Document RjKa53QmpBEXdKDXLYMN12BEn

Fluoroche Samples. Centre AnalyticalLaboratories,Inc. 3048 Research Ddve Phone: (814)231-8032 StateCollege,PA 16801 Fax:(814)231-1253 or(814)231-1580 Ana"cal Report FluorochemicalCharacterizatioonf DrinkingWater Samples Cleveland,Tennessee (W1973) Centre AnalyticalLaboratory Rep**orNto. 023-007A TestingLaboratory CentreAnalyticaLlaboratoryI,nc. 3048 Research Drive StateCollege,PA 16801 3M Environmental Laboratory Contact Kent R. Lindstrom Bldg.2-3E-09 P.O. Box 33331 St.Paul,MN 55133-3331 Phone: (651)778-5352 Requester Kds J.Hansen,Ph.D. 3M EnvironmentalTechnology & SafetyServices Bldg.2-3E-09 P.O. Box 33331 St.Paul,MN 55133-3331 PAGE 1 OF 5 Introduction Resultasrereportfeodrtheanalysoifsa serieosfdrinkiwnagtersamplerseceivebdyCentre AnalyticaLlaboratorieIsn,c.(Centre)frorrthe 3M EnvironmentaLlaboratory.The sampleswere collectefdrom Cleveland,Tennessee. The Centrestudynumber assignedtotheprojectis023007. Specififcluorachemicaclharacterizatiboynliquicdhromatography/tandem mass spectrometry (LC/MS/MS) was requestedforallsamples. A totaolf17 samples were receivedforanalysis. The samples were preparedand analyzedby LC/MS/MS forthefollownglisotffluorochemicals: Table 1:TargetAnalysis Comt)ound Name PerfluorooctanSeulfonate PerfluorooctanSeulfonviamide Perfluorooctanoate Acronvm PFOS PFOSA POAA Data generatedin supportof thisstudywas generatedaccordingto USEPA Good Laboratory Practice(sGLPs). The analyticamlethod used was validatebdy Centre.The validatiopnrotocol and resultasreon fiewithCentre.Data presentedhere isthehighestqualitdyataava7ilabaltethis tme. 2 Sample Receipt The samples were submittedin individuapllasticontainersand were not preserved. Seventeen individuaslample containerswere received.Samples were receivedon 02115/00. The sample collectiodnateswere notsupplied.Chain-of-custodiynformatioinspresentedin Attachmentk Samples MC-127H and MC-134H were notanalyzedas per clienrtequest.(Telephonecallto KsisHansen an 2116100). 3 Holding Times The analyticamlethod used was validatedagainsta mal)(imumholdingtime of 14 days. The stabiliotfytheanalytesofinteresftorlongerperiodshas notbeen determined. PAGE20FS 4 Methods-AnaVicaland Preparatoty 4.1 LC/MSIMS 4.1.1 SamplePreparatifoonrLC/MSIMSAnalysis Sampleswereinititarlelaytewdith200uL of250mgA-sodiumthiosuffsaotleutitoonremove residualchlorineS.o,lidphase extractio(nSPE) was used to preparethe samples for LC/MS/MS analysis.A forty-milliplofrtteironofsample was transferretdoa Cls SPE cartridge. The cartridgweas firsetlutedwith5 mL of40% methanolinwatersolution.The eluatewas discardedand the SPE column was then elutedwith100% methanol. A 5 ml portionof methanolwas collectefdoranalysisby LC/MS/MS. Thistreatmentresultedinan eight-fold concentratioonfthesamples priortoanalysis. 4.1.2 Sample Analysis4y LCIMSIMS InHPLC, an aliquootfextractisinjecteadnd passed througha liquid-phascehromatographic column. Based on theaffiniotfythe analyteforthestationarpyhase inthe column relativteo theliquimdobile phase,the analyteisretainedfora characteristaimcount oftime. Following HPLC separationE,S/MS providesa rapidand accuratemeans foranalyzinga wide range of organiccompounds, incjudinfgluorochemicalsB.ectrosprayisgeneralloyperatedat relafively mildtemperaturesm;oleculesare ionizedf,ragmented,and detected.Ionscharacteristoifc known fluorochemicalasreobservedand quantitateadgainststandards. A HevAeft-PackardHP1 100 HPLC system coupledtoa Micromass UltimaMS/MS was used to analyzethe sample extractsA.nalysiswas performedusingselectedreactionmonitoring (SRM). Samples were extractedon 2/17/00and analyzedby MS/MS between 2117/00and 2118100.The HPLC and MSIMS methods used foranalysiasnd instrumentparameterscan be found inattachmentD. 