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Fluoroc Sample
Cr=ntreAnalyticalLaboratories,Inc.
3048 Research Drive Phone: (814)231-8032
StateCoilege,PA16801 Fax:(814)231-1253or (814)231-1560
Ana"-calRepo4
FluorochemicalCharacterizatioonf DrinkingWater Samples
Columbus, GA (W2336) CentreAnalyticalLaboratoryReport No. 023-007F
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
Reques.ter KrisJ.Hansen,Ph.D. 3M EnvironmentalTechnology & SafetyServices
Bldg.2-3E-09 P.O. Box 33331 St Paul,MN 55133-3331
PAGElOF5
Introduction
Resultasrereportfeodrtheanalysoifsa serieosfddnl(iwnagtersamplesreceivebdyCentre Anafykd LaboratoriesI,nc.(Ceritref)rom the3M EnvironmentaLlaboratoryT.he samples were collectefdrom Columbus, GA. The Centrestudynumber assignedtothe projecits023-007.
Specififcluorochemicaclharacterizatiboynliquicdhromatography/tandem mass spectrometry (LC/MSIMS) was requestedforallsamples. A totaolf16 sampleswere receivedforanalysis.
The samples were preparedand analyzedby LC/MS/MS forthefbllomnglisotffluorochemicals:
Table 1:TargetAnalysis
-Compound Name PerfluorooctanSeuffbnate PerfluorooctanSeulfonviamide -Perfluoro6ctanoate
Acronym PFOS
-PFOSA POAA
Data generatedinsupportof thisstudywas generatedaccordingto USEPA Good Laboratory Pracfioes(GLPs). The analyticamlethod used was validatebdy Centre.The validatiopnrotocol and resultasre on filweithCentre.Data presentedhereisthehighestqualitdyataavailablaetthis time.
2 Sample Receipt
The samples were submittedinindividuapllasticontainersand were not preserved. Sixteen individusaalmple containerswere received.Samples were receivedon 02115100.The samp le collectidoanteswere notsupplied.Chain-of-custodiynformatonispresentedinAttachmentA.
3 Holding Times
The analybcalmethod used was validatedagainsta maxknum holdingtime of 14 days. 'The stabiliotfytheanalytesofinteresftorlongerperiodshas notbeen determined.
PAGE20FS
4 Methods-AnaVicaland Preparatory
.4-1 LC/MS/MS
4.1.1 SwnplePreparatifoonrLC/MSIMSAnalysis
Sampleswereinititarlelaytewdfth200uL of250 mg/L sodium thiosulfatseolutiotno remove residualchlorineS,olid'phasee,*acdon (SPE) was used to preparethe samples for LCIMS/MS analysisA. fo"Hliliterportioonfsample was transferred.atCoisSPE carbidge. The cartridgweas firsetlutedwith5 mL of 40% methanolinwatersolutionT.he eluatewas discardedand the SPE column -wasthen elutedwith100% methanol. A 5 mi portionof methanolwas collectefdoranalysisby LC/MS/MS. Thistreatmentresultedinan eight-fold concentratioonfthesamples priortoanalysis.
4.12 Sample Analysisby LCIMSIMS
InHPLC, an aliquootfexftd isinjededand passed througha liquid-phascehromatographic column. Based on the affiniotfythe analytoforthestationarpyhase inthecolumn relativteo theliquimdobile phase,the analyteisretainedfora characteristaimcount of Ume. Following HPLC separationE,SNS providesa rapidand accuratemeans foranalyzinga wide range of organiccompounds, includinfgluorochemicalsE.lectrospraIysgenerallyoperatedatrelatively. mildtemperaturesm;oleculesare Ionizedf,ragmented,and detected.Ionscharacteristoifc known tuorochemicalsareobserved and quantitateadgainststandards.
A HeWett-PackardHPI 100 HPLC system coupledtoa Micromass UltimaMS/MS was used to analyzethe sample extractsA.nalysiswas performed usingselectedreactionmonitoring (SRM). Samples were extractedon 2/24/00and analyzedby MSIMS between 2126100and 2/27/00T.he HPLC and MSIMS methods used foranalysisand instnimentparameterscan be foundInattachmentD.
5 Analysis
5.1 Calibration
A 7-p6intcalibratiocnurvewas analyzedatthe be4inningand end ofthe analyticaslequence forthecompounds of interesTlhe calibratipoonintswere preparedat 0,25, 50, 100,250, 500,and 1000 ng/L (ppt)The response ofthequanttabonionversustheconcentratiownas plottefdoreach point Using linearegressionwithI/xweightingt,heslope,y-intercepatnd correlaticoonefficie(nrt)and coefficieonftdeterminatio(nrjwere determined.A calbmton curveisacceptableW r2:.0.98(5@ > 0.970). .
