Unofficial Copy - City of Winnipeg
Contents
1. Reagent Preparation Logs All forms reagent logs located in 7urbidityForms xlsx Obtain or download Certificates of Analysis COA for all purchased standards and CRMs Print a LIMS label for placement on the certificate which is then scanned and saved as PDF file in the COA folder Document the calibration of secondary standards on the reagent preparation log sheets and LIMS Chemicals and Standards Label reagents with Material Name Concentration Date Prepared Expiry Date Analyst Initials and Reagent Prep Log Reference Number or LIMS CRM Number Expiry Dates Unless specified all reagents in solid form have an expiry date of 5 years when unopened and 3 years from the date opened Purchased reagents in liquid form have an expiry date of 3 years unopened and 12 months opened All prepared reagents are considered opened on the date made and therefore never exceed 12 months If the vendors expiry date is less than these default dates then use the vendors i e always use the shortest date SOP 15 Turbidity v5 1 docx 6 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 7 of 15 Refer to LIMS Instrument Module and Equipment Logs Instruments Hach 2100N with filter compliant with USEPA 180 1 Hach 2100Q compliant with USEPA 180 1 this portable Nephelometer is a laboratory met2. Action If any of calibration verification duplicate recovery control is outside of the control limits then run two primary calibration standards as a check If one or more of the primary calibration standard s is out and the primary standard has not expired recalibrate the instrument with the primary standards and calibrate the secondary standards If the primary calibration standards are acceptable recalibrate the secondary standards Make sure that the standards have not expired SOP 15 Turbidity v5 1 docx 8 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 9 of 15 Check the sample cell for large scratches or defects in the glass Replace with new ones and index as necessary Do not keep the scratched cells that are causing problems but dispose in the broken glass receptacles If none of the above recommended actions resolve the problem then consult with the supervisor and or quality assurance officer and e Carry out corrective action to resolve the problem and document see Quality Manual for corrective action procedure e Maintain these non conformance records for audit and review Proficiency Testing The laboratory pursues accreditation and proficiency for Turbidity at both laboratory locations 2230 Main St and the Water Treatment Plant through the Canadian Association of
3. Cleaning 1 Wash all new and dirty Turbidity vials with 50 Hydrochloric acid and rinse with copious amounts of water Follow this procedure when monitoring ultra pure water 2 After glassware has been used rinse the sample cell bottle a minimum of three times using DI water 3 Using a mild detergent and soft brush or wipe remove the oil that was used to minimize scratches interferences 4 Store the sample cell s with DI water inside Also helps to identify the clean cell 5 Store sample cells so that their sides will not scratch each other using foam blocks or with cardboard separators SOP 15 Turbidity v5 1 docx 7 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 8 of 15 Disposable plastic containers are reused for routine wastewater samples After each use rinse the containers with hot water followed by copious amounts of DI water Inspect for cleanliness and if any container appears dirty discard and replace with a new container Batch Creation Set up a batch of samples and the Batch QC using the LIMS Batch Creation process as outlined in the LIMS USER MANUAL Each batch is assigned a unique number which is recorded with each test assigned to the batch Method Quality Control The following QC parameters are incorporated into every run and monitored by compliance to th
4. Laboratory Accreditation Beginning in 2001 at the Analytical Services Laboratory and in 2011 at the Water Treatment Plant Laboratory the laboratory participates in the CALA Proficiency Testing program for Turbidity Turbidity is included in the C 04C Test Group Turbidity in Water Warm up Allow the instrument to warm up prior to Calibration or Sample Measurement Instrument warm up with Ratio on is 30 minutes and 60 minutes with Ratio off Use the same pre aligned sample cell for all sample measurements Since the Turbidimeter is used daily the instrument is normally plugged into a timer which turns the instrument on in the morning and off at the end of the work shift The timer is checked and adjusted if necessary once every two months on the same day as the Equipment Calibration with Primary Formazin Standards is conducted and documented on the same worksheet Oiling Oiling shall be performed at least once on all cells sample amp standards each day in use prior to using them 1 Rinse the clean cell with a portion of sample standard and discard 2 Fill the sample cell to the mark 3 Hold the sample cell by the cap and wipe with scratch free cloth to remove water spots and fingerprints 4 Apply a thin bead of oil from the top to the bottom of the cell and spread uniformly with the oiling cloth 5 Wipe the excess so that the glass appears dry Indexing a single sample cell Indexing is important with low turbidi
