanks approx every 10 samples o Water blank usually DI water with the exact composition of reagents as samples and calibration solutions and prepared using the same method transfers vials dilutions etc as samples should be run more frequently and after high concentration samples if instrument carryover is experienced OPR Ongoing precision and recovery approx every 10 samples o A check of one of the calibration standards to make sure equipment is still performing as expected For destructive analysis if enough standard volume is prepared initially this can be taken from the same bottle REF Quality control sample or reference material min once per batch o This is a sample of known concentration typically analyzed by another lab which can be used to check our own method against someone else s DUP Duplicates min once per batch or every 20 samples o An exact replicate of one sample prepared from the beginning in exactly the same way not just back to a sample vial that was analyzed previously to test method precision reproducibility MET SPK Method Spike min once per batch or every 20 samples o Thisistypically performed for samples which require complex extraction procedure A known am
370. the laboratory duplicates calculates the RPD and compares the data to past data from the site to verify consistency When all the data points have been reviewed the project manager compares the data which is acceptable to the data which was planned for the site and verifies that the completion rate goal has been met Any problems with the data or laboratory issues are immediately brought to the attention of the MPCA QAC who contacts the laboratory to assess the problems and find a solution If the problem is particularly severe a data audit or full laboratory audit may be conducted Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No D 1 D 2 and D 3 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 39 of 44 Section D 1 3 Data Validation Methods At least 10 of the data are validated by the MPCA QA Coordinator from the raw data The validation process is consistent with the National Functional Guidelines for Inorganic Data Review If any data problems are identified more data packages are validated If data does not meet the QAPP requirements and are judged to be unusable the analyses are not paid for and the samples are re collected Section D 2 Reconciliation with User Requirements Data quality objectives have been met when a complete report with all data qualifiers has been provided to the MPCA Senior Management Team The report includes a
371. the sediment over itself to provide a thorough yet temperate blending Wild Rice Sulfate Standard Sediment Incubation Experiment Quality Assurance Project Plan Section No B 1 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 22 of 44 Microcosm Construction Custom fabricated microcosms consisted of either polycarbonate or acrylic rigid 8 1 D tubing with a polypropylene bottom cap with either Buna N or silicone O rings for sealing Silicone caulk 100 silicone was used to ensure a thorough seal between the bottom plate and the rigid tubing Vinyl Scotch Super 88 electrical tape was used as a final barrier between the tubing the bottom plate and steel t bolt hose clamps which were used to induce a compression seal between the O ring and the tubing Figures 1 4 show the components of the microcosm and its assembly Microcosm Filling Homogenized sediment was transferred to microcosms and consolidated To minimize soil disturbances the Rhizon filters were pre installed into tapped holes made in the microcosms Pre installing the filters allowed the microcosms to be thoroughly tested for leaks so as to prevent advection of fluid through the duration of the testing and allow for uniform consolidation of the sediment surrounding them A plastic trowel was used to quickly transfer the sediment from the large mixing container to the microcosm to reduce exposure to the air The sediment was consoli
372. tion of Capability Study in Appendix 10 p 57 58 of the QA Manual Intermediate Standard A solution made up from the stock standard solution and diluted as necessary to prepare working standard solutions Internal Standard IS A constant amount of non target analyte that is added to all samples blanks and standards The internal standard calibration process may be used to calculate the concentration of target analyte s and surrogate s that are components of the sample or solution The internal standard should not be present in the original test sample at interfering levels and should behave similarly to the target analyte s Ideally the retention times of internal standards should be near the retention times of the associated target analytes See individual SOPs for additional criteria applicable to the use of internal standards Internal Standard Calibration The process of creating a mathematical relationship by comparing the instrument response of a target analyte in a calibration standard to the response of an internal standard added to the calibration standard The relative response factor RRF created by this process is used to calculate the concentration of the target analyte in other samples to which the internal standard has also been added Internal standards are used to correct for routine variations in instrument response extraction efficiency and or for variations in the exact Minnesota Department of Health Quality Assura
