Document B8GyYXv7ry92Z6v0ro4K4NBXm

Fluoroc Sample Cr=ntrrA=nalyticalLaboratories,Inc. 3048 Research Drive StateCollege,PA 16801 1% Phone: (814)231-8032 Fax:(814)231-1253 or (814)231-1580 Anawcal Report FluorochemicalCharacterizatioonf DrinkingWater Samples Decatur,Alabama (W1979) CentreAnalyticalLaboratoryReport No. 023-007B 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 PAGELOFS Introduction Resultasrereportfeodrtheanalysoifsa'sedeosfdrinkiwnagtersamplesreceivebdy Centr.9 AnaWcal LaboratorieIsn,c.(Centre)from the3M EnvironmentaLlaboratory.The samples were collectefdrom Decatur,Alabama. The Centrestudynumber assignedtotheprojectis023-007. Specififcluorochemiicaclharacterizabobny liquicdhromatography/tandem mass spectrometry (LC/MS/MS) was requestedforallsamples. A'totaolf14 sampleswere receivedforanalysis. The samples were preparedand analyzedby LCIMS/MS forthefollownglisotffluorochemicals: Table1:TargetAnalysis ComDound Name PerfluorooctanSeulfonate PerfluorooctanSeulfonviamide Perfluorooctanoate Acronym PFOS PFOSA POAA Data generatedin supportof thisstudywas generatedaccordingto USEPA Good Laboratory PraeUces(GLPs).-The analyticamlethod used was validatebdy Centre.The validatiopnrotocol and resultasreon filweithCentre.Data presentedhereisthehighestqualitdyata availablaetthis time. 2 Sample Receipt The samples were submittedinindividuapllasticontainersand were not preserved. Fourteen individusaalmple containerwsere received.Samples were receivedon 02/15100.The sample collectiodnateswere notsupplied.Chain-of-custodiynformatonispresentedinAttachmentA- 3. Holding Times. The analyticamlethod used was validatedagainsta ma)dmum holdingtime of 14 days. The stabiliotfytheanalytesofinteresftorlongerperiodshas notbeen determined. PAGE 2OF5 4 Methods-Analyticaanld Preparatory 4.1 LCIMS/MS 4.1.1 SamplePreparatifoonrLC/MS/MSAnalysis Sampleswereinitiatlrleyatewdith200 uL of250 mg/Lsodiumthiosulfsaotleutiotnoremove residucahllodneS.o,lidphase extractio(nSPE) was used to preparethe samplesfor LC/MS/MS anaws. A forty-millilpiotretrionofsample was transferretdo a Cls SPE cartridge. The cartridgweas firsetlutedwith5 mL of 40% methanol inwater solution.The eluatewas discardedand the SPE column was then elutedwith100% methanol. A 5 mi portionof methanol was collectefdoranalysisby LC/MS/MS. This treatmentresultedinan eight-fold concentrationofthe samples priortoanalysis-. 4.1.2 Sample Analysisby LCIMSIMS In HPLC, an aliquotof extractisinjectedand passed througha liquid@@hascehromatographic column. Based on the affiniotfythe analyteforthestationarpyhase inthe column relativteo theliquimdobile phase,the analyteisretainedfora characteristaimcount oftime. Following HPLC separation,ES/MS providesa rapidand accuratemeans foranawng a wide range of organiccompounds, includingfluorochemicalsE.lectrospraiysgenerallyoperatedatrelatively mildtemperatures;molecules are ionizedf,ragmented,and detected. Ions characteristiocf known fluorochemicalasre observed and quantitatedagainststandards. A HeWett-Packard HPI 100 HPLC system coupledtoa Micromass Ultma MS/MS was used to analyzethe sample extractsA.nalysiswas performed using selectedreactionmonitoring (SRM). Samples were extractedon 2/18/00and analyzedby MSIMS between 2tiB/00and 2/19100.The HPLC and MS/MS methods used foranalysisand instrumentparameters can be found inattachmentD. 