5. Test Procedure Oiling Must be performed on all cells in use and each day in use p9 Revision History includes a table for better historical documentation going forward it s much easier to note when a version number might be skipped and how often the revisions occur p 13 Endnotes file and folder locations new section listing the location of all referenced documents p 15 Next Review No Later than October 31 2015 Use the following only if there are no changes required at the next review or there are minor handwritten amendments suitable for continued use i e the SOP does not have to be formally recompiled and distributed Annual Review includes verification ensuring that the laboratory has the most current version of all the referenced methods and manuals and that obsolete documents manuals etc are removed and documented as required Sign the following only if there are no significant changes required at the next review Reviewed By Review Date Next Revision Date Tab 1 Certificates of Analysis Tab 2 Method Validation Tab 3 Quality Control Tables Reagent Logs and Calibrations Tab 4 Quality Control Charts Tab 5 Equipment Maintenance and Operation Logs After completion Control Charts Reagent Logs and Equipment Maintenance logs are placed into the appendices of the master document binder After each calendar year the hard copy charts and logs are turn
6. as in DI water is the water produced by reverse osmosis and ion exchange system At the ASB laboratory this water which meets the laboratory reagent grade water and when further polished is referred to as MilliQ water or WaterPro water at the WTP laboratory Sample History Field or Laboratory Filtration Not applicable Containers Plastic or glass containers are suitable for sample collection Volume Required A minimum of 100 mL of sample is collected Sample Collection All samples are collected by personnel specifically assigned to those duties as described in SOP 17 Sampling SWI 17 05 No Head Space sampling procedure Preservation Analyze samples as soon as possible but if this is not practical preserve by refrigerating at 4 2 C to minimize microbiological decomposition of solids If temperature has an effect on the solubility of the sample then analyze immediately Samples can be left at room temperature when analysis is to be done within 2 hrs Do not refrigerate if sample is to be analyzed within a few hours This can sometimes alter the composition by introducing more precipitated matter Store all standards at room temperature Holding Time Refrigerated samples can be held for 48 hours Sample Pretreatment Gently agitate all samples before examination to ensure a representative measurement Do not alter the pH or other sample conditions Dilute quantitatively very turbid or highly coloured samples befor
7. microscopic organisms cause turbidity in water The turbidity caused by suspended particles is a measure of the clarity of water Since a change in turbidity reflects a change in water quality this is a simple but very important analysis used in water and wastewater monitoring with laboratory or on line instruments A Nephelometer is defined as a turbidity instrument capable of measuring the scattered light at 90 and reported as NTU A Nephelometer consists of a light source a lens aperture and a photoelectric detector at 90 from the transmitted light Very low turbidity exhibits very little change in the direct measurement of transmitted light but isimuch more sensitive at the 90 angle Higher concentrations also cause multiple scattering interference with direct light thus making the 90 a more accurate measurement gSome instruments Hach 2100N also include a forward scatter light detector transmitted light detector and a back scatter light detector If the Ratio On mode is used then the instrument uses a mathematical calculation to ratio the signal from the four detectors Formazin is the only primary standard recognized and approved for calibration of any turbidity instrument ratio or non ratio Formazin can be reproducibly prepared from assayed raw materials and the physical characteristics make it a desirable light scatter calibration standard The Formazin polymer consists of chains of several different lengths which fold into rand
