Document 1g9E19rZ094O54v5xakEyLpbm

Fluoroc Sample CentreAnal icalLaboratoriesI,nc. 3048ResearcDhrive Phone: (814)231-8032 StateCollege,PA 16801 Fax: (814)231-1253or (814)231-1580 An -aI-W-(AL;Mal Report Fluorochemical Characterization of Drinking Water Samples Pensacola,Fl (W2176) Centre AnalyticalLaboratoryReport No. 023-007D TestingLaboratory CentreAnalyticLaalboratoryI,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 KrisJ.Hansen,Ph.D. 3M EnvironmentalTechnology & SafetyServices Bldg.2-3E-09 P.O. Box 33331 St.Paul,MN 55133-3331 PAGE IOFS Introduction Resultasrereportfeodrtheanalysoifsa serieosfdrinkiwnagtersamplesreceivebdyCentre AnalyticaLlaboratodesI,nc.(Centre)from the 3M EnvironmentalLaboratoryT.he samples were collectefdrom Pensacola,Fl.The Centrestudynumber assignedtotheprojecits023-007. Specificfluorochemicaclharacterizatiboynliquicdhromatography/ tandem mass spectrometry (LC/MS/MS) was requestedforallsamples. A totaolf16 sampleswere receivedforanalysis. The samples were preparedand analyzedby LC/MS/MS forthefollowinlgisotffluorochemicals: Table 1:TargetAnalysis Comt)ound Name -PerfluorooctanSeulfonate PerfluorooctanSeulfonviamide FPerfluorooctanoate Acronvm PFOS PFOSA POAA Data generatedinsupportof thisstudywas generatedaccordingto USEPA Good Laboratory Practices(GLPs). The analyticamlethod used was validatebdy Centre.The validatiopnrotocol and resultasre on filweithCentre.Data presentedhere isthehighestqualitdyataavailablaetthis time. 2 Sample Receipt The samples were submittedinindividuapllasticcontainerasnd were notpreserved.Sixteen individuaslample conta@inerwsere received.Samples were receivedon 02/15100.The sample collectiodnateswere notsupplied.Cha@in-of-custoidnyformatioinspresentedinAttachmentA. 3 Holding Times The analyticamlethod used was validatedagainsta maximum holdingtime of 14 days. The stabiliotfytheanalytesofinteresftorlongerperiodshas notbeen determined. PAGE20F5 4 Methods-Analyticanld Preparatory 4.1 LCIMS/MS 4.1.1 SamplePreparatifoonrLCIMSIMSAnalysis Sampleswereinititarlelaytewdith200 uLof250MGILsodiumthiosuffsaotleutitoonremove - residualchlorineS.olidphase extractio(nSPE) was used to preparethe samples for LC/MSIMS analysis.A forty-milliplofrtueorn ofsample was transferretdoa Cig SPE carvidge. The cartridgweas firsetlutedwith5 mL of40% methanolinwatersolution.The eluatewas discardedand theSPE column was then elutedwith100% methanol. A 5 mi portionof methanolwas collectefdoranalysisby LC/MS/MS. T'histreatmentresultedinan eight-fold concentratioonfthesamples priortoanalysis. 4.1.2 Sample Analysisby LCIMSIMS InHPLC, an aliquotofextractisinjecteadnd passed througha liquid-phascehromatographic column. Based on theaffiniotfythe analyteforthestationarpyhase inthecolumn relativteo theliquimdobilephase,the analyteisretainedfora characteristaimcount of time. Following HPLC separationE,S/MS providesa rapidand accuratemeans foranalyzinga wide range.of organiccompounds, includinfgluorochemicalsE.lectrospraiysgenerallyoperatedatrelatively mildtemperaturesm;oleculesare ionized,fragmented,and detected.-Ionscharacteristoifc known fluorochemicalasreobserved and quantitateadgainststandards. A HevAeff-PackardHPI 100 HPLC system coupledtoa Micromass Ultma MS/MS was used to analyzethe sample extractsA.na@sis was performed usingselectedreactionmonitoring (SRM). Samples were extractedon 2122/00and analyzedby MSIMS on 2/23/00.The HPLC and MS/MS methods used foranalysisand instrumentparameterscan be found inattachment D. 5 Analysis 5.1 Calibration A 7-pointcalibratiocnurve was analyzed at the beginningand end of the analyficaslequence forthe compounds of interestT.he calibratipoonintswere preparedat 0, 25, 50, 100,250, 500,and 1000 ng/L (ppt)The response of thequanfitaboinonversustheconcentratiownas plottedforeach point.Using linearegressionWith1/xweightingt,he slope,y-intercepatnd correlaticoonefficie(nrt)and coefficieonftdeterminatio(nr-w2ejre determined.A calibration curveisacceptableffr> 0.985 (? > 0.970). Calibratiosntandardsare preparedusingthesame SPE procedureused forsamples. Calibratoncheck standardswere analyzedperiodical(leyverythreeto fivesample injecbons) throughoutthe analysissequence. Compliance is obtainedif the standardanalyte concentrationasrewithin+/-20% oftheactualvalue. Forthe resultrseportedhere,calibraticorniterwieare met PAGE30F5 5.2 Blanks Extracfbiloannkwsereprepareadnd analyzewditheveryextractbiaotnchofsamplesT.he extractiobnlanksshouldnothave any targetanalytespresentator above the concentratioonf thelow-leveclalibratisotnandard.Forthesesamples,theextractiobnlankswere compliant. Instrumentblanksinthe form of cleanmethanol solventwere alsoanalyzedaftereveryhighlevelcalibratisotnandard,and afterknown high4evelsamples. Again,theblanksshouldnot have any targetanalytespresentat or above the low4evelcalibratisotnandard. For the samplespresentedheretheinstrumenbtlanksarecompliant 5.3 Surrogates Surrogatespikesarenota componentoftheLC/MS/MS analyticmaelthod. 