Solids (TSS, TVSS, TDS, TS, TVS)
Contents
1. The daily use standard CRM or HRM recovery values shall besplotted on Control Charts and shall be within the established upper and lower control limits Ghese values shall also be entered into the QC table in the LIMS Where the CRM _is supplied with a value and confidence limits then those shall be followed unless otherwisesstated Non Conformance and Corrective Action If the CRM or HRM is outside the control limits for any test then reject the batch about 25 samples per CRM and re analyze If the CRM is overthe limits re dry re weigh and recalculate the results If the control limits are still exceeded then reject the batch and re analyze If any of calibration verification duplicateyrecovery replicate recovery spike recovery or control standard value is outside ot Ehe control limits then e Document the non conformance on the Control Chart e Carry out corrective action to resolve the problem See Quality Manual for corrective action procedure Document the correctivesaction and maintain the records for audit and review Proficiency Testing The Analytical Services Branch is accredited to ISO 17025 20005 General Requirements for the Competence of Testing and Calibration Laboratories and actively pursues proficiency for Solids at both laboratory locations Participation in the CALA Proficiency Testing for Solids began in 2000 at 2230 Main St and in 2011 at the Water Treatment Plant TSS TDS and T2. e Samples are not weighed to constant weight Instead a much longer drying time is used for TDS amp TS and a reweighed sample is included in each batch If the reweigh is outside the established quality control limits then the batch is dried for an additional 30 minutes and desiccated again Sludge and samples with high solids or grease content are dried overnight gt 12 hrs e For Total Dissolved Solids some samples such as Industrial wastes and leachates cannot be filtered due to their extremely high content of particulate matter that immediately clog the filter For these samplesyonly the sample is centrifuged at 4000 rpm for 20 minutes and the centrate is used for TDS Scope TSS TVSS TDS TS TVS Applicable Range for 3 to 20 000 3ta20 000 3to20 000 3to20 000 0 03 to 100 routine water wastewater mg L mg L mg L mg L and sludge 0 03 to 40 Minimum Detectable Limits 3 mg b 3 mg L 3 mg L 3 mg L 3 mg L Accuracy Bias relative 0 017 0 017 0 002 0 003 0 003 Precision 0 039 0 043 0 025 0 055 0 01 Expanded Uncertainty U 0 084 0 087 0 065 0 062 0 029 percentage range applies to sludge and biosolids analysis Fit For Use This method is fit for its intended use for the determination of o Total Suspended Solids Total Volatile Suspended Solids and Total Dissolved Solids in the range of 3 mg L to 20 000 mg L in water and wastewater o Total Volatile Solids in the range of 0 03 to 100 in sludge and biosolids o
3. 7 Weigh the vessel on the analytical balance and record as Vessel amp Sample Wt for liquid sample or W3 for Solids Calculate amp Enter results in LIMS SOP 12_Solids_v5 1 docx 15 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 16 of 21 Volatile Solids following the TS 1 Transfer the Crucible from the completed Total Solids analysis into the Muffle furnace at 550 C for 1 hour 2 Remove from the furnace and set on the tile or cooling rack until most of the heat has dissipated then place in desiccator for at least 30 minutes 3 Weigh the crucible on the balance and enter the weight as T S Final Wt in DailySolids xls worksheet or M 4 in the sludge analysis worksheets manual calculation Calculate amp enter results in LIMS Volatile Solids direct method for liquids 1 Record crucible ID in the DailySolid xlseworksheet Use a large crucible that can hold aminimum of 50 mL 2 Transfer and Recordsthe volume of sample used 2 3 full 3 Dry sample in oven at 404 1 C until dry at least 1 hour For samples containing light particulate matter either reduce the blower fan speed of the oven to 50 if possible or cover the sample with an aluminum weigh dish 4 Remove samplesfrom the ovens and allow cooling at room temperature for 5 minutes Transport to the
4. Q City of Winnipeg ON Environmental Standards Division Winnipeg Analytical Services Branch Standard Operating Procedure Solids Total Solids TS Total Suspended Solids TSS Total Volatile Suspended Solids TVSS Total Volatile Solids TVS Total Dissolved Solids TDS Moisture H20 LIMS SOP 12 Procedure ID Solids Version fN Appendices No 008 ASB Appendices No 023 WTP Issue Date October 20 2014 Total Pages 21 Authorized By Courtney Diduck Analytical Services Branch Head Notice Two printed control copies are issued with one copy located in the Analytical Services Branch Laboratory and the otherat the 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 within this document are highlighted and underlined in green font These 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