8. then mix again by inverting the vial few times Insert and align in the sample holder Close the cover and wait for a stable reading If the sample is cold condensation on the sample cell caused by the heat of the lamp may occur This is noticeable by gradual increase in the sample turbidity If this cannot be avoided the lower reading is recorded For samples with turbidities greater than 40 NTU dilute the sample using DI water until it is within range Usethe minimum dilution required to bring the sample within range aiming for a mid to high range Turbidity reading The following table is based on diluting the sample to read inthe 20 to 40 NTU range Extrapolate the initial measurement from the x axis up to the corresponding dilution reddish horizontal bars to determine the dilution required Record the dilution the turbidity measurement and calculate and record the turbidity based on the dilution factor Run a sample blank using the same source water used for the dilution Turbidity Dilution Chart 20 12 5 4 Extended Range 020 40 NTU Best Range Dilution ml Sple mL Total 1 1 Em aes 0 40 80 120 160 200 240 280 320 360 400 440 480 520 560 600 640 680 720 760 800 840 880 Turbidity NTU of undiluted sample SOP 15_Turbidity_v5 1 docx 12 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 20
9. 1 docx 11 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 12 of 15 1 Allow the instrument to warm up and set to Ratio On Signal Averaging and Automatic Ranging 2 Prepare the stray light calibration verification CRM and sample cells by Oiling This step may be omitted only if the cells have already been oiled that day 3 Run the stray light Calibration Verification Standard and the CRM and record in the TURBIDITY QC Records If the calibration is within the acceptable established control limits then proceed with the sample 4 For wastewater effluents industrial or hauled wastes examine the sample and remove any floatable solids and decant any grease 5 Select the most appropriate option of filling the sample cell Option A Samples in containers Ensure that the cap is tightly closed and then invert the container several times Immediately open the lid and fill the sample vial cell to the indicated mark DO NOT shake the sample bottles vigorously as this will introduce air bubbles and give false readings Option B Wastewater aliquots sample cups without lids Gently and thoroughly mix the sample by creating a vortex using a Teflon or Glass stir stick then immediately pore and fill the sample vial cell to the indicated mark and cap Dilution Factor multiplier Wipe and
10. 14 Environmental Standards Division Page 13 of 15 When there are no dilutions Turbidity readings NTU are read directly from the instrument Dilutions Turbidity reported Turbidity reading Calculate diluted samples back to their original concentration Sample NTU Turbidity reading NTU X mL final volume Sample volume mL Calculation of Duplicates or Repeats Difference Duplicate sple Initial sple x 100 Initial sple Calculation of Recovery Recoveryaasta Resultgasta Certified Value x 100 where QAstd is a HRM CRM Calibration Verification Standards or Calibration Check Standard as listed on the Certificate of Analysis or as prepared expected concentration Lab coat and safety glasses goggles must be worn in the laboratory at all times Wear gloves when handling corrosive chemicals wastewater industrial wastes and unknown sample matrices Refer to each chemical MSDS for detailed hazards and handling instructions available on the City of Winnipeg s intranet site Wellness page Sewage samples contain pathogenic organisms Wear gloves eliminate contact above the chest while working and thoroughly wash hands with a disinfectant soap after handling Refer to Environmental Standards Division Health and Safety Manual and applicable safe work procedures ifi the SafeWorkProcedures manual Version No Issue Date Author Reviewers 4 2 G Levesque J Jones 5 0 December 18
11. 2013 G Levesque H Demchenko 5 1 October 24 2014 J Jones G Levesque Revision details are documented in these historical versions Version 5 0 Introduction and Scope updated precision and UNCEFtaINLY cece cece eee eee tees eee e eee e eae eeee eee eae p4 Reagent Preparation Logs added expiry date information sssssssssesseeeeen m p6 Method Quality Control run a sample blank if a dilution is performed eese p8 Acceptance Criteria sample blank shall be 0 1 NTU ssssssseeseen mm mm emen p8 Oiling and Sample Measurement perform oiling daily on all cells in use suseeseesees p9 11 Document Control procedure for Certificates of Analysis added ssssssssssrssssrrrrrssrrrrrnnerrrrenee p 14 SOP 15 Turbidity v5 1 docx 13 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 14 of 15 Current Version 5 1 Hyperlinks to external documents removed from the main body and replaced with endnote references Interferences Condensation at ASB lab use instrument connected to air supply p5 Equipment Maintenance document non routine and Bimonthly checks in LIMS Instrument p7 Reagents Reagent Logs download scan the COA for all CRMS cccceceeseeeseeeeeeeeeeeseeaeteseteees p6