Calibmtonstandardsare preparedusingthesame SPE procedureused forsamples.
Calibratiocnheck standardswere analyzedperiodical(leyverythreeto fivesample injections) throughoutthe analysissequence. Compliance is obta7inedK the standard analyte concentratonsam within+/-20% ofthe actualvalue.
For theresultrseportedhere,calibraticorniterwieare met
PAGE30F5
5.2 Blanks
Extmcbon blankswere preparedand analyzedwitheveryextracffobnatch of samples. The extractiobnlanksshouldnot have any targetanalytespresentator above theconcentratioonf thelow-leveclalbratonstandard.For thesesamples,theextractiobnlankswere compliant.
Instrumentblanksinthe form ofcleanmethanolsolventwere alsoanalyzedaftereveryhighlevelcalibratisotnandard,and afterknown high4evelsamples. Again,theblanksshouldnot have any targetanalytespresentat or above the low-leveclalibratisotnandard. For the samples presentedhere theinstrumentblanksam compliant
5.3 Surrogates Surrogatespikesarenota component oftheLC/MS/MS analyticamlethod.
5.4 Matrix Spikes Matrixspikeswere preparedfor every sample at a concentrationf 100 ngA- using all compounds ofinterestMatrixspikerecoveriesaregiveninAttachmentC. Fieldspikeswere alsopreparedon severalsamples ata concentrabonof 100 ngIL usingall compounds ofinterestFieldspikerecoveriesare alsogiveninAttachmentC. The fielsdpike resultfsorsample MC-529H gave recoveriesforallcompounds of approximately1000 indicatintghatthissample was possiblyspikedat1000 pptinsteadof100 ppt
5.5 Duplicates Allsamples were analyzedinduplicate.R.esultsaregivenalongwiththesample resultsin AftechmentB.
5.6 Laboratory Control Samples Milliwqaterwas spikedwithallcompound ofinteresatt25.and 250 ng/L.AJIrecoveriesforall compounds were between 70-130% ineach LCS.
5.7 Sample Related Comments Fieldblanksamples consistedof empty wntainers. FortymuliliteomftypeI waterfitered througha hypercarbcartridgweas added to the empty containerand analyzedinthesame manner as theothersamples.
6 Data Summary
Pleasesee Attachment B fora detailedlistinogftheanalyticraelsults.
7 DatalSample Retention
Samples are disposed ofone month afterthe reportisissuedunlessotherwisespecified.AJI electronidcata is archivedon retrievablmedia and hard copy reportsare storedin data foldermsaintainedby Cente.
PAGE40F5
8 Affachments
8.1 - AbchmentA:Chefw@d-CustDdy 82 AttachmentB:Resufts. 8.3 AttachmentC:.MatriSxpikeRecoveries(Fieldand LaboratorSypikes) .8.4 AttachmentD: LC/MSIMS Raw AnalyticaDlata
9 Signatures
/lohn M. FlahertyM,86 IndustriSaelrvicesGroup KevinJ Lloyd,Vic;President
Date ac(-" -oo
Date
OtherLab Members ConMbuOng toData
Enaksha Wickremosinhe Karen Smith
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Gamments:
Cc=ntre Analytical
G*ki\@ksmeL.a.bc)ratories,I,nc.
3048 ResearchDrlve,StateCollegePA 16801 814-231-8032 FAX 814-231-1253
AnalytiRceaslultWs2336ColumbusG,A
3M Sample Identification
MC-515H MC-517H MC-520H MC-521H MC-523H MC-526H MC-528H MC-531H NA MC-532H NA MC-533H
Sample Description
Intake-P/N Intake-P/Nduplicate Intake-FieBlldankEmpty Outnow-P/N Outflow-P/Nduplicate Site1 P/N SiteI P/N duplicate Site2 P/N
Site2 PIN duplicate Site3 P/N Site3 P/N duplicate FieldBlank-P/NEmpty -
PFOS (ng/L)
61.2 53.3 <25 61.5 62.5 57.5 55.7 57.4 55.4 61.7 57.8 < 25
PFOSA (ng/L)
11.7J 10.51
25 14.9J 14.9J 14.9J 11.11 12.6J 13.1J 14.8J 11.5 J
25
J - Compound is.presenbtutbelowthereportinlgimiotf25 ng/L.The resulitsan esbmated value.
POAA (ng/L)
25.5 24.7J < 25 28.8 25.3 26.0 23.8 J 26.3 24.6 J 25.4 24.1 J < 25
Pleaserefertothe reversesideforour standardterms and condition& ,2