5. Instruction Manual Tab 5 Method Validation Tab 6 Daily Balance Calibration Checks Supporting Test Methods SOP 51 Glassware Washing SOP 52 Mass and Volume Calibration SOP 50 LIMS User Manual SOP 49 Temperature SOP 12_Solids_v5 1 docx 20 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 21 of 21 Equipment Instruction Manuals Electronic Copies PDF documents Ovens Operations Manuals and Parts List Series 1249 Thermolyne Oven Furnace Temperature Adjustment Procedure Fisher Isotemp Ovens Operating Manual APT line FED E2 Binder Oven Balances MettlerAE200 pdf OhausDiscoveryBalance pdf Sartorius A200S_Manual pdf Water Treatment Plant Hard Copies Balance Manuals located in balance room at 2230 Main Street magazine rack A hard copy of the Binder FED E2 Oven11 is clipped onto the ovens Computer Software Documentation WinWedge Help File on the Balance Computer Available through the LIMS Methods e DailySolids xls Spreadsheet Instruction Manual copy in method binder e PipetteVer xls Instruction Manual Excel program Endnotes file and folder locations Standard Methods for the Examinationsof Water and Waste Water 2504A 2540B 2540C 2540D 2540E 2540G Approved 1997 Editorial Revisions 2011 N Environmental Standards Analytical Services Sta
6. SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 19 of 21 Total Dissolved Solids mg L Total Solids mg L Total Suspended Solids mg L Moisture 100 Total Solids All samples recorded in the DailySolids xls spreadsheet are automatically calculated using the Get Formula function The Quality Control is also calculated using the QC Calculator function Lab coat and safety glasses goggles must be worn in the laboratory at all times Sewage samples contain pathogenic organisms Eliminate contact above the chest i e protect all exposed skin facing the material Read all MSDS caution labels Refer to each chemical MSDS for detailed hazards available on the ity of Winnipeg s intranet site Wellness page Refer to Environmental Standards Division Health and Safety Manualf and applicable Safe Work Procedures in the Safe Work Procedures Manual See Work Safe Procedure Manual for the following OVEN USE CHEMICAL PREPARATION AND HANDLING ACID WASHING Previous Revisions are maintained in the obsolete version 4 3 Version 5 0 November 1 2013 Reviewers H Demchenko G Levesque Scope Range MDL Bias Precision and Uncertainty recalculated cccceeeeeeeeeeeeeaeeas p 3 Fit for Use Statement Rewritten for Clarification ccecece cece eee eens eee e eee ee eee eeeteaeenennes p 3 Sample Requirements updated Sampling Zl rete
7. Tab 2 Reagent Preparation Logs amp Certificates EN 20 TiAl E WORKS EE 20 Tab 4 DailySolids xls Spreadsheets Instruction Manual EN 20 Tab 5 Method Validation eseu 20 Tab 6 Daily Balance Calibration Checke EN 20 Se 20 Supporting Test Methode vs 9 KN Sk ES REENEN KEEN ER vend ER NKER KENNEN EEN EN EES KE KEE EECH caved REENEN EEN ENK dN NEE ECKER 20 Equipment Instruction Manuals cccccceete eter ener nee een n ene nee nee nna ATEAN ene eee nes 21 Computer Software Documentation 21 Endnotes file and folder locations ccceeceseceeeeeneeeeeeeneeeeeeaaeeeeeeaaeeeeeeaaeeeeeeaeeeeeeaeeeeesaeeeeeenaeeeeeeaaes 21 SOP 12_Solids_v5 1 docx 2 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 3 of 21 The measurement of solids content of water and wastewater is important for regulatory purposes and environmental protection The solids content in the different wastewater streams is a measure of the wastewater treatment plant efficiency and solids loading The solids content is also used to determine the wastewater surcharge for industrial and septic waste generators Referenced Method This method is modified from Standard Methods for the Examination of Water and Wastewater 2540 Solids approved by Standard Methods Committee 1997 Editorial Revisions 2011 with the following modifications
8. desiccator remove any covers used and then transfer to ajdesiccator to achieve constant weight at least of 30 min 5 Weigh the vessel on the analytical balance and record as Vessel amp Sample dry Wt or W3 6 Transfer the Crucible into the Muffle furnace at 550 C for 1 hour 7 Remove from the furnace and set on the tile or cooling rack until most of the heat has dissipated then place in desiccator for at least 30 minutes 8 Weigh the crucible on the balance amp enter the weight as TVS Final Wt in DailySolids xls worksheet or W 4 in the sludge analysis worksheets manual calculation SOP 12_Solids_v5 1 docx 16 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 17 of 21 Total Dissolved Solids Direct method NO TSS from TSS method Collected filtrate from the Total Dissolved Solids Total Suspended Solids Total Suspended Solids Total Solids By Calculation method Water raw water basins IW etc 1 Record Crucible or aluminum pan ID number in the DailySolid xls spreadsheet Use a large crucible that can contain a minimum of 50 mL of sample 2 Weigh a crucible pan on the analytical balance and record the vessel weight in the spreadsheet 3 Place a 100 mL beaker or plastic cup in the filtration dorne apparatus Place a filter funnel containing 47 mrmeglass