12. 4 Tab 2 Method Validation ssessssssssesseseene EEE EERE EEE nnn 14 Tab 3 Quality Control Tables rte e ce tek eee ve cee a xa exa EX ev EYE CERERI 14 Tab 4 Quality Control Charts aed e EX XX ERR KE ERR EFIE RR ERE KR ED a o 14 Tab 5 Equipment Maintenance and Operation LOgS s s s ssssssssrrssrrrsrnrunenrnurnnnnerrnurrnns 14 Document Comt olivis spPERRERRERRRERRXERRRRXEDEARRRRRR RARE ARUREIRRRER RE RRRRRRERIRARRRIRARRRRRAREERIRR PO 14 Refer ell OS Lsoscoceone sone pone OSERERCUREUSUEKEREREKEKEERKEREREKEKREREKFRERE ERR VO VE RUEVEVEVETRVRVOFTE PESE EERVPR 14 Equipment Instruction Manuals ccceceee eee e eee eee eee ene emen eene 14 Reference Texts cccccccecece eee eee e eee sea sea sea sua sua sua REESE sese ssa sea sea sea sea sea sea sea EEE se nnn EES 15 Endnotes file and folder locations esssssssssessssessssenmem mmm 15 SOP 15 Turbidity v5 1 docx Date Printed 30 10 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 3 of 15 Turbidity is a measure of an optical property that causes light in an aqueous sample to be absorbed and scattered by minute particles rather than transmitted The higher the intensity of scattered light the higher the turbidity Suspended and colloidal matter such as clay silt finely divided organic and inorganic matter and plankton and other
13. Q City of Winnipeg Environmental Standards Division ON Winnipeg Analytical Services Branch Standard Operating Procedure Turbidity by Nephelometer LIMS SOP 15 Procedure ID Turbidity Version 5 1 Appendices No 009 ASB 024 WTP Issue Date October 29 2014 Total Pages 15 Approved By Courtney DIdUCKk Analytical Services Branch Head Notice Two printed control copies are issued with one copy located in the Analytical Services Laboratory and the other atthe Water Treatment Plant Laboratory Each copy is authorized by signature of the Analytical Services Branch Head Only the controlled copy documentation is to be used in the laboratory This controlled copy cannot be photocopied or reproduced without authorization Electronic copies are accessible in PDF format from the method folder and the intranet folder N Environmental Standards Analytical Services SOP PDFs Hyperlinks to external documents and navigation within this document are highlighted and underlined in green font These links are functional in the electronic version of this document when the user has permission and the document is viewed within the City of Winnipeg s intranet site from the above mentioned folder All documents pertaining to this SOP are maintained in subfolders of the following Master Folder N Environmental Standards Methods Turbidity SOP 15 Latest revisions are highlighted in blue print All hand written amendments e
14. d label the top of the bottle with the new reading 3 Remove from the sample holder and repeat with the 1 2 NTU 10 20 NTU 100 200 NTU and 200 4000 NTU 4 Use the stray light and a second standard calibration verification each day that the instrument is in use Record the readings in the TURBIDITY QC Records 5 Index Sample cells after every calibration to determine if the cells are still performing optimally Removing Air Bubbles Degassing is recommended to remove air and other entrained gases prior to sample measurement Use method A B or a combination of both methods when the interfering air bubbles are visible A Applying a vacuum Fill the sample cell and apply vacuum with a clean oil free hand operated pump fitted with a rubber stopper A large syringe fitted with a 1 rubber stopper can also be used Allow the sample to sit at atmospheric pressure for a minute before capping and sample measurement B Ultrasonic bath Excess application of ultrasonic waves may alter the particle size Do not exceed the recommended time as predetermined using the method outlined in the equipment manual Record the maximum time for future use Fill the sample cell leave uncapped and immerse to 2 3 in an ultrasonic bath until the visible air particles are removed or the maximum time is reached whichever occurs first For all other samples bring the sample containers to the instrument Sample Measurement SOP 15 Turbidity v5