373. tion B 7 Instrument Equipment Calibration and Frequency sese 32 Section B 7 OVetVIew esee eaa oreet arabe e ete Eee terr ee aiii 32 Section B 7 2 Laboratory Procedures ooooonoccnonononcnnnconnnonononcnnncnnncnnoco neon nooo nc nono nono nn ene ennetene tenete nennen nee 32 Section B 8 Inspection Acceptance of Supplies and Consumables eee 33 Section B 9 Data Management ete ne iere ORE ee e ERES SSE EE ERE Pe EUR IR rts 33 Section B 9 1 Data R cording eiie tiep E eripe Debe E e carb ERE hee ere ensis 33 Section B 9 2 Data tr nsfOrm tiOnD see ere rer ee rent e eet pl d reiten 33 Section B 9 3 Data Transmittal eco eese tete teet ee dete tette etc deer tees a d debe 33 Section B 9 4 Data Rejection ned dd 33 Section B 9 5 Data Tracking serene eR tes 34 Section B 9 6 Data Storage and Retention ee eee eeceesceseceecesecesecsaecaeecseeeseseaeseeeeseseeseeseensesnseenas 34 Section C Assessment and Oversight et eee ie o e n rte ic eee re tree dede eec 35 Section C T Response Actions cete eredi rere cei EEA E edge us inen Pe ee HER de evene doctae iubeas 35 Section C 1 1 Laboratory Audits eese nennen nenne trennen teen nee nente nnne 35 Section C 1 2 Performance Evaluation PE Studies esses eene 35 Section C 2 Corrective Action Reports to Management ocooccocccononononnncnnnnnnnonnnonoco noc eene enne eene nen
374. tion Date Time click on the button near the middle of the screen This will take you to another screen where the date and time can be edited Editing Field and Trip Blank information This information can only be edited through the initial entry screen and only one sample can be edited at a time 1 Once inside initial entry hit F7 or click on the Enter Query button at the top of the screen to put it in Qu ry Mode 2 Type in the sample number and then hit FS or the Execute Query button 3 This will pull up the information on the sample and allow you to edit the Field Blank and or Trip Blank info 4 After making changes hit F3 to commit the changes to the database X Repeat as needed to edit additional samples Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 13 of 57 USING THE VIEW SCREENS TO FIND SAMPLE RECORDS The View screens can be used to obtain missing sample information look up results or search for specific samples There are five options listed under View but we only use the first and last options Lab Review and PWS Table View Lab Review Screen 1 From the main screen use the mouse to select View and pull down to select Lab Review 2 The screen will read Data Review by and will list four search options Sample Number PWS Number Collect Date and Collecto
375. tion No B 5 Revision No 0 Date 12 9 2013 Effective Date Date of Last Signature Page 30 of 44 Table 6 QC Acceptance Criteria for Target Analytes in Sediment Target Analyte Blanks LCS R MS R Duplicates RPD Laboratory Appendix Acid Volatile Sulfide AVS lt RL 70 130 80 120 50 MDH Environmental Appendix C ICP MS for Extractable lt RL 70 130 80 120 50 UMD CE Appendix D Metals Total Sulfur lt RL 70 130 80 120 50 LacCore LRC Appendix E Total Carbon lt RL 70 130 80 120 50 LacCore LRC Appendix E Total Nitrogen lt RL 70 130 80 120 50 LacCore LRC Appendix E Percent Solids lt RL 70 130 80 120 50 MDH Environmental Appendix C Section B 5 1 1 Method Blanks One method blank is prepared and analyzed with each batch of up to 20 samples to demonstrate that there are no interferences from the glassware reagents and analytical system Target analytes of concern should not be present in the method blank at the report level concentration If any method blank shows target analytes above the report level an instrument blank should be analyzed to demonstrate that there was no carry over from standards or samples If there was carry over clean the analytical system and re inject the method blank If the method blank contamination cannot be attributed to carry over the samples that were associated with the blank should be re prepared and re analyzed Section B 5 1 2 Matrix
376. to the blank column of the Sulfur Coulometry Template There will be no weight recorded for your blank a After you have blank entered into the spreadsheet it will automatically correct each sample and standard 2 Enter standard and sample mass resultant ug S and sample run time the sulfur coulometer displays the sample run times in the coulometer into the Sulfur Coulometry Template a This spreadsheet will automatically calculate the 96 TS equation below demonstrates the calculation the spreadsheet makes for you Make sure that your standards and duplicates are within the acceptable range If standards and duplicates are not within the acceptable range samples must be run again Document History and References Atkin B P Somerfield C 1994 The determination of total sulphur in geological materials by coulometric titration Chem Geol 111 131 134 Wilkins Bischoff 2006 Coulometric determination of total sulfur and reduced inorganic sulfur fractions in environmental samples Talanta 70 4 766 773
