Document E5kryg5574jaomagK55LvrmL

Fluoroch Samples. ...... 3048 Research rive Phone: (814)231-8032 Laborator!iEs,Inc. StateCollege,PA 16801 Fax:(814)231-1253 or(814)231-1580 AnaW(;alReport FluorochemicalCharacterizationof DrinkingWater Samples PortSt.Lucie,Fl(W2363) Centre An.alyticalLaboratoryReport No. 023-007E 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 Os J.Hansen,Ph.D. 3M EnvironmentalTechnology & SafetyServices Bldg.2-3E-09 P.O. Box 33331 St.Paul,MN 55133-3331 PAGE 1OF:5 Introduction Resultasrereportfeodrtheanalysoifsa serieosfdrini(wiantgersamplesreceivebdyCentre AnalyticaLlaborato(iesI,nc.(Centre)from the3M EnvironmentalLaboratory.The samples were collectefdrom PortSt.Lucie,Fl.The Centrestudynumber assignedtotheprojectis023-007. Specififcluorochemicaclharacterizatiboynliquicdhromatography/tandem mass spectrometry (LCIMS/MS) was requestedforall'samplesA.totaolf16 samples were receivedforanalysis. The samples were preparedand analyzedby LC/MS/MS forthefollownglisotffluorochemicals: Table 1:TargetAnalysis Compound Name PerfluorooctanSeulfonate PerfluorooctanSeulfonviamide Perfluorooctanoate Acronym PFOS PFOSA POAA Data generatedin supportof 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 submittedinindividuapllasbccontainersand were notpreserved.Sixteen individuaslample containerwsere received.Samples were receivedon 02115/00.The samp)e collectiodnateswere notsupplied.Chain-of-custodiynformatonispresentedinAttachmentA- 3 Holding Times The analyticamlethod used was validatedagainsta maximum holdingtime of 14 days. The stabiliotfythe analytesofinteresftorlongerperiodshas notbeen determined. PAGE20F5 4 Methods-AnalyticalndPreparatoly 4.1 LCIMSIMS 4.1.1 Sample PreparationforLCIMSIMS Analysis Samples were initiatlrleyatedwith200 uL of250 mg/L sodium thiosulfastoelutiotno remove residuaclhlorineS.olidphase extractio(nSPE) was used to preparethe samples for LC/MS/MS analysis.A forty-milliploirtteironofsample was transferretdoa Cia SPE cartridge. The,cartridgweas firsetlutedwith5 mL of40% methanol inwatersolution.The eluatewas discardedand the SPE column was then elutedwith100% methanol. A 5 mi portionof methanolwas collectefdoranalysisby LC/MSIMS. Thistreatmentresultedin an dight-fold concentratioonfthesamples priortoanalysis. 4.1.2 Sample Analysisby LC/MSIMS InHPLC, an aliquotofextractisinjecteadnd passed througha liquid-phascehromatographic column. Based on the affiniotfythe analyteforthe stationarpyhase inthe column relativteo theliquimdobile phase,the analyteisreta7inefdora characteristaimcount of time. Following HPLC separationE,SIMS providesa rapidand accuratemeans foranalyzinga wide range of organiccompounds, includinfgluorochemicalsE.lectrospraiysgenerallyoperatedatrelabvely mildtemperaturesm;oleculesare ionizedf,ragmented,and detected.Ionscharacteristoifc known fluorochemicalasreobservedand quantitateadgainststandards. A HevAett-PackardHP1 100 HPLC system coupledtoa Micromass Ultma MS/MS was used to analyzethe sample extractsA.nalysiswas performed usingselectedreactionmonitoring (SRM). Samples were