15. e control results in the Enter Results Enter Batch QC Data function 1 A stray light check A secondary standard check CalVer control chart One independent Formazin standard CRM with every batch One duplicate with every batch Mo o opu JM If any dilution is performed run a sample blank using the same source water used for the dilutions Record all QC data in QC Module of LIMS Verify QG data against established upper and lower control limits If a QC standard is out of control treat as a non conformance If the duplicate has a turbidity over 40 NTU perform the duplicate analysis on a different dilution Since the range is linear this should confirm that the reading is accurate Ex If the sample is diluted 1 2 then do a duplicate with 1 4 Acceptance Criteria Calibration verification shall be within the established upper and lower control limits of three standard deviations 3 90 These values shall be plotted on a control chart and are also entered in the LIMS Duplicate amp replicate recovery shall be within the established upper and lower control limits of three standard deviations 8 6 These values shall also be entered into the LIMS QC Stray light shall be within 0 003 NTU of the recorded value in the LIMS The reference value shall also be clearly marked on the stray light standard Sample blank shall be 0 1 NTU This value shall be entered into the LIMS QC Non Conformance and Corrective
16. e measuring All samples greater than 40 NTU must be diluted with DI water Taking Aliquots 24 Hour composite wastewater effluent samples are initially collected in large plastic containers 16L or 20L which are then transported back to the laboratory Taking aliquots from those containers is not possible therefore a representative portion is poured into 2L beakers to reduce the volume down to 1 to 2L This portion is considered as the original sample For turbidity analysis fill a plastic sample cup about 2 3 full from the 2L beaker following the procedure Sample Aliquots in SOP 17 Sampling Ensure that the cups are uniquely identified Duplicates are also taken from these containers Interferences Air bubbles can create a positive interference Remove air bubbles by degassing vacuum or ultrasonic bath as outlined in the instrument manual Model 2100N Laboratory Turbidimeter SOP 15 Turbidity v5 1 docx 5 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 6 of 15 Scratches finger marks or dirt on the walls of the sample cell may give erroneous readings Use silicone oil and cloth to minimize interferences as outlined in the Test Procedure Oiling Floating grease and oil may require skimming off before measurement Condensation can form on the cell giving erroneous readings if t
17. ed into electronic format as PDF files These are filed in the Turbidity Method QC RECORDS Historical PDF folder and hard copies are destroyed in accordance with the documented policy of the Quality Manual Certificates of Analysis verify that the PDF version is available from the COA folder Scan and file any missing documents then destroy the paper copy as per the Quality Manual policy Equipment Instruction Manuals Hach Model 2100N Turbidimeter Instrument Manual HachModel2100AN pdf SOP 15 Turbidity v5 1 docx 14 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 15 of 15 2100N Laboratory Turbidimeter QuickReference 2100N pdf Manual Change Notice 2100 Series Laboratory Turbidimeters Operation Manual ManualChangeNotice 2100series pdf Reference Texts 2130A Turbidity amp 2130 B Nephelometric Method Standard Methods for the Examination of Water and Wastewater Turbidity Science Technical Information Series Booklet No 11 Michael J Sadar EPA 180 1 Turbidity Nephelometric Endnotes file and folder locations All forms worksheets reagent logs located in N Environmental Standards Methods Turbidity SOP 15 FORMS Control Charts are printed from ChartGenerator xIlsm workboolcin N Environmental Standards MAnalytical Services Charts Standard Methods for the Exami
18. er that may be used when the Hach 2100N is being serviced Follow the Vendor s Instrument Manual for calibration and use and following this SOP for all other sections The Nephelometer located in the WQ laboratory is equipped with an air line When the relative humidity is high and samples are cold condensation can occur on the sample vials and on the optical lens inside the instrument This is noticeable by gradually increasing Turbidity readings and by visual inspection of the vials When this occurs turn the air flow on or bring the samples closer to room temperature Supplies amp Glassware 30 mL sample cell see Indexing a Sample Cell Oiling cloth Pipette s Class A volumetric flask or mixing cylinder 50 mL 47 mm filter flask assembly with filter dome Consumables e Always keep a replacement bulb on hand e Filtration apparatus and glass fibre filter paper e 0 2 um Teflon or glass fibre filter paper Equipment Manuals Equipment Instruction Manuals arewlisted in References page 14 The hard copy of the 2100 N Hach is located in the Water Quality laboratory in the magazine rack near the instrument Equipment Maintenance Logs Document all non routine maintenance equipment problems arising from any error codes and the bi monthly calibrations in the corresponding LIMS instrument logs Inspect the sample cell for large or excessive scratching and discard as required Rinse the glassware with DI water prior to use