377. tus For Emergency samples there should be an additional note on the memo or data sheet requesting Emergency status 1 Write Priority 1 or Emergency at the top of the data sheet 2 Process the samples up to initial entry During initial data entry you will need to change the priority level for each analysis code In the Pri column change the 3 to a 1 or 0 3 Press the F3 key to commit the data when you are finished o 4 Use the eDiting screen to enter the received date in the Priority Memo date field This date is used to calculate the holding time for priority billing purposes You can also change the priority status at this time if you forgot to do so during initial entry Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 22 of 57 5 Attach the labels to the samples 6 Make copies of the data sheet and separate memo if necessary one copy for each Unit Supervisor involved one for Sample Receiving and one for the Lab Manager Also make extra copies of the data sheet to give to the lab analysts to help remind them of the priority status 7 Deliver the samples to the appropriate labs making sure that the analysts are aware of the priority sample status 8 Runa Daily Entry Log List for the priority samples and deliver it to clerical Write Priority on top of the log sh
378. ual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 21 of 67 http fyi health state mn us ph l environmental index html laboratory personnel approves staffing plans and has overall responsibility for the administration of the Environmental Laboratory Management includes laboratory operations and project management functions which have responsibility for ensuring that analyses are conducted according to program requirements establishing contracts compiling and distributing reports and preparing budgets Environmental Laboratory Quality Assurance Officer ensures that the quality of the data generated by the laboratory meets the goals of the laboratory s policies maintains quality assurance records conducts internal audits requires and tracks corrective actions and responds to requests for corrective actions due to deficiencies noted during external audits by the USEPA clients or proficiency testing studies Environmental Laboratory Testing Unit Supervisors are responsible for supervision of analysts They also ensure that testing procedures are current and accurate adequate training is provided and documented for all analysts required quality control practices are performed analysts perform timely review of QC results data are appropriately reviewed for errors in calculations or transcriptions and all out of specification situations are reso
379. ublic Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 29 of 57 e TESTS WITH A 7 DAY HOLD TIME 1 Solids 2 Solids total volatile 3 Solids suspended 4 Solids suspended volatile 5 Solids total dissolved 88 Sulfide 283 pHin sediment 402 SVOC s in water by GCMS BNA 410 Dalapon SDWA 411 Haloacetic Acid ICR 420 PCB Aroclors in water 470 PAH in water by HPLC 474 DRO in water 476 DRO in sediment 500 PCB oil 510 PAH in water by GCMS 512 PAH in water by GCMS SIM TESTS WITH a 14 DAY 2 WEEK HOLD TIME 22 Alkalinity total 26 Cyanide Free SDWA 69 Nitrate Drinking Water 86 Cyanide total 90 Cyanide amenable 406 Herbicides 407 BNA s by GCMS SDWA 409 Glyphosate 412 Haloacetonitriles 413 Chloral Hydrate 462 VOCs special 463 VOCs amp Gas fuel 464 THMs 468 VOCs 473 GRO in water 475 GRO in sediment 498 VOCs White Caps UNPRESERVED METALS Including Copper Lead Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory l Effective Date Date of last signature Page 30 of 57 e TESTS WITH A 28 DAY 4 WEEK HOLD TIME 14 Conductance 25 degrees C 23 Chloride total 27 Sulfate total SDWA 28 Sulfate total turbidimetric 29 Fluoride total 30 Silica 37 Fluoride dissolved 46 Chloride dissolved 48 Sulfate dissolved 49 Sulfate
380. ubmitted some substitutions can be made Non thiosulfate Bacteriology bottles can be used for fluoride nitrate nitrite and sulfate General bottles can be used for nitrate if sample is 2 days old or less Nutrient bottles can be used for nitrate this is routinely done by the MPCA Free Cyanide and Total Cyanide bottles are interchangeable if there is adequate sample volume Other substitutions may be possible check with the lab when incorrect bottles have been submitted In all cases above check with the laboratory before submitting the sample and write a receiving comment that briefly describes the bottle substitution Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 37 of 57 Bacteriology samples must be submitted in a sterile bottle preferably our own Colilert Thiosulfate or Non Thiosulfate bottles Occasionally a collector may submit a bacteriology sample in their own sterile bottle and this is usually acceptable but check with the laboratory before submitting If the bottle submission problem cannot be resolved Notify the collector or appropriate EH Rep via phone or email List the analyses that cannot be run and why If some of the analyses can still be run cross out the codes that willnot be run Make note of the cancelled analyses and the date the collector was notified under Receivin
