Document V3wK7oMVyN3oZM0e40QymeOLp

Fluoroch Samples Centre AnalyticalLaboratop!Fs,Inc. 3048 Research Ddve StateCollege,PA 16801 0 Phone: (814)231-8032 Fax:(814)231-1253 or(814)231-1580 AnaWcal Report FluorochemicalCharacterizatioonf DrinkingWater Samples Mobile,Alabama (W2151) Centre AnalyticalLaboratoryReport No. 023-007C TestingLaboratory CentreAnalyticLaalboratoryI,nc. 3048 Research Drive StateCollege,PA 16801 3M Environmental Laboratory Contact Kent R. Lindstmm Bldg.2-3E-09 P.O. Box 33331 St.Paul,MN 55133-3331 Phone: (651)778-5352 Requester KrisJ.Hansen, Ph.D. 3M EnvironmentalTechnology & SafetyServices Bldg.2-3E-09 P.O. Box 33331 St.Paul,MN 55133-3331 PAGE 1OF5 Introduction Resultasrereportfeodrtheanalysoifsa serieosfdrinkiwnagtersamplesreceivebdyCentre Ana"cal LaboratorieIsn,c.(Centre)from the3M EnvironmentaLlaboratoryT.he samples were collectefdrom Mobile,Alabama. The Centrestudynumber assignedtotheprojectis023-007. Specififcluorochemicaclharacterizatiboyn liquicdhromatography/tandem mass spectrometry (LC/MS/MS) was requestedforallsamples. A totalof16 samples were receivedforanalysis. The samples were preparedand analyzedby LC/MS/MS forthefollowinlgisotffluorochemicals: Table 1:TargetAnalysis ComDound Name. PerfluorooctanSeuffonate PerfluorooctanSeulfonviamide Perfluorooctanoate Acronvm PFOS PFOSA POAA Data generatedinsupportof thisstudywas generatedaccordingto USEPA Good Laboratory Practice(sGLPs). 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. Sixteen individusaalmple containerwsere received.Samples were receivedon 02/15/00.The sample collecfidoanteswere notsupplied.Chain-of-custodiynformatioinspresentedinAttachmentA. 3 Holding Times The analyticamlethod used was validatedagainsta maximum holdingtime of 14 days. The stabiliotfytheanalytesofinteresftorlongerperiodshas notbeen determined. PAGE20F5 4 Methods-AnaVicaland Preparatoty 4.1 LC/MSIMS 4.1.1 SamplePreparatifoonrLC/MSIMSAnalysis Sampleswereinititarlelaytewdith200uLof250 mg/Lsodiumthiosulfsaotleutitoonremove residualchlorineS.o;lidphase extractio(nSPE) was used to preparethe samples for LC/MS/MS analysis.A forty-milliplofrtteironofsample was transferretdoa Cle SPE cartridge. The cartridgweas firsetlutedwith5 mL of40% methanolinwatersolution.The eluatewas discardedand the SPE column was thenelutedwith100% methanol.A 5 mi portionof methanolwas collectefdoranalysisby LC/MS/MS. Thistreatmentresultedinan eight-fold concentratioonfthesamples priortoanalysis. 4.1.2 Sample Analysisby LCIMS/MS InHPLC, an aliquotofextractisinjecteadnd.passed througha liquid-phascehromatographic column. Based on theaffiniotfythe analyteforthe stationarpyhase inthe column relativteo theliquimdobilephase,the analyteisretainedfora characterisatmiocunt of time. Following HPLC separationE,S/MS providesa rapidand accuratemeans foranalyzinga wide range of organiccompounds, includinfgluorochemicalsE.lectrospraiysgenerallyoperatedatrelatively mildtemperaturesm;oleculesare ionizedf,ragmented,and detected.Ionscharacteristoifc known fluorochemicalasreobservedand quantitateadgainststandards. A HeWett-PackardHP1 100 HPLC system coupledtoa Micromass Ulbma MS/MS was used to analyze-thesample extractsA.nalysiswas performedusingselectedreactionmonitoring (SRM). Samples were extracteodn 2/23/00and analyzedby MS/MS between 2/23/00and 2/24/00.The HPLC and MS/MS methods used foranalysiasnd instrumentparameterscan be found inattachmentD. 