5 Analysis 5.1 Calibration A 7-p6intcalibratiocnurve was analyzed at the beginningand end of the analyticaslequence forthe compounds of interestT.he calibratiopnointswere preparedat 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt)The response ofthe quantitatioinonversus the concentrationwas plottedforeach point.Using linearregressionwith1/xweighting,the slope,y-interoepatnd correlatiocnoefficie(nrt)and coefficienotf determination(r-2wjere determined. A calibration curve isacceptableifr> 0.985 (@ > 0.970). Calibratiosntandardsare prepared usingthe same SPE procedureused forsamples. Calibratiocnheck standardswere analyzed periodical(leyverythreeto fivesample injectons) throughoutthe analysissequence. Compliance is obtained ff the standard andyte concentrationasre within+/-20% of the actualvalue. For the resultsreportedhere,calibratiocnriteriwaere met PAGE30F5 5.2 Blanks Extractbolnankwsereprepareadndana4eedwitheveryextractbiaotnchofsamplesT.he extractiobnlanksshouldnothave any targetanalytespresentatorabove the concentratioonf thelow-leveclalibratisotnandard.Forthesesamples,theextractonblankswere compliant Instrumentblanksinthe form of cleanmethanolsolventwere alsoanalyzedaftereveryhigh-leveclalibratisotnandard,and afterknown high-leveslamples. Again,the blanksshould not have any targetanalytespresentat or above the low4evelcalibratisotnandard. For the samples presentedheretheinstrumentblanksare compliant. 5.3 Surrogates Surrogatespikesare nota component ofthe LCIMS/MS analyticamlethod. 5.4 Matrix Spikes Matrixspikes were prepared for every sample at a concentrationof 100 ng/L using all compounds ofinterestMatrixspikerecoveriesaregiveninAttachmentC. Fieldspikeswere alsopreparedon severd samples ata concentratioonf 100 ng/L usingall oompounds ofinterestFieldspikerecoveriesarealsogiveninAttachmentC. 5.5 Duplicates Allsamples were analyzedinduplicate.Resultsare givenalongwiththe sample resultsin AttachmentB. 5.6 Laboratory Control Samples Milliwqaterwas spikedwithallcompound ofinteresatt25 and 250 ng/L.Initianlalysisofthe 25 ngA-LCS showed low recoveryforPFOS. The standardwas reinjecteadnd was foundto have acceptablerecovery(70-130%).Allotherrecoveriefsorallcompounds were between 70130% ineach LCS. 5.7 Sample Related Comments Fieldblank samples consistedof empty containers.Fortymillilitoefrstype I water filtered througha hypercarbcartridgweas added to theempty containerand analyzedinthesame manner as theothersamples. '6 Data Summary Pleasesee AttachmentB fora detaileldistinogftheanalyticraelsults. 7 DatalSample Retention Samples are disposedof one month afterthe reportisIssued unlessotherwisespecffied.AJI electronidcata is archivedon retrievablmeedia and hard copy reportsare storedin data foldersmaintainedby Centre. PAGE4QF5 PM 8 Attachments 8.1 AffadynentA:Chain-of-CustDdy 82 AftachmentB: Resufts. 