5 Analysis 5.1 Calibration A 7-pointcalibraticounrvewas analyzedatthe beginningand end ofthe analyticaslequence forthe compounds of interestThe calibratipoonintswere preparedat 0, 25, 50, 100,250, 500, and 1000 ng/L (ppt)The response ofthequantftatoinonversustheconcentratiownas Plottedforeach point Using linearegressionwith1/xweightingt,he slope,y-:interceapntd correlaticoonefficie(nrt)and coefficieonftdeterminatio(n@jwere determined.A calibration curveisacceptableW r> 0.985 (@ > 0.970). Calibratiosntandardsare preparedusingthesame SPE procedureused forsamples. Calibratiocnheck standardswere analyzedperiodical(leyverythreetofivesample injections) throughoutthe analysissequence. Compliance is obtainedff the standardanalyte concentrationasrewithin+/-20% oftheactualvalue. For ther-esultrseportedhere,calibraticorniteriwaere met PAGE3 OFS 5.2 Blanks ExtracUbolnankwsereprepareadndanalyzewditheveryextracuboantchofsamplesT.he extractiobnlanksshouldnothave any targetanalytespresentator above theconcentratioonf thelow-leveclalibratisotnandard.Forthesesamples,theextractiobnlankswere compliant Instrumentblanksinthe form of cleanmethanolsolventwere alsoanalyzedaftereveryhighlevelcalibratisotnandard,and afterknown high-leveslamples. Again,the blanksshouldnot have any targetanalytespresentat or above the low-leveclalibratisotnandard. For the samples presentedhere theinstrumentblanksarecompliant. 5.3 Surrogates Surrogatespikesarenota component oftheLC/MS/MS analyticmaelthod. 5.4 Matrix Spikes Matrix spikes were prepared for every sample at a concentrationof 100 ng/L using all compounds ofinterestM.atrixspikerecoveriesaregiveninAttachmentC. Fieldspikeswere alsopreparedon severalsamples ata concentratioonf 100 ng/L usingall compounds ofinterestFieldspikerecoverieasre alsogiveninAttachmentC. 5.5 Duplicates AJIsamples were analyzedinduplicate.Resultsare givenalongwiththe sample resultsin AttachmentB. 5.6 Laboratory Control Samples Milliwqaterwas spikedwithallcompound ofinteresatt25 and 250 ngA-. Initiaanlalysisofthe 25 ngILLCS showed low recoveryforPFOS. The standardwas re@injectaendd was foundto have acceptablerecovery(70-130%).AJIotherrecoveriefsorallcompounds were between 70130% ineach LCS. 5.7 Sample Related Comments Fieldblank samples consistedof empty containers.Fortymillilitoefrstype Iwater filtered througha hypercarbcartridgweas added to theempty containerand analyzedinthesame manner as theothersamples. 6 Data Summaty Pleasesee AttachmentB fora detaileldistinogftheanalyticraelsults. 7 DatalSample Retention Samples are disposedofone month afterthe reportisissuedunlessotherwisespecified.AJI electronidcata isarchivedon retrievablmedia and hard copy reportsare storedin data foldersmaintainedby Centre. PAGE4 OFS 8 Attachments 8.1 AttachmentA: Chain-of-CustDdy 82 AttachmentB: Results. 