9. liter volumetric flask 3 Open the bottle carefully and transfer the contents into the volumetric flask with the use of a funnel 4 Ensure that the entire standard is added to the flask by carefully rinsing the bottle and the cap three or four times with deionised water Dilute up to 1000 ml mark with deionised water and mix Transfer standard solution into a clean and dry polyethylene bottle Label with the identification consensus value and expiry date of six months and record in LIMS Label the Solution Make sure to mix for at least 30 seconds before sampling Run this standard with the first aliquot of every new HRM and Use for parameters not covered by the HRM TDS TVSS Refer to LIMS Instrument Module and Equipment Logs Instruments e repeater Pipettes with wide bore tips e analytical balance 0 0001g capacity e analytical balance 0 01g capacity for sludge analysis e oven set at 104 C 1 C e oven set at 180 C 2 C e muffle Oven set at 550 C 450 C Ensure that all volumetric dispensers auto pipettes are verified each day in use Other Equipment amp Supplies e filter dome apparatus e desiccators e gooches Bitumen Crucibles Coors 44 mm top diameter 33 mm bottom diameter 24 mm height e crucibles H F Coors large e crucible Tongs normal and extra long e manifolds stainless steel 3 place vacuum filtration manifolds e metal trays these trays were custom made so that the whole tray is place
10. 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 9 of 21 Gooche Filter Preparation Gooche Preparation Aluminum Dish Filter Preparation 1 Place gooche in the dishwashing basket and wash according to 1 4 Place 47 mm glass fiber filter Glassware Washing Program 1 2 Remove gooche from the dishwasher 5 Filter 100 mL of de ionized water 3 Place and center a new 32 mm 9344H through each gooche and continue glass fiber filter paper in the gooche suction until all traces of water are with the wrinkled side up patterned gone side down 4 Place each gooche on the vacuum 5b Place 47 mm 9344H glass fiber filtration manifold filter paper into a labeled aluminum dish paper wrinkled side up into the filtration apparatus 5 Filter 100 mL of DI water through each gooche and continue suction until all traces of water are gone 6 If the Gooche will be used for TVSS thisistep can be skipped but to prevent breakage please ensure that the Gooches are dry before Step 7 7 Dry in oven at 104 1 C at least bhour 8 Remove from oven and place in muffle oven 550 C for 1 hour 9 Remove from muffle oven and allow the heat to dissipate 10 Place in desiceator until ready to used fat least 30 minutes Crucible preparation 1 Empty and wipe the inside of the crucible with a paper towe
11. Folder N Environmental Standards Methods Solids SOP 12 Latest revisions are highlighted in blue print All hand written amendments except 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 12_Solids_v5 1 docx Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 2 of 21 All forms reagent logs are located in N Environmental Standards Methods Solids SOP 12 FORMS SolidsForms xlsx Control Charts N Environmental Standards Analytical Services Charts ChartGenerator xls REINER e Ree E EE 2 INtHOAUCH OMAN SCONS sired ean n E E A EE E E AR EE R TE 3 SUMOV O MoO EE 4 Sample Requirements EE 4 CMS MANGAS Ge ROA SIMS erraina innra Aa EEA AAAA ae ne ees 5 Reagent Preparation LOGS w sccsiseccsindessatendesaasasieeancievdiis RECKEN SE NNN ENK SKSEAENN EENS RS EEN KEN KEEN dE N SN 5 Expiry Dates cascissacavesacnse se KERSCHEN KOR ENN REH EENS EN EN KEE ENNRAN dunner KEEN NENNEN EE NEE SE ENEE NEEN 5 Diatomaceous Earth Pre preparation for HM 5 TSS HRM 100 mg L amp 1 000 FAG EEN WEE 6 TS TDS HRM 700 mg Total Solids or Total Dissolved Solids L EE 6 Certified Reference Material
12. Total Solids in the range of 3 mg L to 20 000 mg L in water and wastewater and the range of 0 03 to 40 in sludge and biosolids Method Validation By G Levesque QA Officer Date October 23 2009 Last validation update by G Levesque QA Officer Date October 31 2013 SOP 12_Solids_v5 1 docx 3 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 4 of 21 Total suspended solids are determined by filtering a well mixed measured volume of sample through a weighed standard glass fibre filter in a gooche crucible The residue retained on the filter is dried at 104 C 1 to a constant weight The increase in weight of the filter and gooche represents the total suspended solids The filtrate from the total suspended solids can be used to determine the Total Dissolved Solids Volatile suspended solids are determined by igniting the residue from the total suspended solids analysis in a muffle oven at 550 C Total solids are determined by adding a known volume of a well mixed sample into a weighed crucible and after heating to dryness is dried to a constant weight Moisture is the loss of weight due to evaporation when dried Volatile Solids is the weight loss after ignition of the total solids residue at 550 C When total solids and total suspended solids are determined on thessame sample total dissolv
13. VSS are included in the C 04A Test Group Solids TVSS or TVS are not analyzed at the Water Treatment Plant because the test is not required The laboratory also participates in the Phenova Proficiency Testing program two to four times per year for TS and TVS at 2230 Main St and for TS at the Water Treatment Plant Laboratory Additional parameters are done if included and part of the sample or group SOP 12_Solids_v5 1 docx 11 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 12 of 21 Taking Aliquots Ssub samples For larger volumes place the sample up to 1 litre into a large beaker so there is sufficient room for mixing Using a small ladle stir the contents until a vortex is obtained Take several small ladle full and transfer into a graduate cylinder Always use the smallest graduate cylinder that can hold the total volume Use CLASS A TC to contain glassware e 1 10 mL use an auto pipette e 10 20 mL use a 10 mL auto pipette two times e 20 25 mL use a 25 mL graduate cylinder e 25 50 use a 50 mL graduate cylinder e 50 100 use a 100 mL graduate cylinder e 100 500 use a 250 mL graduate cylinder twice if needed For smaller volumes create a vortex by manually stirring the sample or by using a magnetic stirring bar and stirrer Using a wide bore pipette tip take the aliquot midway i