381. uction during development of the method i Although Lachat Instrument publishes method performance data including MDL precision accuracy and carryover studies we cannot guarantee that each laboratory will be capable of meeting such performance Individual laboratory and instrument conditions as well as laboratory technique play a major role in determining method performance The support data serves as a guide of the potential method performance 10 115 01 3 E Post MUR Page 13 3 December 2010 sat Some labs may not be able to reach this level of performance for various reasons while other labs may exceed it 14 POLLUTION PREVENTION 14 1 14 2 14 3 Pollution prevention encompasses any technique that reduces or eliminates the quantity or toxicity of waste at the point of generation Numerous opportunities for pollution prevention exist in laboratory operation The USEPA has established a preferred hierarchy of environmental management techniques that places pollution prevention as the management option of first choice Whenever feasible laboratory personnel should use pollution prevention techniques to address their waste generation When wastes cannot be feasibly reduced at the source the Agency recommends recycling as the next best option The quantity of chemicals purchased should be based on expected usage during its shelf life and disposal cost of unused material Actual reagent preparation volumes should reflect anti
382. uded or referenced positive and negative culture controls gt confirmation verification of presumptive total coliform positive samples sterility controls proficiency testing and quality control samples SECTION 14 0 DATA REDUCTION VERIFICATION VALIDATION AND REPORTING The laboratory performs data reduction and validation in accordance with the requirements in the approved methods and as cited in the Code of Federal Regulations The laboratory uses Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 36 of 67 http fyi health state mn us phl environmental index html the USEPA guidance documents as cited in Section 16 0 and clients project specific quality assurance plans to validate the data produced A Reduction and Validation Process Raw data are transformed into reportable results using mathematical calculations and analyte identification obtained from direct readings from instruments or calculations based on instrument output readings or response Data reduction activities may be conducted manually by analysts converting analytical output to sample concentrations using calculations or automatically using instrument or other validated computer software The laboratory maintains records demonstrating that the calculations provide the expected results Factors such as dil
383. uminum alternating coil support PVC PUMP TUBES MUST BE USED FOR THIS METHOD Tee s 1 and 2 are mounted on left side of manifold board From sampler to tee fitting 1 The black pump tube is cut 3 cm outside of the tabs on both sides The outlet of the black sample pump tube is connected to tee fitting 1 with 50 cm of 0 8 mm id manifold tubing From digestion reagents 1 and 2 Orange white pump tubes are connected to tee s 1 and 2 through 50 and 50 cm lengths of manifold tubing Heater inside of the sample prep module a total of 880 cm of 0 032 i d manifold tubing is used 700 cm is wrapped on a high temperature heater with 90 cm remaining for connection at the inlet and outlet The outlet of tee 1 is connected to a 4 5 cm coil The outlet of the coil is connected to the heater inlet and the heater outlet is connect to the inlet of tee 2 Tee s 1 and 2 are mounted on the chemistry manifold board l The UV 254 lamp inside of the sample prep module has 450 cm of zeus tubing Lachat Part No 50728 wrapped around the UV lamp with 50 cm for a 10 115 01 3 E Post MUR Page 21 3 December 2010 sat Note 6 Note 7 Note 8 Note 9 Note 10 total of 550 cm of tubing remaining at each end for connections The outlet of tee 2 is connected to the UV inlet and the UV outlet is connected to the tubular membrane debubbler a Aluminum coil support Alternating aluminum coil sup
384. ur samples diluted are necessary to be adjusted to 2 HNO3 using 10096 HNO3 The amount of 10096 HNO3 needed to add to samples is calculated based on the final volume of your sample and the content of HNO3 originally contained in your sample iii To be sure a smooth analysis process put no less than 3 ml of each sample in vials that are set in trays of auto sampler If you need replicate from the same vial consider to double the sample volume 9 Data processing a After running a batch of sample with the plasma shut down the data can be processed and reprocessed Go to Dataset tab on main menu from the list of the analyzed samples select the ones you are to process In the column of Read type define the selected samples as blank sample standard spike etc by right click and make appropriate selection on the pop out window Double check the columns of Aliquot Volume and Dilute to Volume for each selected sample correct it if necessary This can save you quite some time in reporting the results Click the button of Summary Report to set up a file to receive a summary result of your processing Check Use original Conditions if nothing change from the original conditions e g aliquot volume method file etc Uncheck this option if you made any change from the original condition for this reprocess Check Save Reprocessed Data if you want to save a copy of the reprocessed data which is useful for you to v