19. he sample is too cold Samples should warm up to close to room temperature before analysis If it s still a problem consider using the Nephelometer in the WQ lab which is connected to the air supply When turned on the air circulates through the sample chamber and prevents condensation from happening Light absorbing materials cause a negative interference at high levels while at low concentrations these particles may contribute to turbidity Make note of any known matrices ex solvents The presence of dissolved color causing substances that absorb light may cause a negative interference Instruments that have the four detectors and the Ratio On have the capability of either correcting for slight color interference or optically blanking out the color effect Refer to LIMS Summary Reports List of Certified Reference Materials and List of Qualified Supplier amp Materials for purchasing the requiredychemicals and solutions Also review previous Laboratory Purchase Requisitions e Laboratory deionized water e Silicone oil always use Hach silicone oil which has the same refractive index as the glass sample cells e Primary Certified Formazin Standards for equipment calibration Available in a set of lt 0 10 20 200 1000 amp 4000 NTU e Secondary Formazin GelsStandards and stray light measurement sample each day of use and calibrated against the primary standards e Independent Primary Formazin Standard for CRM mid range
20. ity reading is within 0 01 NTU Any sample cell that exceeds 0 01 in all positions cannot be used for turbidity measurement 4 Continue with the other sample cells while always comparing to the first indexed cell Equipment Calibration with Primary Formazin Standards StablCal Calibration is done every 2 months or as required Remove the wavelength filter required per EPA standard and clean as required using a lint free non scratching cloth Put back in place with the Front label towards the front closest to you 1 Never mix the 0 1 NTU standard For all other standards if they have not been used for some time shake vigorously for 2 3 minutes then let the standards sit undisturbed for 5 minutes to remove air bubbles Otherwise invert 10 times to mix There should be no solids settled on the bottom of the vial Fill a clean sample cell with high quality water cap and oil Place in the sample holder and close the cover Press the CAL key the SO light will go on and the NTU value from the last calibration will be displayed 5 Press ENTER the instrument counts down from 60 to 0 and then makes a measurement This result is stored in the instrument and is used to compensate for the turbidity of the dilution water or blank 6 The meter will advance to the next standard the S1 light is on and the display reads the next expected NTU ex 20 00 Remove the standard from the compartment 7 Mix oil and insert into the ne
21. nation of Water and Wastewater download from on line account http www standardmethods org as PDF in N Environmental Standards Analytical Services Standard Methods Method Validation Data is located in N Environmental Standards Methods Wr rbidity SOP 15 METHOD VALIDATION All Standard Operating Procedure SOP 17 Sampling SOP 51 Glassware SOP 50 LIMS User Manual in N Environmental Standards Analytical Services SOP PDFs 6 Certificates of Analysis are downloaded or scanned and filed in the corresponding folder and named according to its Chemical ID No in N Environmental StandardsNAnalytical Services Certificate Of Analysis CRM Stds Equipment Operation Manuals are available from the following two locations N Environmental Standards MMethodsWNTurbidity SOP 15 MANUALS N EnvironmentaliStandards Analytical Services Instrument amp Software 8 Access MSDS from the Gity of Winnipeg intranet Wellness webpage at http citynet intrahom toc wellness stm Safety Manual located in N Environmental Standards Safety SafetyManual 10 Safe Work Procedures in N Environmental Standards Safety Safe Work Procedures Safe Work Procedures 11 Perform the review as described in the Method Validation Method Review section of the Quality Assurance Manual SOP 16 QAM in N Environmental Standards Methods Quality Manual SOP 16 The official MS Word document of this SOP is maintained in a secure controlled location N Environmen