extractedon 2/25100and analyzedby MS/MS on 2/26100.The HPLC and MSIMS methods used foranalysisand instrumentparameterscan be foundinattachment D. 5 Analysis 5.1 Calibration A 7-pointcalibratiocnurve was analyzed at the beginningand end of the analyticaslequence forthe compounds of interesTthe calibratipoonintswere preparedat 0, 25, 50, 100,250, 500,and 1000 ng/L(ppt)The responseof thequanfitabo!nonversustheconcentrabonwas plottefdoreach pdint.Using linearegressiownithllxweightingt,heslope,y-interceapntd correlaticoonefficie(nrt)and coef5c7ioonftdeterminatio(nr)were determined.A calibration curveisacceptableK r> 0.985 0.970). Calibrabonstandardsare preparedusingthesame SPE procedureused forsamples. Calibraflocnheck standardswere analyzedperiodical(leyverythreetofivesample injeabons) throughoutthe analysissequence. Compliance is obtainedI the standardanalyte concentrationasrewithin+/-20% oftheactualvalue. For theresultsreportedhere,calibraticorniterwieare met. PAGE3 OF5 5.2 Blanks Extractiobnlankswere preparedand analyzedwitheveryextractonbatchof samples. The extractiobnlanksshouldnot have any targetanalytespresentator above the concentratioonf thelow-leveclalibratisotnandard.For thesesamples,theextractiobnlankswere compliant Instrumentblanksintheform ofcleanmethanolsolventwere 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 analyucalmethod. 5.4 MatrixSpikes Matrixspikeswere preparedforevery sample at a concentratioonf 100 ngA- using all compounds ofinterestM.abix spikerecoveriesaregiveninAttachmentC. Fieldspikeswere alsopreparedon severalsamples ata concentratioonf 100 ng/L usingall compounds ofinterestF.ieldspikerecoveriesare alsogiveninAttachmentC. 5.5 Duplicates Allsamples were analyzedinduplicate.Resultsare givenalong%Witthhe sample resultsin AttachmentB. 5.6 LaboratoryControlSamples Milliwqaterwas spikedwithallcompound ofinteresatt25 and 250 ng/L.Allrecoveriesforall compounds were between 70-130% ineach LCS. 5.7 Sample Related Comments Fieldblanksamples consistedof empty containers.Fortymillilitoefrtsype I waterfiltered througha hypercarbcartridgweas added to the empty containerand analyzedinthe same manner as theothersamples. 6 Data Summaty Pleasesee AttachmentB fora detaileldistinogftheanalyucarlesults. 7 DatalSampie Retention Samples are disposedof one month afterthe reportisissuedunlessotherwisespecifiedA.ll electronidcata isarchivedon retrievablmedia and hard copy reportsare storedin data foldersmaintainedby Centre. PAGE4OF5 8 Attachments 8.1 AftachrnentkC-hain-of-CustDdy 8.2 AttachmentB: Resuftsl8.3 AttachmentC: MatrixSpikeRecoveries(Fieladnd LaboratorySpikes) 8.4 AttachmentD: LCIMS/MS Raw AnalyticaDlata 9 Signatures Joh/n/Mflah er-industriSaelrvicesGroup KevinJ Lloyd,Vice President Date --oo Date OtherLab Member s ContribubngtoData Enaksha Wickremesinhe Karen Smith PAGE 5 OFS amn 3M Envii iiientaLlaboratoi-y Chain ofCustody/Reque, Form 38178 - PM Shipping Address: 3M Bldg.2-3E-09 935 Bush Avenue St.PatA.MN 55106 Telephone: SarMle Receiving-(.651)7784945 Alternate:(651)T78-6753 FAX: (651)7784176 ProjecItD/ProjeNcotme Template ProjectLead Dept:.