385. us by phone email or fax o If a collector calls ask them for the following information Collector Name Date and time samples willarrive at MDH Total number of samples Analyses requested on each sample Sample type lake water stream water sediment paint etc Priority One Chain of Custody Information If they domot provide enough information in an email fax or phone message contact them for more detail e Pass this information onto the lab by sending a New Task through GroupWise to the bactichem unit Be sure and mark the correct day of delivery in the message Sandy Bissonette and Beth Endersbe of the MPCA collect water samples on a routine basis from the spring through the fall of each year They provide us with their planned schedule ahead of time usually via email They frequently order BOD and Fecal Coliform tests They collect these samples from six different routes or loops MPCA SAMPLE BOTTLE ORDERS MPCA Warehouse Bottle Supply The MPCA stocks their warehouse with MDH bacteriology cyanide metals mercury nutrient Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last Sonate Page 50 of 57 and general all 3 sizes bottles They fill most of their bottle orders from that supply The MPCA courier Ed Norwig drops off and picks up bottle orders when he brings samples in Standing Month
386. used multiple times For these bottle types Fluoride Nitrate Cyanide and Microbiology we need to peel back 1 3 of the backing on both sides of the label and fold the backing toward the middle of the label Place the label on the bottle so that only the sides of the label adhere to it This makes it easier to remove the labels for cleaning Refer to the data sheets as you label to ensure labels are placed on the correct samples If bottles are wet wipe them off with disposable towels and or use rubber bands to hold the labels in place The labels will print out grouped by bottle type The upper right label for each group should describe which bottle they are for Special Sample Bottle Labeling BOD CBOD samples s part of the processing of these samples the lab will submerge them in water so the regular labels will not work Using a black sharpie permanent marker write the sample number on a 1 x 2 1 2 white shamrock label Place this label on the shoulder of the bottle and deliver the printed labels along with the samples to the lab Chlorophyll Pheophytin filter Unwrap the filter s and make sure the filtered volume is written on the petri dish If it is not check the data sheet for this info and write it on the dish If the volume is not on the data sheet either call the collector Place one label with just the sample number no test code on the petri dish containing the filter Do not cover any information written on th dish R
387. ut 10 g Stock Standard 1 2 3 or 4 Divide the actual weight of the solution added by 0 01 and make up to this resulting total weight with Solution 1 1 5 mL H SO4L Shake to mix Working Standard Concentration ug P L By Volume Volume mL of stock standards 1 2 3 or 4 12 5 diluted to 250 mL with Solution 1 Volume mL of Standard A diluted to 250 mL with Solution 1 By Weight Weight g of stock standards 1 2 3 or 4 diluted to final weight 250 g divided by factor below with Solution 1 Weight g of Standard A diluted to final weight 250g divided by factor below with solution 1 Division Factor Divide exact weight of the standard by this factor to give final weight 10 115 01 3 E Post MUR i Page 7 3 December 2010 sat 8 SAMPLE COLLECTION PRESERVATION AND STORAGE 8 1 S2 8 3 Samples should be collected in plastic or glass bottles All bottles must be thoroughly cleaned and acid rinsed The volume collected should be sufficient to insure a representative sample allow for replicate analysis if required and minimize waste disposal For NPDES monitoring samples must be preserved by addition of concentrated H SO to pH lt 2 This is accomplished by adding no more than 1 5 mL concentrated H SO per liter and verifying that the pH is less than 2 If the pH is still greater than 2 more sulfuric acid is add d until the pH is lt 2 Samples are stored at lt 6 C Acid pres
388. ution sample weight sample volume and significant figures are accounted for in data reduction formulas described in each standard operating procedure Manual integration is allowed if peaks are not properly integrated by the instrument software All manually integrated peaks are clearly identified and documented to show how and why the manual integration was selected over the automated peak integration result Analytical batches include QC data as specified per the method requirements and client requests When the analyst batches samples the LIMS will add appropriate QC samples to the run log to assure the analysis includes method required QC and client requested QC items The LIMS captures results of QC sample analysis from the instrument and allows the laboratory staff to plot control charts from QC data Typically the laboratory staff monitors results of matrix spike matrix spike duplicates sample duplicates laboratory control samples blanks and various other measurements For QC plotting the laboratory staff may select the number of points to include in a graph or viewable data In some cases additional data are needed for monitoring trends and the analysts may query additional data or display a larger number of points from the analysis dates selected Method required limits or in house acceptance limits are set for each method and matrix analyzed Acceptance limits may also be specified by the client to meet a data quality objective D