14. ch Method Date October 20 2014 Environmental Standards Division Page 20 of 21 Reviewed By Review Date After each calendar year the hard copy charts and logs are turned into electronic format as a single PDF file These are filed in the Methods Solids QC RECORDS Historical PDF folder and hard copies are destroyed in accordance with the documented policy in the Quality Manual All workbooks with manual calculations are catalogued filed and maintained for a period of 7 years Mark the destruction date as the workbook year 8 A copy of all electronic worksheets created by DailySolids xlsx and imported into the LIMS is maintained in the generic analyst wwdanalyst folder G Solids Certificates of Analysis are also converted in PDF formats and filed in the Certificate of Analysis folder and simply named according to the LIMS Chemical ID Tab 1 Control Charts House Reference Standard Certified Reference Material Tab 2 Reagent Preparation Logs amp Certificates Certificates of Analysis for CRM originals scanned amp filed in Certificates of Analysis folder Reagent Log TSS HRM1000 Reagent Log TSS HRM100 Reagent Log TS QC700 Tab 3 Worksheets Word Document templates for Manual Data Calculations e NE Dewatered Sludge Worksheet WkshtDewateredSludge doc e NE amp SE Raw Sludge Worksheet WkshtNESERawSludge doc e WE Fermentor Sludge Worksheet WkshtFermentorSludge doc Tab 4 DailySolids xls Spreadsheets
15. d inside of the oven s and is made to fit in the desiccators as well This reduces the time required to transfer the items NOTE these trays CAN NOT go inside the 550 C Muffle Oven Consumables e Whatman 934AH glass microfiber filter or equivalent 32 mm diameter with 1 5 um pore size 47 mm diameter with 1 5 um pore size SOP 12_Solids_v5 1 docx 7 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 8 of 21 e Whatman 934AH glass microfiber filters Pre washed amp dried filters 32 mm diameter with 1 5 um pore size Delta Scientific Part No F92432VOL Manufactured by Environmental Express NO SUBSTITUTIONS e Plastic Cups 100 mL e Disposable Aluminum weighing dish 50 amp 150 mL Equipment Maintenance Document equipment maintenance in LIMS equipment log Refer to the Equipment Instruction Manuals listed in the References section page 21 Bar coded Pre weighed Filters A bar coded pre washed amp pre weighed filters manufactured by Environmental Express is an approved filter for Total Suspended Solids The filters are available in the 47 mm size and are ready to use as is The bar code contains an identification number and the weight of the filter Both are also printed in readable font onto a labeled aluminum pan Opened packages must be kept in the desiccators until ready to use T
16. ded in the sample and dispersed by vigorous stirring 5 times to create a vortex before withdrawing a sub sample for filtration Floating debris excluding oil amp grease is excluded Allow samples to warm to room temperature before analysis Containers Samples should be collected in a plastic or glass bottle and transported to the laboratory as soon as possible for analysis Volume Required Excessive residue on the filter can produce a water trapping crust which can result in sample loss or incomplete drying The sample size should be limited to produce a residue of less than 200 mg Samples containing visible suspended solids require less volume for analysis For water samples containing little or no visible suspended solids a greater sample volume may be required for analysis Collect a minimum of 500 mb forturbid samples and 1 litre for water samples Interferences Samples with high dissolved solids may cause positive interferences These effects can be minimized with adequate washing to remove dissolved solids which may get trapped in the filter pores Filter clogging from excessive solids captured in the filter may prolong filtration time and produce high results To overcome this us amp a smaller sample volume for filtration or use a larger size filter Reagent Preparation Logs Document the preparation of all reagents calibration stock solutions reference material stock solutions and working standards on the rea
17. der Centrate Mixed Liquor amp Return or Waste Activated S 5 Pour a volume that will yield 25 to 5 ilransferS volume of well mixed 200 mg of dried residue If residue is Centrate mixed liquor or return lt 20 mg increase volume of sample activated sludge using a wide bore auto pipette 6 Rinse cylinder twice with de ionized water and add rinse to sample Continue suction until filter appears dry If enough sample was used ther should be a visible residue covering the whole filter If filtration takes more than 40 minutes repeat using smaller volume 7 Record the Sample volume in the DailySolid xls workbook or logbook 8 Transfer gooche aluminum dish with sample to drying oven at 104 C 1 C Dry for atleast one hour For samples with light particulate matter either reduce the blower fan speed of the oven to 50 or cover the sample with an aluminum pan 9 Remove from oven and cool at room temperature for about 5 minutes Transport to the desiccator remove any covers used then place in desiccator for at least 30 minutes to achieve constant weight Continued on next page SOP 12_Solids_v5 1 docx 13 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 14 of 21 Bar coded filters A 10 Weigh the gooche aluminum 10 Zero the balance then use dish with sample and record the t