5 Analysis 5.1 Calibration A 7-pointcalibraticounrve was analyzedat thebeginningand end ofthe analyticaslequence forthecompounds of interestThe calibratipoonintswere preparedat 0, 25, 50, 100,250, 500,and 1000 ngA- (ppt)The response ofthe quantftaboinonversustheconcentratiownas plottefdoreach point Using linearegressiownith1/xweightingt,he slope,y-interceapntd correlaticooneffidie(nrt)and coefficieonftdeterminatio(ne)were determined.A calibration curveisacceptableffr> 0.985 (r,>20.970). Calibratiosntandardsarepreparedusingthesame SPE procedureused forsamples. Calibratiocnheck standardswere analyzedperiodical(leyverythreetofivesample injecuons) throughoutthe analysissequence. Compliance Is obtainedff the standardanalyto concentrationasrewithin+/-20% ofthe actualvalue. For theresultsreportedhere,calibraticorniterwieare met. PAGE3 OF5 5.2 Blanks ExtracUbolnankwsereprepareadndanalyzemd(itehvereyxtractbiaotnchofsamplesT.he extractiobnlanksshouldnot have any targetanalytespresentatorabove the concentratioonf thelow-leveclalibraflsotnandard.Forthesesamples,theextractiobnlankswere compliant. Instrumentblanksinthe form ofcleanmethanolsolventwere alsoanalyzedaftereveryhighlevelcalibratisotnandard,and afterknown high-leveslamples. Again,the blanksshouldnot have any target,analytpersesentat or above the low-leveclalibratisotnandard. For the samples presentedheretheinstrumentblanksarecompliant 5.3 Surrogates Surrogatespikesare nota component oftheLC/MStMS analyticmaelthod. 5.4 Matrix Spikes Matrixspikes were prepared for every sample at a concentratioonf 100 ng/L using all compounds ofintereslMatrixspiker.ecoveriesaregiveninAttachmentC. Fieldspikeswere alsopreparedon severalsamples ata concentratioonf 100 ng/L usingall compounds ofinterestFieldspikerecoveriesarealsogiveninAttachmentC. 5.5 Duplicates Allsamples were analyzedinduplicate.Resultsare given along withthe sample resultsin AttachmentB. 5.6 Laboratory Control Samples Milliwqaterwas spikedwithallcompound ofinteresatt25 and 250 ng/L, Initiaanlalysisofthe 25 ng/LLCS showed low recoveryforPFOS. The standardwas reinjecteadnd was foundto have acceptablerecovery(70-130%).Allotherrecoveriesforallcompounds were between 70130% ineach LCS. 5.7 Sample Related Comments Fieldblanksamples consistedof empty containers.FortymillilitoefrstypeIwater filtered througha hypercarbcartridgweas added tothe empty conta7inearnd analyzedinthe same manner as theothersamples. 6 Data Summary Please see AttachmentB fora detaileldistinogftheanalyticraelsults. 7 DatalSample Retention Sampies are disposedofone month afterthe reportisissuedunlessotherwisespecified.AJI electronidcata is archivedon retrievablmedia and hard copy reportsare storedin data foldersmaintainedby Centre. PAGE4 OF5 8 Attachments 8.1 Attachmentk Chah-of-CustDdy 8.2 AttachmentB: Resufts. 8.3 AttachmentC: MatrixSpike Recove@es (Fieladnd LaboratorySpikes) 8.4 AttachmentD: LC/MS/MS Raw AnalyticaDlata 9 Signatures ,",Ohn IndustriSaelrvicesGroup m KevinJ Uoyd, Vice President Date e-" -C)o Date OtherLab Members ContribubngtoData Enaksha Wi "kremesinhe Karen Smithc PAGE 5 OF5 MMM 3H EiiviimentaLlaboratorCyhain ofCustody /Reque. Fam 3877a - PM Shipping Address: 3M Bldg. 2-3E-09 Telephone: SanWIs ROCOlving' (651)771-4948 ProjectID/ProjecNtame ral@)-oo Template 935 Bush Averpio SL Pstd, M14 55 106 Alternate: (651) 7784733 FAX: PSI) 778-6176 ContactName @i-i@2 @.4isei(L ProjectLead 1Dept.