389. vation then standards should be prepared to match the acid level of tbe samples Solution 1 1 5 ml L Sulfuric acid By Weight To a tared 4 L container add 3994 g mL DI water and then add 11 04 g 6 mL sulfuric acid H2SO4 and mix f Standard 1 Stock Standard 250 mg P L In a 1 L volumetric flask dissolve 1 099 g primary standard grade anhydrous potassium phosphate monobasic KH PO that has been dried for one hour at 105 C in about 800 mL DI water Dilute to the mark with DI water and invert to mix Prepare monthly Standard 2 Intermediate Stock Standard 1 0 mg P L By Volume Ina1L volumetric flask add about 550 mL solution 1 and 4 0 mL Stock Standard Standard 1 Dilute to the mark with solution 1 Invert to mix Prepare weekly By Weight To a tared 1 L container add about 4 g Stock Standard Standard 1 Divide the actual weight of the solution added by 0 004 and make up to this resulting total weight with solution 1 Shake to mix Prepare weekly RE Working Standards Working Standards Prepare Weekly Concentration mg P L By Volume Volume mL of stock standard2 diluted to 250 mL with solution 1 Volume mL of Standard D diluted to 250mL with Solution 1 By Weight Weight g of stock standard 2 diluted 125 to final weight 250 g divided by factor below with solution 1 Weight g of Standard D diluted to 250g with Solution 1 Division Factor Divide exact weight of the s
390. ve Date Date of last signature Page 13 of 67 http fyi health state mn us phl environmental index htmi apparatus that may give false positive results The MB is also known as a Laboratory Reagent Blank LRB laboratory blank laboratory method blank reagent blank or preparation blank Method Detection Limit MDL The minimum concentration of an analyte that can be measured and reported with 99 confidence that the concentration is greater than zero The MDL is determined from multiple analysis of samples in a given matrix containing the analyte See 40 CFR 136 App B for the procedure used to determine the MDL Minimum Reporting Level MRL The lowest concentration for which future recovery is predicted to fall with high confidence 99 between 50 and 150 For additional information see the UCMR2 Laboratory Approval Manual version 2 0 October 2006 Monthly Applies to those months during which the analysis is performed Must Describes an action activity or procedural step that is required Must is synonymous with shall National Environmental Laboratory Accreditation Conference NELAC A voluntary association of state and federal agencies whose purpose is to establish and promote mutually acceptable performance standards for the operation of environmental laboratories The current name for this association is The NELAC Institute TNI National Environmental Laboratory Accreditation Program NELAP The overall National En
391. ver the samples to the Organics Laboratory with copies of the paperwork Minnesota Department of Health Sample Receiving Procedure Manual Public Health Laboratory Division Revision Environmental Laboratory Effective Date Date of last signature Page 55 of 57 MINNESOTA OSHA LABOR AND INDUSTRY SAMPLES Minnesota OSHA is part of the State Labor and Industry Agency They collect IBVOSDERHVO samples from worksites as part of their response to complaints OSHA very rarely submits any water samples Instead they submit Bulk samples for Metals and Asbestos Carbon Air filters for solvents Cartridge filters for formaldehyde Cassette filters for Metals and Silica Dust samples for Metals Paint samples for Metals Wipe samples for Metals Other Miscellaneous samples THE PROGRAM CODE FOR ALL MN OSHA SAMPLESAS MG The Data Sheet used for MN OSHA samples does not have analysis code columns nor does it have the Program Code printed anywhere This makes it more difficult to process the samples because we have to look up the analysis codes for each set of samples that come in One section of the form has a list of Analytical Methods that looks like this Metals AAFL AAFU ICP Solvents GC GC MS HPLC Asbestos Ph C PLM TEM Silica X ray Misc Analysts are supposed to circle the method they want and we use the afed to help determine which analytical codes to assign and which Lab Unit should receive the samples Sometimes they wr