18. eCheck Gold ne uiiman re iah eset eeeeeeeseeeeeeanenenaes 6 Equipment amp Supplies sisi dived onsen da bada anedin T SE A DEE 7 Instruments e EE eg ee H Bar coded Pre weighed Filteren 8 Glassware Preparation 228 EE nee n Ee 8 Gooche Preparation for Prewashed Filters Part No F9O2432VOL 0 ceecceceeeceeeeeeeeeeeceeeeeseeeesseeenenees 8 Gooche Filter Preparation ENEE 9 Crucible preparation EEN WE 9 Quality Control Plan ticiis tcciniictienst teeciinece e EES SEET EEN 10 Daily Balance Chek EE E OI Wit EE 10 Batch Creaton Aen MR O 10 Method Quality Control ET ff EE 10 Acceptance Criteria ET w WEN H 11 Non Conformance and CorrectivevACtion 2y ceccccccccceceeeeececcaececeeeeeeeceaeaeceeeeeeesecacaeeeeeeesesennineeeeeeess 11 Proficiency NOStiNG esorare din WEE 11 Test Vielen TIET EE 12 Taking Aliquots eub samplesg A RENE 12 Solids Oe ET TEE 12 Total Suspended Soks ON ET 13 Total Volatile Suspended Solids cece ee eeceeeaeeeeeeeeeeceaeaeceeeeeeesecacaeeeeeeeseseceaaeeeeeeeeeeeees 14 Volatile Solids following the Ti 16 Volatile Solids direct method for Ioudes 16 Total Dissolved Zuel leegen eege deeg edd a ide kd stdin Add ee Eed Ad Ae 17 Data Analysis amp CalCulations icicieicccictoisinisinicinieemeiisinieanisini cars EUR EE EE EIERE seen ries on 18 Dal E 19 FRGVISION PUSIO EE 19 Document Lut e EE 20 Appendice E 20 Tab 1 Control Chas esst age ge ENe NEES EEN AER eeh ENa EES WEE NEESS EES EE EEE EE Ne 20
19. ed solids can be determined by calculation LIMS Test Codes TSSwv Total Suspended Solids weight per volume mg L TVSSwv Total Volatile Suspended Solids weight per volume mg L TVSS Total Volatile Suspended Solids TSwv Total Solids weight per volume mg b TS Total Solids TVS Total Volatile Solids TDSwv Total Dissolved Solids weight per volume mg L Moisture Moisture the amount of water in the sample calculated from Total Solids Sample History Some samples are collected by internal clients and submitted delivered directly to the laboratory Routine samples are collected by laboratory personnel assigned to the task following SOP 17 Sampling Field or Laboratory Filtration Not required Preservation If the test is not performed within 2 hours of sample reception at the laboratory the sample must be stored at 4 C 2 C Holding Time Analysis is normally performed within 24 hours of sample collection Refrigerated samples can be held for no longer than seven 7 days Sample Pre treatment SOP 12_Solids_v5 1 docx 4 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 5 of 21 Large non homogenous particles should be excluded from the test aliquot if it is determined that their inclusion is not desired in the final results Floating oil and grease if present should be inclu
20. fiber filter paper onto the dome and position it to collect the filtrate directly into the beaker 4 Filter approximately 10 to 20 mL of DI water through the filter followed by approximately 10 to 20 mL of sample Break the suction and open the dome Remove the beaker or plastic cup and discard the filtrate 5 Place a clean dry 100 ML ordarger plastic cup in the filtration dome apparatus and filter upto 100 mL of sample through the filter Break thessuctian and open the dome 6 Transfer SO fo 10 mt of filtrate using a graduate cylinder into the weighedyCrucible Record the volume of filtrate used 7 Gransfer the crucible with sample into a drying oven at 180 2 C until dry and for 1 hour more usually overnight For samples containing light particulate matter either reduce the blower fan speec of the oven to 50 if possible or cover the sample with an aluminum weigh dish 8 Remove from oven and cool at room temperature for about 15 min 9 Place in desiccator for at least 30 minutes 10 Weigh crucible with sample on the analytical balance and record the weight as weight of vessel amp dry sample in the DailySolids xls a Enter results in LIMS SOP 12_Solids_v5 1 docx 17 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 18 of 21 Calculations are automatically done when u
21. gent preparation log sheets behind Tab 3 Label reagents with Material Name Date Prepared and Reagent Prep Log Reference Number or LIMS ID All Reagent preparation forms are available in SolidsForms xisxff All Certified Reference Materials are entered into the LIMS Chemicals and Standards Module and a copy of in the COA is scanned downloaded into the COA folder De ionized R O Water is used when making any reagent unless otherwise stated 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 Diatomaceous Earth Pre preparation for HRM The diatomaceous earth is prepared in the following manner to remove the finest particles which may not get trapped in the glass filter paper SOP 12_Solids_v5 1 docx 5 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 6 of 21 1 Prepare the Diatomaceous Earth by placing approximately 50 grams into a 2 liter beaker 2 Add 2 litres of deionised water stirring vig