# (main) A(M-Y-A- 11291 Company )rLaboratoryAnalytical intji FMal F@eportDue Dal Ti CInnItternalDue Date Class/Job/P ect fo Date Available 17128 AywLA 1! -L:l o'- MailingAddress 0 C0L City,State,Zip ix Telephone# (toaI) -7-&2- to0 IES Special Instructions andfor Specific Regulatory Requkements: (method. UmN of do(solon, ropwtkv ungs, sic.) -@oct P-D 69V- FAX Date Due c ontractLab flu- o 1 Preservatives: Com 0 w;z vy)DVI LT,AL Item ClientSample Identification ffILLi1!511 Y23:iZl@k-'PIA) 2- 3M LIMS# Date Tlme Sampled Sampled A) -A@IA ce c E o 00 0= z a 5Z 3: z 0 Matrix/ I I i0 1 II Media ErOor the number of cordakwrs of *ad'] ---7 1 1 OF I (E 3. ML- @ills" 4. LiI'lIA 6. lni--Li1;1z-lOU411ou-)PI/V 7. PIC-(4;Ni-O(Ak L-AAJ :Tit-kiLL.,th a- in(--LI;J49-DiA--Vd3OIAfj rL.Cm iv f Pi 9. C.-q 2511 -" @ic" I I I- -, I - 10. WINC-Ll:)ukl-5@liti-P/A) Collectebdy( rint)A: )IA Item Relinquishedby/Affiliation Collectorssignature: Time Date Shipped Via: Received by/A Sample ConditionUpon Receipt: 0 Acceptable 0 Other Temperature: c 4&Received on Ice OtherAssodated CoCs: 1-112; 1# 1'7"L's I" '?A 1-11-Lst -71 Cc& to. I')I 'LI it-2130, t7l *3 1.1'7 L'63, 1713 4.1-712-0 K@Y LAC Comments: $'adds" tormo fiowao uwm UW" mw mm wo 3M Envii Form 38778 -PWO ShippingAddress: 3M Bldg.2-3E-09 935]3ush Avenue St.Patd.MN 55106 mentalLaboratory Telephone: Smwle Receiving:(651)778-4948 Alternate(.651)778-6763 FAX- 1651)7764176 Contact Name 'S Company ChainofCustody/Reque. )rLaboratorAynalytical ProjecItD/ProjecNtame Template ProjectLead DepL # (M21n) -Lag M!!-00-1 I tAL)Iii(, Finai@e@poorrDttuD@@ee D'aatt@'4@ InternaDlue Date -Class/Job/P ect#oc)iooS5 17129 -Date Available PDI,@@v -5@5al MailingAddress-- 0 CL CRY, State.Zip @*1 P,4 Old ll:k3 Telephone # toI@t@-I),1I7N16-1,;b(g FAX to ;paclallnstrucdona*ntvorSpocine RegulatoryRequkmwnts: mogiod, Srnkofdatectkw%repcmlinugnitse,lm) Date Due ContractLab Prese@r@vaattiivvese-s: Comp k),a15-1 ob;AL, 0 0 0 r_ 0 z ca 0 -B Z r- 2: x 7- 0 - 0 Item 2. -P I ClientSample Identification 3M Date Time MatrFxt- LIMS# Samr)ted Sampled MediO Enterthemanbor-- alnwsofeachl (E ISI A4A A) 141kiLe T- I 3. 4. -o 51 -a--Sl-bk -P)A.) Pi/t.) 6. 7. 8. 10. CollJeEctebdy (print): IlleItctee'mmedby (pln')*=ReilinqRueilaisnhqeudishebdbiyylfaal@ffifllialtlisotnion E3 0 Collecto@ssign lure: ped Via., @@Rei:ij@edb'y/Affiliation arriplCeonditionUpon Receipt: 0 Acceptable 0 Other: amperature: c 0 Receivedon Ice NetAssociateCdoca: 1) 120,1'71 zi o 1'71 -@Lx,1'71 n Copies to: '71Z'zi 1'7,lti1713LI,1'71!W-1l-7133,171 Bq geFs 01-12, CkkhM -Aowmowwb-a SwnDlos I..Pf- Cornmwft., Cc=ntre Analytical Laboratorir=s, Inc. 3048ResearchDriveS,tateCollegePA 16801 814-231-8032 FAX 814-231-1253 AnalytiRceaslultWs2151MobilAel,abama 3M Sample Identification MC-415H MC-417H MC-420H MC-421 H MC423H MC-426H MC428H MC-431H NA MC432H NA MC-433H Sample Description Intake-P/N Intake-P/dNuplicate Intake-FielBdlankEmpty Outflow-P/N Oufflow-P/Nduplicate Site1 PIN SiteI P/N duplicate Site2 P/N Site2 P/N duplicate Site3 P/N Site3 P/N duplicate FieldBlank-PINEmpty 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 1<25 < 25 < 25 < 25 < 25 POAA (ng/L) < 25 <25 < 25 < 26 < 25 < 25 < 25 < 25 < 25 < 25 <25 < 25 Please refertothereversesideforour standard terinsand conditions.