#(main) ContactName vi Company t: MailingAddress 0 C0L City,State,Zip t- W. Telephone # P(9 i FAX# SpecialInstructionsand/or SpecificRegulatory Requirements: (meffiod,limito(detedion,repoilVg mfts,etc@) eg -)rLaboratoryAnalytical 17133 41A @-I)yi/illiLqA(tgf FiAl RepbrtDue Date InternaDlue Date Class/Job/Prject t9ol oa:!,,S-cNpa@ Date Available Date Due ContractLab L Preservatives: Comp 0 In A,)11?) L (D E 0 z U) 0 0 zc x 3: > z o -0 0 Item ClientSample Identification 3M Date Time Matrix/ LIMS# Sampled Sampled Media Enter the nLKnber ofcontainersof each (E 1- 2. *1 L@ Len tA -PIA) 47,u =i@i e-14&.I" A@@ /UI,4L04:;f---p4f- 3. -VIICAI& ;V-( 4- U 41A) (b@4 . 6. M t Cid-@ipt-jPJA) 7. g. lo. Collectedby (print): Item Relinquished by/Afriliation Collectoes signature: Ti ..sh*I-P* eceived b Mlintio Sample Condition Upon Receipt: 0 Acceptable 0 Other: c Temperature: 0 Received on Ice OtherA*SodeledCoCs: 1-1 t LVI 1-1I'L%. 1-iI*LL#i-71*L-5,nl-lgc-opietso; 13 q_ Page Of Original- Accompanying Samples Comments: Last Page - Originator See Reverse Side forInsimclions 3M Envii Form 38778 - PWO Shipping Address: 3M BMg.2-3E-09 935 Bush Avenue 06 St.Paul.MN 55 iiientaLlaboratory Telephone: Sample Receiving:(651)7794949 Alternate:(651)718-41753 FAX: (GSI)778-6176 Contact Name Company @A@ic-i l)m8-(Q 'tr: ii MailingAddress icf 01 0 CL tu City.State,Zip 5@. w ITelephone 9@ SpeciniInstructionsandfor Speclnc Regulatory Requirements: (me0iod,limitofdetectionr,eportinmgRs. etc.) -0(9 ppy-@ Item f ClientSample ldentirication Chain ofCustody /Reque..,),r.LaboratoryAnalytical 17134 ProjectID/ProjectNime Template # ProjectLead Dept.# (main) 41r)"e 4 L4;L.)I ynL)& i)f'7)flkIIAA4 Fi?tARlepbrt Due Date internalD e Date C'nceflob(Prlect (DO@CS-:5 Date Available P 0 &@CZ 7?@ 1 FAX Date Due ContractLab Preservatives: Comple E o z 0U) 0 > 0 z C) zii(c0 i 3M Date Time Matrix/ LIMS# Sampled Sampled Media Enterthe rk)mberof containersofeach (Ent 2. - W L to aLI)i -f2) -EV i -EleA 3. yn C -Lt)-50P Spi 4. --PIA AIV 6. 7. 8. 9. 10. --------------------- Collectedby (print): A //A Item Relinqulshedby/Afrillation Tir@e' Collector'ssign lure: Date Shipped Vla: Received by/AMIlation 0 Sample ConditionUpon Receipt: 0 Acceptable 0 Other: Temperature: Ic 4DReceived on Ice OllierAss@iatedCoCs: %-)ILVI 1-1ILI, I-)I'LLA1-) 014 Copie to: Page -I-R Of Original-Accompanying Samples Cornments: Last Page - Originator See Reverse Side forinstructions Cc=ntrc=Analytical Laborator!Fs, Inc. 3048 Research Drive,StateCollegePA 16801 814-231-8032 FAX 814-231-1253 AnalyticRaelsultWs2363PortSt.LucieF,l 3M Sample Identification MC-61 5H MC-617H MC-620H MC-621 H MC-623H MC-626H MC-628H MC-631 H NA MC-632H NA MC-633H Sample Description lntake@P/N Intake-P/dNuplicate Intake-FieBlldank Empty Oufflow-P/N Oufflow-PINduplicate Site1 P/N SiteI PIN duplicate Site2 P/N Site2 P/N duplicate Site3 P/N Site3 P/N duplicate FieldBlank-P/NEmpty PFOS (na) <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 Pleaserefertothereversesideforour standardtei7nsand conditions.