22. he 1 Insert the Sample Label in the DailySolid xls worksheet Use a large worksheet workbook crucible that can hold at least 50 mL 2 Weigh the vessel on the analytical balance Record as W1 solid sample or Vessel Wt liquid sample solids 3 Centrate Water and Wastewater Q 3 Cakeusing a spatula transfer well mixed aliquot into a scoop a representative graduated cylinder sample liquids 3 Polymer mix the sample by 3 Sludge mix the sample inverting the bottle 5 times and by inverting the bottle 5 pour an aliquot to fill the times and pour sample into aluminum boat 2 3 full the Chugible until 2 3 full 4 Record the volume of the sample in the DailySolid xls spreadsheet 4 Record the weight of the Sample amp Vessel as W2in the worksheet 5 Dry sample in oven at 104 5 Dry crucibles with sample in 1 Cuntil dry atleast 1 hour For oven at 104 1 C overnight For samples containing light particulate samples containing light particulate matter either reduce the Blower matter either reduce the blower fan speed of the oven to 50 Nuf fan speed of the oven to 50 if possible or cover the sampleWwith possible or cover the sample with an aluminum weigh dish an aluminum weigh dish 6 Remove sample from the ovens and allow to cool atroom temperature for 5 10 minutes Transport to the desiccator remove any covers then place in the desiccator to achieve constant weight at least 30 min
23. hese filters are currently used at the Water Treatment Plant Laboratory Use CLASS A glassware for all volumetric measurements e Graduated cylinders various sizes Class A to contain e Beakers various sizes Wash all glassware as described in SOP 51 Glasswarelf using the Heinicke dishwasher Programi or manually with acid washifg and or soap amp water Gooche Preparation for Prewashed Filters Part No F92432VOL A pre washed and dried glass fibre filter paper purchased from Delta Scientific may be used for the Total Suspended Solids test and Volatile Suspended Solids The filter can be placed inside a prepared gooche in advance or immediately prior to use and weighing The gooche only requires washing and drying 1 Place gooche in the dishwashing basket and wash according to Glassware Washing Program 1 which uses a hot cycle and Deionized water in the rinse cycles 2 Remove goochesfrom the dishwasher 3 Inspect each gooche for cleanliness and residue If any residue is discovered remove the gooche for additional acid washing as described in SOP 51 Glassware washing Usually 50 HCl 4 If the gooches are not dry then place in 104 C oven for about 15 20 minutes Remove and cool down 5 Place a F92432VOL filter inside the gooche with the shinier flatter side down The gooche requires no further action and can be placed in the desiccator for use SOP 12_ Solids _v5 1 docx 8 Date Printed 10 22
24. ksheet tab Balance Cal Log is in SolidsForms xls Auto pipette verifications are done daily and recorded in LIMS The Internal Calibration function on Balance3 is performed at least once per week and recorded in the LIMS Batch Creation All sludge s amp cakes are weighed to two decimal places using a top loading balance and documented in the corresponding daily workbooks All workbooks are bound and created by ASB staff using the approved templates and cover pages listed in Appendices Tab 3 Worksheets page 20 Unless otherwise indicated all charts are available from the following spreadsheet ChartGenerator xlsx Method Quality Control Include and run the blank and CRM oreHRM or combination of at the beginning of the batch and after every 25 to 30 samples If a batch contains samples with expected results in the low and medium high range consider batching similar samples and using two different levels of HRM CRM e Filter 200mL of deionised water into a gooche and use it as a Blank with every batch of samples run e Analyze 25 to 50mh of the TSS HRM standard with every batch of TSS e Analyze 25 to 50m1 of CRM for TSS with every new bottle of HRM e Run one TDS HRM or CRM with every batch of TDS e Run one TS HRM or CRM with every batch of Total Solids e Analyze one replicate or duplicate sample for all test parameters in the batch TSS TVSS TS TVS and TDS with every batch of plant sam
25. l Acid wash with 50 HCI according to the Manual Acid Washing Procedure in SOP 51 Glassware Washing and observing all of the safety described in the Safe Work Procedures Manual 2 Wash crucible manually with soap water and brush until all debris has been cleaned 3 Rinse with tap water followed by de ionized water 4 Dry crucible in oven at 104 C 1 C for at least 1 hour 5 Ignite the clean crucibles in muffle oven for 1 hour at 550 C This step is skipped at the Water Treatment Plant lab and with glass beakers because no TVSS tests are conducted 6 Remove from muffle oven and place onto a heat resistant pad or tile and allow the heat to dissipate then place in desiccator until ready to use SOP 12_Solids_v5 1 docx 9 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 10 of 21 Daily Balance Check Daily mass balance checks are done and recorded in LIMS The balance should be checked by simulating the TSS test as follows verify with a mid range weight 20 g tare the balance with the weight and verify again by adding a low range weight 500 mg or less to the balance Remove the weights re zero tare and verify with a high range similar to a crucible with sample The daily balance check for the top loading balance is initially documented on hardcopy and entered in the LIMS The wor
