Document 70mMV972YZYNrznR0nv3mNoKa

CentreAnalyticaLlaboratoriesI,nc. 3048ResearchDrive Phone: (814)231-8032 StateCollege,PA 16801 Fax:(814)231-1253 or (814)231-1580 Ana calReport Fluorochemical Characterization of Surface Water Samples Pensacola, Fi (W2176) Centre AnalyticalLaboratory Report No. 023-014C Testing Laboratory Centre AnalyticaLlaboratory,Inc. 3048 Research Drive State College,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 Environmental Technology & Safety Services Bldg. 2-3E-09 P.O. Box 33331 St.Paul, MN 55133-3331 PAGELOFS Introduction Resultasrereportefdortheanalysiosfa serieosfsurfacweatersamplesreceivebdyCentre AnalyticaLlaboratoriesI,nc.(Centre)from the3M EnvironmentalLaboratory.The samples were collectefdrom Pensacola,Fl.The Centre studynumber assignedtothe projectis023-014. Specificfluorochemicaclharacterizatiboyn liquicdhromatography / tandem mass spectrometry (LC/MS/MS) was requestedforallsamples. A totalof 8 samples were receivedforanalysis. The samples were prepared and analyzedby LC/MS/MS forthe followinlgisotf fluorochemicals: Table 1:TargetAnalysis Comr)ound Name PerfluorooctaneSulfonate PerfluorooctaneSulfonviamide Perfluorooctanoate Acronvm PFOS PFOSA P()I^o - The analyticamlethod used was validatebdy Centre. The validatiopnrotocoland resultsare on filweithCentre. Data presentedhere isthe highestqualitdyata availablaet thistime. 2 Sample Receipt The samples were submittedin individuapllasticontainersand were not preserved. Sixteen individuaslample containerswere received.Samples were receivedon 05/03/00.The sample collectidoanteswere notsuppliedC.hain-of-custoidnyformabonispresentedinAttachmentA. 3 Holding Times The analyticalmethod used was validatedagainst a maxiffium holding time of 14 days. The stabiliotfythe analytesof interesftorlongerperiodshas notbeen determined. PAGE 2 OF 5 4 Methods-AnalyticaanldPreparatory 4.1 LC/MS/MS 4.1.1 SamplePreparatiofnorLC/MSIMSAnalysis Sampleswereinitiatlrleyatewdith200 uL of250mg/Lsodiumthiosulfsaotleutiotnoremove residualchlorineS.olidphase extractio(nSPE) was used to prepare the samples for LC/MS/MS analysis.A forty-milliploirtteironof sample was transferretdoa Cla SPE cartridge. The cartridgweas firsetlutedwith5 mL of 40% methanol inwatersolution.The eluatewas discardedand the SPE column was then elutedwith 100% methanol. A 5 mi portionof methanol was collectedforanalysisby LC/MS/MS. This treatmentresultedinan eight-fold concentratioonfthe samples priortoanalysis. 4.1.2 Sample Analysis by LCIMS/MS In HPLC, an aliquotof extractisinjectedand passed through a liquid-phascehromatographic column. Based on theaffirtofftytheanalyteforthe stationarpyhase inthecolumn relativteo theliquimdobile phase,the analyteisretainedfora charactehstiacmount of time. Following HPLC separationE,S/MS providesa rapidand accuratemeant foranalyzinga wide range of organic compounds, includingfluorochemicalsE.lectrosprayisgenerallyoperatedat relatively mild temperatures;molecules are ionizedf,ragmented,and detected. Ionscharactebstiocf known fluorochemicalsareobserved and quantitateadgainststandards. A HeWett-Packard HP1 100 HPLC system coupled toa Micromass UlfimaMSIMS was used to analyze the sample extractsA.nalysiswas performed using selectedreactionmonitoring (SRM). Samples were extractedon 5/17/00and analyzed by MS/MS on 5/19/00.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 beginning and end of the analyticalsequence forthe compounds of interestT.he calibratiopnointswere prepared at 0,25, 50, 100,250, 500, and 1000 ng/L (ppt)The response of the quantitatioinonversusthe concentratiownas plottedforeach point.Using linearregressionwith 1/xweighting,theslope,y-intercepatnd correlatiocnoefficien(tr)and coefficieonft determinatio(nr2)were determined.A calibration curve isacceptableifr > 0.985 (@ > 0.970). Calibratiosntandardsare prepared usingthesame SPE procedureused forsamples. Calibratiocnheck standardswere analyzedpedodicall(yeverythreetofivesample injections) throughoutthe analysissequence. Compliance is obtainedif the standardanalyte concentrationsarewithin+/-20% of