8.3 AttachmentC: MatrixSpikeRecoveries(Fieladnd LaboratorySpikes) 8.4 AttachmentD: LCIMSIMS Raw AnalyticaDlata 9 Signatures //'JoJ'ho2nhbn- M. FlahertyM,a naoer-IndustriSaelrvicesGroup KevinJ Uoyd, VicePresident Z/C? Date @ixek-00 Date Other Lab Members ContributintgoData Enaksha Wickremesinhe Karen Smith PAGE5QF5 3M Envii Fam 387?8 - PWO Shipping Address: 3M Skig.2-3E-09 935 Bush Avwwo st P" MN 55108 -mentalLaboratory Telephone: $-"Oo Rec*Mno: (451)7784M AltwnM*: fell)77"753 FAX. (651)7T"Iyg ContactName 4rb Company L-;im t: MailingAddress city,State,Zip 15, Telephone -ipeciallnstrucuonsandfot specificRegulatoryRequirements: (FnothockOMA ofd(AecUM reponkv uts. @tQ) D c) ChainofCri-stod/yReque,%')'rLaborAtorAynalytical 17122 Project lp/Project Name Mli j-CO-7 IZol-6 Template ProidctLood-'A@-6r,;ias@t,in Dept.# (miln) L);E&i -:r&42if)eie'U!T4 L4.A-he A,@,ako lnalfteportDue DatW InternaDlue Date rig-titflnhfencpt3#&)10<lvc;-OCA Date Available Po &yy Date Due FAX 0 ContractLob Preserva0ves: 0 .,4L jtem 1. 2. ClientSample Identification :nZiAi@L_,V;elA I_Ajo 3M LIMS# Date Sampled ..U" -AJI4 3. 4. 5. 6. -OLA_Wbu-PIA) 7. Y)l 8 m c 4 -OLacw -.Vfa,$akl,pm 9- -PJA) 10. lm(-;;LAtOI4 P Collected by (print): 0 Item Ft6Hnquish6dby/Aftillatidii- @&O 0z (3 zG0o a zE2 0 0 Tkne Matrix/ Sampled Media &dr ft runber ofcontainersofeach A)IA1,,AtW eoilectoessignature: I Vii@ -Fed i.4C @;,, . . @LIAM list Sample ConditionUpon Receipt: & Acceptable 0 Other Temperature: Othw AssockdedCoca- c 0 Received on lee :tO$ t-IIA% 1-1 Copiestw. Page of Orinina-lAccomoonvina Swnplos pp'. mCo mots: %'NVE'nlvii Form 38770 - PWO Shipping Address,. 3M Bldg,2-3E-09 935 Bush Avenue SL Paul,MN 65 106 ment,aLlaboratory Telephone: Sample Receiving:(651)778-4948 Alternate:(GSI)TYS-6753 FAX: (651)7784176 Conl 75 Company ChainofCustody/Reque. )rLaboratorAynalylical 17 1 2z ProjecItD/ProjecNtame M2,@CUI nlt Template I Vin Fin R portDue is ProjectLead Z@rif:,C@q InternaDlue Date Dept.#(main)___14atil f@i---"ob/Pject#cXglo-t@-&<S-o Ck Date Available a MailingAddress 06 - City,State,Zip 0 J@m w @Tel@,l@one Special Instructions andfor specific Regulatory Requirements: (meuiod.hmk ofdatedion.reportingunits,sic) FAX 1 -7-7@5-IoL--)@ Date Due' ContractLab -0 ILI tk)11-7@ 4L- Item ClientSample Identification I. -;o@v i:gI-T-if-ld_II-A),l oLe-0p 2. Mr @-aZo 5itz I :n@IA -CIA U.. :2PI;4 3- ML-,;L3oA Pl/u 4. 3mLIMS# wi" Date Sampled Preservatives: 00 0 z U) 0 0 :s x > z 0 Time Sampled A)LA Matrix/ Media Enterthe number of containersof UA-K-Y 0 @ L.) 20 E :3 zc 00 5. 6. 7. 8. 9. 10. Collectebdy( rint): lem Relinquishedby/Affillati6n.,..,,@2:,:.,!i !L. MePL'.l Dits Collectors ignature: ppeidMa.'' :'@@@d by/Affilia 0 Sample ConditionUpon Recelpt: Temperature: c Other AssociatedCoCsi I-)1.)Ol 1-1 0 Acceptable 0 Other 0 Received on Ice l@713&, 1-71;2-7# Copiesto: )61 1-)1:)1,1'7130,1-71'61,1-7153, r7i'3LI Co m ments: Centrc= Analytical @*Ns6N.4=WwLaboratorieIsn,c,. 3048 ResearchDrive,StateCollegePA 16801 814-231-8032 FAX 814-231-1253 AnalyticRaelsultWs1979DecatuArl,abama 3M Sample Identification MC-215H MC-217H MC-220H MC-221 H MC-223H MC-226H MC-228H MC-233H Sample Description Intake-P/N Intake-P/dNuplicate Intake-FieBlldankEmpty Oufflow-P/N Outflow-P/Nduplicate SiteI P/N SiteI PIN duplicate FieldBlankP/N Empty PFOS (ng/L) < 25 < 25 <-25 c@25 < 25 < 25 < 25 < 25 PFOSA (ng/L) < 25 < 25 <25 <25 <25 <25 < 25 < 25 POAA (ng/L) < 25 < 25 <25 < 25 < 25 < 25 < 25 < 25 Pleaserefertothe reverseside)orour standardforinsand condhions.