26. ndard Methods Method Validation Data is in N Environmental Standards Methods Solids MethodValidation i SOP 17 Sampling and Supporting Work Instructions SWI 17 in N Environmental Standards Methods Sampling SOP 17 SWI 17 V SolidsForms xlsx fa N Environmental Standards Methods Solids SOP 12 FORMS Certificates of Analysis COA are in N Environmental Standards Analytical Services Certificate Of Analysis CRM Stds i Equipment Manuals where available have been created and copied into the following folders N Environmental Standards Analytical Services Instrument amp Software Ovens amp Furnaces N Environmental Standards Analytical Services Instrument amp Software Manuals Balances vi SOP 51 Glassware in N Environmental Standards Analytical Services SOP PDFs vii Chart Generator in N Environmental Standards Analytical Services Charts x http citynet intrahom toc wellness stm SafetyManual word document in N Environmental Standards Safety SafetyManual Safe Work Procedures individual PDF located in N Environmental Standards Safety Safe Work Procedures Safe Work Procedures pdf SOP 12_Solids_v5 1 docx 21 Date Printed 10 22 2014
27. nto the sample depth and halfway between the wall of the beaker andymiddle of the vortex Transfer directly to the filter media Solids Methods Goache Crucible or Beaker Preparation Preparation Total Suspended Direct method Solids Total Solids Direct Moisture method all Total Dissolved Solids Total Volatile Total Volatile Suspended Solids Solids SOP 12_Solids_v5 1 docx 12 Date Printed 10 22 2014 Accredited Test Method Analytical Services Branch Environmental Standards Division Method Name SOP 12 Solids v5 1 Method Date October 20 2014 Page 13 of 21 Total Suspended Solids Bar coded Filters 1 Import Batch into the DailySolid xls worksheet 1 Obtain a new bar codedfilter e Obtain clean gooche aluminum dish from desiccator from desiccator record the ID e Record the Vessel ID in the DailySolid xls worksheet numberin the logbook 2 Weigh gooche aluminum dish on the analytical balance A e Record the weight of vessel with filter as Vessel Wt 2 Record the weight from the pan label as Filter Wt Aluminum Dish 3 Place gooche on manifold and turn on 3 Transfer filter from the aluminum suction Squirt enough DI water onto the filter ae ee ee ee to wet completely and to stick to the Gooche apparatus Turn oq suction 4 Mix the sample by inverting sample bottle 5 times or stirring until a vortex is created Transfer an aliquot into the Class A graduated Cylin
28. orously for 5 minutes Allow settling for 30 minutes 4 Decant all of the liquid Transfer the solid into a smaller beaker and dry overnight at 104 1 C 5 Remove from oven cool for 15 20 minutes at room temperature then transfer into desiccators until room temperature is reached Transfer to a clean plastic wide mouth bottle and label Store in the desiccator Diatomaceous Earth does not expire w 6 Pre weigh several standards ahead of time into separate 25 mL vials Label cap and store in a desiccator TSS HRM 100 mg L amp 1 000 mg L Enter the standard in the Chemical amp Standard module of the LIMS as a Reference Material in order to use it in the QC Module Appears in drop down list Larger quantities can be prepared by multiplying the weight of the solid in the same volume of water 1 Accurately weigh 0 204 grams into a clean oven dri d glass vial with screw cap Record the weight 2 Put 1 5 L of deionised water into a 2 liter volumetrie flask 3 Open the bottle carefully and transfer the contents into the volumetric flask using a funnel 4 Ensure that the entire standard is added to the flask by carefully rinsing the bottle and the cap three to four times with deionised water Add wash into the volumetric flask 5 Dilute up to 2000 ml mark with deionised water and mix thoroughly 6 Mix thoroughly again before transferring into a 2 L plastic container and label with expiry date of 6 months To
29. ples Preferably separate large batches into two one with all the volumetric measurement weight volume and one with the gravimetric measurement only weigh weight TS TVS When two separate samples are collected at the source then these shall be documented as duplicates This is feasible with any grab sample e Reweigh another sample to confirm the completeness of the drying and desiccating and balance stability Dry the sample for an additional 30 minutes and desiccate for another 30 minutes then reweigh e Record the values for the QC samples in the LIMS QC database e Compare the results with the control limits SOP 12_Solids_v5 1 docx 10 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 11 of 21 e If any quality standard or blank exceeds the upper or lower control limits repeat the analysis of the corresponding quality standard or blank e If the value exceeds the upper or lower control limits a second time generate a non conformance report and carry out corrective actions This may include cleaning of glassware preparation of new standards and or repeat analysis of the batch Acceptance Criteria o EAr Ke Deg B lee VATNS Sample Blank 3 mg L 3 mg L 3 mg L HRM CRM 11 9 3 11 11 11 Duplicate 11 10 7 7 4 Repeat reweigh 6 6 7