392. verified before continuing analysis Periodic reanalysis of the QCS is recommended as a continuing calibration check 10 115 01 3 E Post MUR Page 11 3 December 2010 sat 11 2 CALIBRATION PROCEDURE 11 2 1 11 2 2 11 2 3 11 2 4 Prepare reagent and standards as described in section 5 Set up manifold as shown in section 12 l Input data system parameters as in section 12 Pump DI water through all reagent lines and check for leaks and smooth flow Switch to reagents and allow the system to equilibrate until a stable baseline is achieved 11 2 5 11 2 6 Place samples and or standards in the autosampler Input the information required by the data system such as concentration replicates and QC scheme See Section 12 Calibrate the instrument by injecting the standards The data system will then associate the concentrations with the instrument responses for each standard 11 3 SYSTEM NOTES 11 3 1 11 3 2 11 3 3 11 3 4 11 3 5 11 3 6 For information on system maintenance and troubleshooting refer to the Lachat Troubleshooting Guide in the System Operation Manual Allow more than 20 minutes for the heating unit in the sample prep module to warm to 120 C Tubing crimp formation has been observed in the past with the PTFE manifold tubing when no liquid is running through heater tubing and the tubing is allowed to bake Running liquid DI or reagents through the heater whenever the temperatur
393. vironmental Laboratory Accreditation Program of which NELAC is a part Percent Recovery A measure of the accuracy of a measurement in a given matrix A known amount of analyte is added to a blank or sample and the concentration found is divided by the concentration of the spike The result is multiplied by 100 to express the value in percent The formula is as follows Cs Cu t x 100 Recovery where C Measured concentration of the spiked sample aliquot or blank C Measured concentration of the unspiked sample aliquot Use 0 for an LFB or LCS C 7 True value of the concentration of the spike added to the sample or blank Percent Relative Standard Deviation RSD A measurement of the precision of a series of replicate analyses where the Standard Deviation S of the replicates is expressed as a percent of the mean X value To calculate Minnesota Department of Health Quality Assurance Manual Public Health Laboratory Division Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 14 of 67 http fyi health state mn us phl environmental index html RSD x100 where S Standard Deviation X Mean value Post Digestion Spike PDS An aliquot of a sample to which known quantities of the target analytes are added after digestion to determine matrix effects Precision The measure of mutual agreement among individual measurements of replicate samples under
394. vision Filename qao001 Environmental Laboratory Revision 9 Effective Date Date of last signature Page 66 of 67 http fyi health state mn us phl environmental index html Appendix 13 Corrective Action Form for Non conforming Work Corrective Action Form CAF Corrective Action Form Revision 3 Created on 04 16 08 Page of 2 Paramctcr s CAF Number completed by QAO PT Program if applicable Issue Date date of observed deficiency CAF Due Dale 2 weeks afler Issue Date A corrective action form is required when departures from the established quality assurance and quality control policies and procedures occur or in the event of a proficiency test PT failure Non conformance activities and PT failures require an investigation and documentation of potential causes and corrective actions The analyst should complete the Corrective Action Form CAF within avo weeks of recognizing the deficiency The Quality Assurance Officer reviews and files the original submission and monitors the corrective action progress and effectiveness AnalysVinvestigator Report Value Sample Number s Truc Value Analysis Date i Control Limit Ranges Method Instrument Acceptance Range if applicable Description of Problem check those that apply Anerror in transcription dilution decimals units calculations and or significant figures e g compare instrument printout with result sheet and compare graded PT report wit
395. will be the time that should be entered in the software as the sample reaches first valve 10 107 04 3 D 2 Dec 2010 sat 17 2 SUPPORT DATA FOR QUIKCHEM 8000 8500 Calibration Data for Total Nitrogen Low Range File Name OM 11 19 2007 12 48 56PM OMN Acq Date 19 Nov 2007 Calibration Graph and Statistics MIZ Calibration Results Channel 1 i 5 BEE FINI a F l RE 11 19 2007 141 9 2007 Conc 5 13e 5 Area 2 0 0612 Area 0 0557 Correlation Coefficient r 0 99999 Weighting 17x 10 107 04 3 D Page 17 2 Dec 2010 sat 0 0372 4 0 0264 mg E a 2 0241 SS wan 0 0240 mon Y a 9 0245 ma m ea prm 4 i ENDE ps ja ii a de Pn ER AA j 4 1 80 3 Time 25e3 Method Detection Limit for Nitrogen using a 0 02 mg N L standard MDL 0 003 mg N L Standard Deviation s 0 00096 mg N L Mean x 0 025 mg N L Known Value 0 02 mg N L File Name OM_11 19 2007_12 48 56PM OMN Acq Date 19 Nov 2007 1 08 Voks 2 0857 Ma 25e 3 Time sj Precision Data for Nitrogen using a 1 0 mg N L standard RSD 0 75 Standard Deviation s 0 0075 mg N L Mean x 1 00 mg N L Known Value 1 00 mg N L File Name OM 11 19 2007 12