22. ocx 3 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 4 of 15 Working measurement Range The working range is 0 05 to 40 NTU This is the only true linear range in a Nephelometer Samples greater than 40 NTU are diluted within this working range and calculated Detection Limit The Minimum Detection Limit based on 3 standard deviations of repeated measurements of a low level standard is 0 05 NTU Note Even water molecules will scatter light therefore pure distilled or DI water cannot have a zero turbidity reading and a Turbidity Meter cannot be set to zero Accuracy Bias The bias based on a Certified Reference Material used in every batch as relative bias is 0 995 and is thus not used in any calculated result Precision The precision calculated as two times the Relative Standard Deviation from duplicates included in each batch is 0 024 ASB and 0 060 WTP Uncertainty The uncertainty of the method based on the combined uncertainty of the Duplicates and Certified Reference Material is 0 031 ASB and 0 063 WTP Ucombined Udupi Uem Or RSDcomb RSDuaupi RSDem Fit for use This method is fit for its intended use for the determination of Turbidity in water and wastewater and other aqueous solutions in the applicable range of 0 05 to 10 000 NTU Method Validation By Ge
23. om configurations This results in a wide array of particle sizes and shapes that are found in real samples This randomness yields statistically reproducible scatter on all makes and models of turbidimeters Secondary standards can consist of either Formazin or suspensions of micro spheres of styrene divinylbenzene copolymer Scope This method pertains to the measurement of Turbidity in water and wastewater when measurements are conducted in the laboratory Referenced Method This method is modified from Standard Method for the Examination of Water and Wastewater Approved by Standard Methods Committee 1997 Editorial Revisions 2011 2130A Turbidity amp 2130 B Nephelometric Method The method contains the following modifications i The instrument measures at three angles three ratios which it then averages ii The laboratory purchases all of the Primary and Secondary Standards iii Samples over 40 NTU are diluted in range with laboratory reagent grade water iv Samples are normally not degassed unless the air bubbles are visible v The meter located in the Analytical Services Branch WQ section is attached to an air source to prevent condensation of the Turbidity Cells The latter occurs during summer months only Applicable Instrument Range The applicable range is 0 05 to 10 000 NTU but samples greater than 40 NTU must be diluted The higher range is only used to estimate the dilution required SOP 15 Turbidity v5 1 d
24. on sseeessseeeeese enne n Ra s EE ansa nnne anna nnn nnn 7 Quality Control Pari iscscscses enu exencacseneuexm sencresescr eal Nar oreet 8 Method Quality Control sese fl eese 8 Acceptance Criteria eter ee e petrae noh nre miren en Ra ded hx een ka nere 8 Non Conformance and Corrective Action 5 sssssssssssssssssenesememememe nemen 8 Proficiency Testing uio rie ee all Nee rdiet eve xta eei cestode 9 JE cidqoe nelt pec mU 0 CTUM 9 Warmi Up pee ad uc 9 errore ec CST DIOCESIS 9 Indexing a single sample cell E Sh 2 Mace eee eens nnne 9 Indexing several sample cells JARE aE ANAE EEA ENEE A 10 Equipment Calibration with Primary Formazin Standards StablCal 10 Calibration of SecondarysStandards Gelex StablCal s s ssssssssrsssrrrsrrrrsrrrrurnrenrrrreren 11 Removing Air BUDDRGS SQ Denen ra Ernan ETENE EO EEEE A enne 11 Sample MeasurgmentNS D cec eerta ERE RR EET A Aa 11 Data Analysis amp CaloWatlglis iiieee reor erre renane nnna alo nes un eh nenas EE ar Es RUE EE 13 STi axi tee eT M er Tr TCT CCr TCE TCLS CRTC CETCCURT CEST ORT RCCL PC CrT Terr Ter Cert Terr Teer 13 auciliccos H EMMPEETMT 13 Currerit VERSION 5 T ires coccisexor ta leven cerne one e ea on ein by wi uo a Or a un X UY X RC EX C RED E TRE T 14 APPGNICES f ss 14 Tab 1 Certificates of ANalySiS cc cece eee eee emen eene en 1
25. rry LevesquepQuality Assurance Officer August 5 2011 and last updated on October 29 2014 The Nephelometer or ratio turbidimeter is routinely calibrated against Formazin polymer primary standards Secondary standards which are then standardized against the primary standard are used in the daily use of the instrument The sample s is then measured under the same operating conditions and a direct readout is obtained Special handling and the use of silicone oil on the glass sample cells minimize interferences Air bubbles must also be removed or minimized by one of several techniques Samples greater than 40 NTU are diluted to fall within the O to 40 NTU range the only true linear range of any ratio turbidity meters The higher range is only used to determine or estimate the dilution required Readings can be obtained with Manual or Automatic Range selection and with signal averaging on or off With Signal Averaging On ten readings are taken and the average is displayed Under normal operating conditions Automatic Range Selection with Signal Averaging and Ratio On is used A USEPA filter is also used for all aqueous sample matrices LIMS Test Codes and Definitions Turbidity Turbidity by Nephelometer SOP 15 Turbidity v5 1 docx 4 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 5 of 15 DI