the actualvalue. For the resultsreportedhere,calibratiocnriteriwaere met. PAGE30F5 5.2 Blanks ExtractbiloannkwsereprepareadndanalyzewdithevereyxtractbiaotnchofsamplesT.he extractiobnlanksshouldnothave any targetanalytespresentatorabove theconcentrabonof thelow-leveclalibratisotnandard.Forthese samples,theextractiobnlankswere compliant. Instrumentblanksintheform ofcleanmethanol solventwere alsoanalyzedaftereveryhighlevelcalibrabosntandard,and afterknown high-leveslamples. Again,the blanksshouldnot have any targetanalytespresentat or above the low-leveclalibrabosntandard.For the samples presentedheretheinstrumenbtlanksarecompliant. 5.3 Surrogates Surrogatespikesare nota component oftheLC/MS/MS analyticamlethod. 5.4 Matrix Spikes Matrixspikeswere preparedforeveryfieldsample (excludingblanks)at a concentratioonf 100 ng/L usingallcompounds ofinterestM.atrixspikerecoveriesaregiveninAttachmentC. Alllaboratormyatrixspikesshowed recoverieosfallcompounds between 70-130%. Fieldspikeswere preparedon sample MC-301H at a concentratioonf 100 ng/L usingall compounds ofinterestF.ieldspikerecoveriesarealsogiveninAttachmentC. Allfielsdpikes showed recoverieosfallcompounds between 70-130%. 5.5 Duplicates Adifieldsamples (excludinbglanks)were analyzedinduplicate.Resultsare givenalongwith thesample resultisnAttachmentB. 5.6 Laboratory Control Samples Milliwqaterwas spikedwithallcompound ofinteresatt25 and 250 ng/L.Allrecoveriesforall compounds were between 70-130% ineach LCS. Recoveriesare givenwiththe raw datain AttachmentD. 5.7 Sample Related Comments Fieldblanksamples consistedof empty containers.FortymillilitoefrtsypeIwater filtered througha hypercarbcartridgweas added to the empty containerand analyzedinthe same manner as theothersamples. 6 Data Summary Please see AttachmentB fora detaileldistinogftheanalyticraelsults. 7 DatalSample Retention Samples are disposedofone month afterthe reportisissuedunlessotherwisespecifiedA.ll electronidcata isarchivedon retrievabmledia and hard copy reportsare storedin data foldersmaintainedby Centre. PAGE4 OF5 8 Attachments 8.1 AttachmentA Chain-of-Custody 8.2 Attachment B:Results. 8.3 AttachmentC: Mabix SpikeRecovehes (Fieldand LaboratorySpikes) 8.4 Attachment D: LC/MS/MS Raw AnalyticaDlata 9 Signatures ohn M. ons Manager Date Kevin J Lloyd,Vice President Date Other Lab Members Contributintgo Data Enaksha Wickremesinhe Karen Smith David Bell PAGE50F=5 ANALYTICALREPORT- Cc=ntrc=An;i3lytical Laboratories, Inc. 3048ResearchDrive,StateCollegePA 16801 .814-231-8032 FAX 814-231-1253 AnalyticaRlesultsW2176 PensacolaF,l 3M Sample Identifleation Sample Description PFOS (ng/L) MC-301 H MC-303H MC-306H NA MC-307H NA MC-308H MC-384H NA Site1 P/N SurfaceWater SiteI P/N SurfaceWater Duplicate Site2 P/N SurfaceWater Site2 PIN SurfaceWater Duplicate Site3 PIN SurfaceWater Site3 PIN SurfaceWater Dupiciate FieldBlank-PIN Empty QuietSurface Water Quiet SurfaceWater Duplicate 20.8 J 19.0 1 28.5 22.8J 20.9J 18.5 1 < 25 15.7 1 17.4 J J - Compound ispresent,but below the reportinglimiotf 25 ng/L The resultisan estimatedvalue. PFOSA (ng/L) < 25 < 25 < 25 < 25 -c25 < 25 < 25 < 25 < 25 Method DetectionUmits are approximately2.5 ngIL forPFOS and PFOSA and 7.5 ngIL forPOAA- POAA (ng/L) < 25 < 25 < 25 < 25 < 25 < 25 < 25 < 25 < 25 Please refer to the reverse side for our standard terms and conditions. Lo L4z k6@."e Quietwater, Mchigan Ave. at 4 173 Mobile Highway -b-Z .............. Avery Street Pumping Statiio Cinfluent) 727 TArg w IV-K a(, " ip Texar Bayou Site #3 Texar Bayou Site iLexar ilsayou Site #1 7 !92 29 rrft ECUA-Mam StreetPOIW (emuent) 019m@ftpQuestoormlrom:olgggGD'T. Inc Additional sampling sites shown on north map Environmental Sampling Sitesand Supply Chain FacilitiefsorPensacola,FL ug e Alternativesample 184 siteatTimber Creek near PerdidoIan did[ i nLL 186 H el9;t, Rd T- 0 232 - ---------- 297 Pin;-F-or-4,s 95 .-B d 742 3@i 291 3 173 296 *low kbpql -metDom '=n;o.;019 DT. Inc Additionalsampling sites sbown on south map i Environmental Sampling Sitesand Supply Chain FacilitieNsorth--ofPensacola,FL