396. y means that sample possession must be traceable from the time samples are collected until the samples or their derived data are used for enforcement purposes or are introduced as evidence in legal proceedings A Chain of Custody Form C of C must accompany the samples a d all parties handling the samples must sign the form in the designated place on the form at the appropriate time There are several acceptable methods for submitting Chain of Custody samples 1 The collector may use a MDH C of C in addition to their regular data sheet 2 The collector may use the MDH C of C alone and write all of the necessary data on it 3 The collector may use the Chain of Custody Form provided by their agency or company There are three custody status choices on the MDH C of C Standard Civil and Criminal Custody Forms provided by other agencies usually have the same three custody status choices When samples come in accompanied by a C of C form ask the collector if the samples are Chain of Custody The collector or submitter should select the appropriate option by circling it on the form based on their desired level of custody Standard This is for samples that do not require true Chain of Custody handling Often the C of C form is used for regular sampling The forms should still be signed but there is no custody code to assign for such samples and they should be processed as normal Civil This is for custody samples that may go to
397. y Handbook The handbook also covers information about ordering bottles scheduling samples with the lab delivering samples and special custody guidelines The handbook is posted at both the internal website http fyi health state mn us phl environmental index html and the external website http www health state mn us divs phl environmental handbook internet envhandbook html Information on all samples is entered into the laboratory s computer data base First the sample receiving staff records a unique laboratory sample number which is then associated with all the analyses that are requested on the sample The sample receiving staff also enters a project code ID and the received date Labels which indicate which analyses are to be performed on each of the sample containers are then printed and put on the bottles Secondly the sample receiving staff enters information about the site location and the date and time of collection Samples are delivered from the sample receiving area to the Inorganic Chemistry Unit or the Organic Chemistry Unit to perform tests All samples are stored separately from standards and reagents to prevent cross contamination and are returned to the appropriate storage area after sufficient sample has been obtained for analysis Sample fractions extracts and other items created during sample preparation are stored in accordance with the requirements of the analytical procedure Analysts use queries to generate w
398. y Manager Sample Receiving Unit mm m Inorganic Chemistry Unit Supervisor B A Lm ES 4 Analysts in the Inorganic Chemistry Unit oo EA Organic Chemistry Unit Supervisor Quality Assurance Officer o Operations Unit Supervisor o Analysts in the Organic Chemistry Unit Radiation Project Safety Officer Coordinators mE Clinical Laboratory Section p Minnesota Department of Health Public Health Laboratory Division Environmental Laboratory Quality Assurance Manual Filename qao001 Revision 9 Effective Date Date of last signature Page 43 of 67 http fyi health state mn us phl environmental index html Appendix 2 Training Record for an Individual Standard Operating Procedure MDH Environmental Laboratory Document Number 2006 02 ANALYST ANALYSIS AN CODE Date Received MDH SOP w EIA Read Reference Method Reviewed Methods with Trainer washed Method Performed is icine Procedures with zo joe Lo 33 YE date 2 ES op etu o a Completed MDL Stud MN Comprise pe suey 14 Additional Comments and Notes 1 we certify that the training for this method has been completed Wainer 1 signature date trainer 2 signature date Page 1 of 1 L agree to follow this method as presented agree that will not make changes to this method without supervisor s approval analyst signature at completion of training
399. ystems serve only one Mobile Home Park or apartment building The system operator usually submits the bacteriology fluoride nitrate and other routine samples while MDH Sanitarians collect non routine samples NON COMMUNITY SYSTEMS These private systems usually serve one facility and they are usually smaller than community systems However it is possible for a large factory private to serv more clients than a Mobile Home Park public The system owner usually submits routine samples while MDH Sanitarians collect non routine samples Transient means that individuals use the system no more than 8 hours day on average If the facility is a business it has no more than 25 employees Non transient means that individuals use the system more than 8 hours day If the facility is a business it has more than 25 employees The same population uses the facility on a daily basis The HD Program Code is assigned to licensed facilities with short term transient use Examples are resorts campground golf courses restaurants and supper clubs The HU Program Code is assigned to non licensed facilities with short term use Examples are churches parks wayside rests and small businesses The HW Program Code is usually assigned to non licensed facilities with long term non transient use Examples are schools daycare centers factories and larger businesses Minnesota Department of Health Sample Receiving Procedure Manual Public H

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