30. prepare a 1 000 mg L weight ten times 10 x the amount of Diatomaceous Earth in the same amount of de ionized water TS TDS HRM 700mg Total Solids or Total Dissolved Solids L 1 Dissolve 0 700 gs 0 002 g NaCl in deionised water in a clean 1 L volumetric flask containing 500 ml of deionised water Shake well until all NaCl is dissolved Make up to 1 L and shake This standard is prepared quarterly ee ee Label with identification concentration analyst preparation and expiry date of six months and record in Reagent Log QC700 House Reference Material Certified Reference Material peCheck Solids peCheck Solids 2 verify and obtain the Consensus value and the Confidence Interval stated on the Certificate of Analysis This standard should be added to batches that include samples in the mid range peCheck Solids 3 verify and obtain the Consensus value and the Confidence Interval stated on the Certificate of Analysis This standard is added to batches that include Industrial Waste samples and to check high level House Reference Material SOP 12_Solids_v5 1 docx 6 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 7 of 21 Preparation of the Certified Reference Material peCheck 1 To prevent solids sticking to the cap Do Not Shake bottle before use 2 Put 800 ml of deionised water into a 1
31. rence eee eeeeeeeeeeeaeeneeas p 4 Current Version 5 1 Version 5 1 October 10 2014 Reviewers J Jones G Levesque Removed most hyperlinks to external documents folders Introduction and Scope referenced method sas sacs css yess ied Sen sdassziasaovventssosuann a a h i aE aii p 3 Sample Requirements analyze within 2 hours if not refrigerated ccccceeesecceceeeeeeeeeeeeaeeeeeeeeeeeees p 4 Glassware Preparation may be washed manually eee eee eeeeeeee eee eeeeeeteeeeesaeeeeeeaaeeeeetaeeeeetaeeeeeeaeeeeeeas p 8 Inspect amp acid wash gooches that are still dirty after going through the dehwasher p 8 Crucible beaker Preparation Crucibles are not put in the dishwasher step removed ssssssse111s1 p 9 Quality Control Plan Internal balance calibration is performed on Balance p 10 Appendices added Tab 6 Daily Balance Calibration Check p 20 References added balance user manual references ssssssinenteesstttrttnsttettttn tn nsttertnnn nn nsttentn nnne neee ent p 21 Endnotes new section in References for listing file and folder locations in one place p 21 Update flow charts on pages 13 to 17 Next Review No Later than October 20 2015 Sign the following only if there are no significant changes required at the next review SOP 12_Solids_v5 1 docx 19 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Bran
32. sing the DailySolids xls program A manual calculation to verify the formula must be done and recorded at least once after any revisions or changes are incorporated into the DailySolids xls program Manual Calculations TOTAL SOLIDS TS Fe WET WEIGHT ei DRY WEIGHT ei SOLIDS T S w2 wi W1 weight g of vessel gooche crucible crucible aluminumdish or beaker For total suspended solids W1 weight of prepared gooche filter W2 weight g of the vessel amp sample For total suspended solids W2 weight of dried gooche filter sample W3 weight of vessel and dried residue after drying at 104 1 C or 180 42 C W4 weight g of residue after ignition at 550 C W5 W2 W1 or sample weight W6 W3 Wi or dry sample weight W7 W3 W4 or weight of volatile component V sample volume mL Total Suspended Solids Mg kb W2 W1 X 1000 x 1000 V mL Total Volatile Suspended Solids mg L W3 W4 x 1000 x 1000 V mL Or W7x 1000 x 1000 V mL Total Solids mg L W2 W1 X 1000 X 1000 or W5 x 1000 x 1000 V V mL Total Solids W3 W1 x 100 or W6 x 100 W5 W2 W1 Total Volatile Solids W3 W4 X 100 or W7 x 100 W6 W3 W1 Volatile Solids mg L W3 W4 x 1000 x 1000 V mL Total Dissolved Solids mg L W2 W1 X 1000 X 1000 V mL Or by calculation only SOP 12_Solids_v5 1 docx 18 Date Printed 10 22 2014 Accredited Test Method Method Name
33. weezers to transfer the filter directly weight as Vessel amp Sample Wtin onto the balance pan Recordin the DailySolids xls worksheet workbook as Filter Sample wt Enter results in LIMS by Batch Import or manual batch entry Save gooche for enccccccccccccscccessscccesccccs otal Volatile Suspended Solids Total Volatile Suspended Solids I i If the TSS test is not required follow the PSS procedure Steps 1 i through 10 but skipping step 2 The first weights not necessary The weight in step 10 is the first weight recorded i 1 Transfer the gooche aluminum dish from the completed TSS analysis into the muffle ovenyset at 550 oC for 1 hour 2 Remove from the muffle oven and set on the tile or cooling rack until mostiof the heat has dissipated 3 Place ingtheydesiccator for at least 30 minutes samples should cool to room temperature 4 Weigh onsthe analytical balance and enter the weight as 7VSS or TS Final Wt in the DailySolids xls worksheet DO NOT ALLOW THE GOOCHES TO SIT OUTSIDE THE DESSICATOR FOR MORE THAN 5 MINUTES Enter results in LIMS by Batch Import SOP 12_Solids_v5 1 docx 14 Date Printed 10 22 2014 Accredited Test Method Method Name SOP 12 Solids v5 1 Analytical Services Branch Method Date October 20 2014 Environmental Standards Division Page 15 of 21 Total Solids Total Solids mg L Total Solids liquid sample solid sample 1 Record crucible ID number in t
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