8.3 AttachmentC: MatrixSpikeRecoveries(Fieldand LaboratorySpikes) 8.4 AttachmentD: LC/MS/MS Raw AnalyticaDlata 9 Signatures ohn-M. FlahertyM, a e -IndustriSaelrvicesGroup Date /"(:Ic KevinJ Uoyd,-Vice President Date OtherLab Members ContributngtoData Enaksha Wickromesinhe Karen Smith PAGESOF5 iomw Lim" Lmo Low Mw jm im @so 3M Liivii Form 38778 - PYVO Sl,lpl)inAgdd(.sa@ 31.1filij2.3E W !IjSfJu'liA i.tiu. St 551cis iticiitLaalboi-atoi-y Telephone: Saniple Receiving:(6511778-4940 'Alternate1:651)??8-6753 FAX: (6511776-6176 ContactName n Company M2iling Address fx/ll CL City,State,Zip -DI Telephone Special Instructionsandior SpikclflcRegulatory Requirements: (nialtio4l.imituf LialecliDrne,poilingunits,eic.) ell rv 11-7 2,3. _VAL 4. ClientSample Identification -m3+ALe-PIA) -:r J Chain ofCustody/Reque, ProjectID/ProjecNtame Template ProjectL ad Dept. (main) -)LraboratorAynalytical 17120 4-Difid4:"ll(- FIintna eI ppoto:tDDDuauete@DDaattee@'l@@4::@@7L@ Innteerrnnal@Due Date ---'Job/Proje9ctr'V',i -a-E= Date Available DateDue FAX Contract L.ab Preservatives: Co 0 Cl) A3 000 E z cn 0 0 fi z c > z o ii0 0 3iT- Date LIMS# Sampled Time Sampled Loiri -A2A1 -W LA Matrix/ I Media Enterthenumber of co tainersof each 172 6- 7. _ML-l 4 14-cui- 910. colIL-Ctebdy (print): k u cLo-Lo-to-YSpil @3 Item Relinquishedby/Affiliation C) 0 Collector'ssignature- Time Date ShippedVia: Received b)Y/IAA.Mlll*atl'O SainpleConditionUpon Receipt: Temperature: c 0(@.erAssociated CoCs.@ 10 Acceptable 0 Other: 0 Received on Ice copies I(): P.Ua ofJ;7, Orininal-Accomoonvim Samning *AWN A&W aw am dam AW AN M M M M M M a'@'Al@IIN'iiiiientalLaboi-atoi-y Fc,tina8776-PVJO 3t.)bi.lil2 JE U9 ijilB,ush Av.iiua st pdt4l..it4651r,6 Telephone: SaiiipleReceiving:(651) 7784946 Allainate:(651) 778-6753 FAX@. (661) 773-5176 .9 --. Coiita(;tNaine @LL-1-1-6 U) Company 0 Mailing Addfe CL City, State, Zip IY Telephone Special Instructionsand/orSpecificRegulatory Requirernents: (iii.itiuldi.iio)fidiei.ciiunr,epoilingunitse,tc.) 7@L) Item Client Sample ldentirication Dw-p- 2. 3. 4. 5. 13;?11-S;jU 3 A) 6. A) 7. 8. 9. 10. Chain ofCustody/Reque, ProjectID/ProjecNtame Template # Project Lead Dept. (main) -)LraboratoryAnalytical -14-la4ife'prt@Due Datw internalDue Date Cl-a-ss/Job/Pr 'ect 17121 . Date Available Date Due FAX Contract @ab C, Preservatives: Co 0 3M LIMS# Date Sampled Time Sampled .0 > z 0 0E 0 in z 3 0 m zc 0 -- x B0 0 mit-rix-/ Media Enter the rv-wnberof containers-ofeach Collect ed by( rint): -0 Item 0 .C: L) Relinquished by/Affiliation Time Date Collectoes sign ture: Ship p ed Via: Received by/Affiliatio Saiiiple Condition Upon Receipt: -Felllpera[Llfe: c ()II,LArN@,,ciateCdOCS: I-loo, 1-11-31, 0 Acceptable 0 Other: 0 Received 2-5, 1-) on Ice Copies to: Comments: 1..J. A,-L fit Orion.1- Cc=ntrr=Analytical Laboratorir=s,I,nc. 3048ResearchDrive,StateCollegePA 16801 814-231-8032 FAX 814-231-1253 AnalyticRaelsultWs1973ClevelanTde,nnesse 3M Sample Identification MC-1 15H MC-1 17H MC-120H MC-121H MC-123H MC-126H MC-128H MC-131H NA MC-132H NA MC-1 33H Sample Description Intake-P/N Intake-P/dNuplicate Intake-FieBlldank Oufflow@PIN Oufflow@P/Nduplicate Site1 P/N SiteI P/t4duplicate Site2 PIN Site2 P/N duplicate Site3 P/N Site3 P/N duplicate FieldBlankP/N Empty PFOS (ng/L) < 25 < 25 < 25 < 25 <25 <25 <25 <25 <25 <25 <25 <25 PFOSA (ng/L) < 25 <25 < 25 < 25 < 25 < 25 < 25 < 25 < 25 < 25 <25 < 25 POAA (ng/L) < 25 <25 <25 <25 <25 < 25 <25 <25 <25 <25 <25 < 25 Please referto thereverseside forour standard tenns and condftions.