26. tal Standards Quality Assurance SourceDocs Current Word SOP 15_Turbidity_v5 1 docx SOP 15 Turbidity v5 1 docx 15 Date Printed 10 30 2014
27. ty water because it minimizes the background interferences that come from scratches or inconsistency in the actual glass SOP 15 Turbidity v5 1 docx 9 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 10 of 15 Always index the sample cells following the equipment calibration with primary standards as well as any new sample cells before they are put into use 1 Fill a clean sample cell with high quality water and cap 2 Prepare the sample cell by oiling 3 Insert the sample cell in the instrument line up the mark and close the lid Press Enter and record the reading 4 Lift the cover rotate the cell 1 8 turn clockwise close the lid press Enter and record the reading Continue this procedure until the smallest NTU reading is obtained Place a mark on the sample cell marking band adjacent to the index mark of the instrument Point or arrow on the plastic housing 7 Usethis mark to align the sample cell for all measurements Indexing several sample cells 1 Index the first sample cell as above 2 Fill the second sample cell with high quality water Insert and close the lid If the turbidity reading is within 0 01 NTU of the first indexed cell then add a permanent orientation mark to the cell If not rotate 1 8 of a turn and note the reading 3 Continue until the turbid
28. xcept for spelling or grammatical errors must be approved immediately by the Analytical Services Branch Head or Quality Assurance Officer who shall initial and date the amendments The procedure shall be formally revised and reissued as soon as practicable SOP 15_Turbidity_v5 1 docx 1 Date Printed 10 29 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 2 of 15 All forms reagent logs are located in TurbidityForms xlsx Control Charts are printed from ChartGenerator xIsm jr jsr Wegeoncoci m TT 2 Introduction and SCOpe i ocv v ee e Ex EN p rEERDUREERKUEEEREDERER E EEEENU FE YE EEEEE EE E EK SEEEEERKE 3 SCOP GC esa rpm 3 Referenced Method cierre vx cere cere Cv e SEVA SER OEYR EVA VA YER chee EVE VERE cei 3 Summan Of Methodus ssa ad a ERRARE ERE AR UR VERRE VERRE EBENE VIRA ERAN VOY EFE XXXIX Y FREE ERA 4 Sample Requirements n e paesessasncsi uA RE RREREREREPREERKRRRERERRERERRERRPRRRERFRERRRIRERRRIRERER 5 Sample BIStOTV i iciciese iro rkka nkukakka ex EXER AIME tose pas KR NEDUAERERVAEERKREATKEEAWER NEN DE D ARR EECUERE REUS 5 InterferenCces iced sect eive ecu daa vv Ve ve Eo e EYE e a A ia ee e de indiya 5 Chemicals amp Reagernts sisses rr EE EFE ER FERRE ERE EFE NN eee e ree E EP EE EYES 6 Equipment amp Supplies onerare ren ner oe ree nereosnb eee enne nnns 7 Glassware Preparati
29. xt standard 20 NTU into the sample holder align and close the cover SOP 15 Turbidity v5 1 docx 10 Date Printed 10 30 2014 Accredited Test Procedure Method Name SOP 15 Turbidity by Nephelometer v5 1 ASB amp WTP Laboratory Issue Date October 29 2014 Environmental Standards Division Page 11 of 15 8 Press ENTER and continue as in step 4 with the 200 1000 and 4000 NTU standards 9 After the 4000 NTU is completed the instrument returns to the dilution water standard SO light will be on press the CAL key to store the new calibration curve 10 Document the calibration in the Equipment Log and corresponding LIMS Instrument log Label the instrument with the Date of Last Calibration and Date of Next Calibration due date and analyst who performed it 11 Index the sample cell s 12 Proceed to Calibration of Secondary Standards If any problems are encountered or the calibration is not linear an error message will appear Review the instrument manual for diagnosing problems Calibration of Secondary Standards Gelex StablCal 9 Secondary standards are recalibrated following every calibration or as required 1 Verify that the instrument is warmed up and set to Ratio On Signal Averaging and Automatic Ranging Starting with the Stray Light standard oil insert and align in the sample holder Close the cover and wait for a stable reading 2 Record the reading in the Equipment and Secondary Calibration records an
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