5.4 Matrix Spikes Matrixspikeswere preparedforevery sample at a concentratioonf 100 ngA- using all compounds ofinterestM.atrixspikerecoveriesaregiveninAttachmentC. Fieldspikeswere alsopreparedon severalsamples ata concentratioonf 100 ng/Lusingall compounds ofinterestF.ieldspikerecoveriesare alsogiveninAttachmentC. The fielsdpike resultfsorsample MC-329H gave recoveriesforallcompounds of approximately1000 %, indilcatntghatthissample was possiblsypikedat 1000 pptinsteadof 100 ppt. 5.5 Duplicates Allsamples were anawed in duplicate.Resultsare given along withthe sample resultsin AttachmentB. 5.6 Laboratory Control Samples Milliwqaterwas spikedwithallcompound ofinteresatt25 and 250 ngIL. lnitaainalysisofthe 25 ngILLCS 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 Iwater filtered througha hypercarbcartridgweas added tothe empty containerand analyzedin thesame manner as theothersamples. 6 Data Summary Pleasesee AttachmentB fora detaileldistionfgtheanalyticraelsults. 7 DatalSample Retention samples are disposedof one month afterthereportisissuedunlessotherwisespecifiedA.JI electronidcata is archivedon retrievablmeedia and hard copy reportsare storedin data foldersmaintainedby Centre. PAGE4QF5 8 Attachments 8.1 AttachmentA:Chain-d-Custody .8.2 AttachmentB: Resufts. 8.3 AttachmentC: MatrixSpikeRecoveries(Fieladnd LaboratorySpikes) 8.4 AttachmentD: LC/MSIMS Raw AnalyticaDlata 9 Signatures @Joo2hhnLTMfa eI@rlya,@er-industrial ServicesGroup Date KevinJ LJoyd,Vice President Date OtherLab Members ContribufintgoData Enaksha Wickremesinhe Karen Smith PAGE50F5 33 CL c C5 Chain of Custoo'y 0 3 4b tr p pa !D 72. w c- 7 @J CL 0 cr 0a C6 0 0 cr ---------- 0 zv n* Report Results M Lr fA 3 KE to: t. Li c 0 0 0 2 cn 00 N ii @IIA 3 C36 4. 0 CO) 0 0 rL 06 (D (D CL HN03 "a H2SO4 cr 0 0 C Up 0 IL VOCs im 0 N one CCDA as cr cr Other TotalNumber of F" Containem > !r .9 oflt 0 No am @ am m " 3M Efnvii Form 313778- PWO ShippingAddress: 3t.1Bldg.2-3E-09 935 13ushAv a06 St.P,,,, Nw,l,u inentalLaboratoiry Telephone: Sample Receivingl:gil)7784948 Aftem I*:(851)77$4753 FAX: (;fil7l714176 ContactName Company Mailing Address 0 Pn ix City, late,Zip Telephone OL-0m: S SpecialInstmcdons andforSpecificRegul fy Reqiuiremonts: (MoUiod.lmk ofdot*cuon.reportintgnks.air-) A) -01 m" "M"M=== ChainofCustody/Reque. )rLaboratorAynalytical ProjectID/PrqjectName TeMP12te ProjecLtead f3f,,-, Dept.# (main) p OR-5-CD7 Mtjl-@- - it I innaa@litoporDtD@uDeatDat r7@@in InterrinnaDapluoleedDauuatete Class/Job/P ect 17127 Date Available Date Due FAX Contract Lab Preservatives: Co 0 f)iyw Item ClientSample ldentirication 2. -2,4)4 ykjL4b -P 3- M &@pa- 5@+1 1 1 Ak @D -C)I A 4. _M t 551 N -5; iva - IA) 5. illL @ap, 14-5ite3 -PIA)- 0 3M LIMS# )nk Date Sampled. Time Sampled %.@14 Matr[YJ Media Erderthem uAiz4, 5c 0 0 > N0 E 0a zc 0 ofcmainers ofeach 7. 8. 9. 10. '0>o1. C@oo@llleeccteiedby (print): A.)114 .q list" u 0 m u Relinquished by/Afrillatlon - -----Time Date Collectoes signature: k) IT- Shipped Via: Receiveid by/Affiliation 3ample Condition Upon Receipt: 0 Acceptable 0 Other. emperature.- c 0 Received on Ice therAssodal6dCoCs1:-71-zoi-liznli,Lili-)rz3,nizs,7C"s to: 71 Commmu: of Cr=ntrc=Analytical 0 Laboratories, Inc. 3048 ResearchDrive,StateCollegePA 16801 814-231-8032 FAX 814-231-1253 AnalytiRceaslultWs2171Ponsar-oFlla, 3M Sample Identification Sample Descdption MC-315H MC-317H MC-320H MC-321 H MC-323H MC-326H MC-328H MC-331H NA MC-332H NA MC-333H Intake-P/N Intake-P/dNuplicate Intake-FielBdlankEmpty Oufflow-P/N Oufflow-P/Nduplicate Site1 P/N Site1 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 .46.6 42.3 < 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 refertothe reversesideforour standardformsand conditions.