Document N22ga69vLKZ2VQgQ5YBz4oEwg

ntpeAnalyticaLlabopatopieIsn,c. 3048ResearchDrive Phone: (814)231-8032 StateCollege,PA 16801 Fax: (814)231-1253 or (814)231-1580 Ana@fi(;Raelport Fluorochemical Characterizationof Surface Water Samples Decatur,Alabama (Wl979) Centre AnalyticalLaboratory Report No. 023-007B Testing Laboratory 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 KrisJ.Hansen, Ph.D. 3M EnvironmentalTechnology & SafetyServices Bldg.2-3E-09 P.O. Box 33331 St.Paul,MN 55133-3331 PAGE I OF5 Introduction Resultasrereportefdortheanalysiosfa serieosfsurfacweatersamplesreceivebdy Centre AnalyticaLlaboratoriesI,nc.(Centre)from the3M EnvironmentalLaboratory.The samples were collectefdrom Decatur,Alabama. The Centre studynumber assigned tothe projectis023-014. Specificfluorochemicaclharacterizatiboyn liquidchromatography / tandem mass spectrometry (LC/MS/MS) was requestedforallsamples. A totalof9 samples were receivedforanalysis. The samples were preparedand analyzedby LC/MS/MS forthefollowinglisotf fluorochemicals: Table 1:TargetAnalysis COMDound Name PerfluorooctanSeulfonate PerfluorooctanSeulfonviamide Perfluorooctanoate Acronvm PFOS PFOSA POAA The analyticamlethod used was validatedby Centre. The validatiopnrotocoland resultsare on filweithCentre. Data presentedhere isthe highestqualitdyata availableatthistime. 2 Sample Receipt The samples were submittedin individuapllasticcontainersand were not preserved. Nine individuaslample containerwsere received.Sample MC-202H was not analyzedas per client request(.E-maiclommunicatiofnromKiisHansenon 5/16/00S)a.mpleswere receiveodn 05/03/00. The sample collectiodnates were not supplied. Chain-of-custodyinformatoins presentedinAttachmentA- 3 Holding Times The analyticamlethod used was validatedagainsta maximum holdingbme of 14 days. The stabiliotftyheanalytesofinteresftorlongerpedods has notbeen determined. PAGE20PS 4 Methods-AnalyticaanldPreparatory 4.1 LC/MS/MS 4.1.1 SamplePreparatiofnorLC/MS/MSAnalysis Sampleswereinititarlelaytewdith200 uL of250 mg/Lsodiumthiosulfsaotleutiotnoremove residualchlorineS.olidphase extractio(nSPE) was used to prepare the samples for LC/MS/MS analysis.A forty-millilpiotretrionof sample was transferretdo a C,8 SPE cartridge. The cartridgweas firsetlutedwith5 mL of 40% methanol inwater solution.The eluatewas discardedand the SPE column was then elutedwith 100% methanol. A 5 ml portionof methanol was collectefdoranalysisby LC/MS/MS. This treatmentresultedinan eight-fold concentratioonfthesamples priortoanalysis. 4.1.2 Sample Analysis by LCIMSIMS In HPLC, an aliquotof extractisinjectedand passed through a liquid-phascehromatographic column. Based on theaffiniotfythe analyteforthestationarpyhase inthe column relativteo theliquimdobile phase,the anave isretainedfora characteristaimcount ofbme. FollovAng HPLC separationE,S/MS providesa rapidand accuratemeans foranalyzinga wide range of organiccompounds, includingfluorochemicalsE.lectrosprayisgenerallyoperated atrelatively mildtemperatures;molecules are ionized,fragmented,and detected. Ions characteristoifc known fluorochemicalasre observed and quantitatedagainststandards. A Hewlett-PackardHP1 100 HPLC system coupled to a Micromass UltimaMS/MS was used to analyzethe sample extractsA.nalysiswas performed using selectedreactionmonitoring (SRM). Samples were extractedon 5/16/00and analyzed by MS/MS between 5/19/00and 5/20/00.The HPLC and MS/MS methods used foranalysisand instrumentparameters can be found inattachmentD. 5 Analysis 5.1 Calibration A 7-pointcalibratiocnurve was analyzed at the beginning-and end of the analyticaslequence forthe compounds of interestT.he calibratiopnointswere prepared at 0, 25, 50, 100,250, 500, and 1000 ng/L (ppt)The response of the quanfitabonionversus the concentratiownas plottedforeach point.Using linearregressionwith 1/xw(e@)ghfingt,he slope,y-intercepatnd correlatiocnoefficien(tr)and coefficienotf determination were determined. A calibration curveisacceptableifr> 0.985 (@ > 0.970). Calibratiosntandardsare preparedusingthe same SPE procedure used forsamples. Calibratiocnheck standardswere analyzedpe@@ically (everythreetofivesample injections) throughoutthe analysissequence. Compliance is obtained if the standard analyte concentrationsarewithin+/-20% of theactualvalue. Forthe resultsreportedhere,calibratiocnriteriwaere met. PAGE30F5 5.2 Blanks Extradonblankswere preparedand analyzedwitheveryextractiobnatchofsamples.The extractiobnlanksshouldnothave any targetanalytespresentatorabove theconcentrationf thelow-leveclalibratisotnandard.Forthesesamples,theextractiobnlankswere compliant. Instrumenbtlanksintheform ofcleanmethanolsolventwere alsoanalyzedaftereveryhighlevelcalibratisotnandarda,nd afterknown high-leveslamples. Again,theblanksshouldnot have any targetanalytespresentat or above the low-leveclalibratisotnandard.For the samplespresentedheretheinstrumenbtlanksarecompliant. 5.3 Surrogates Surrogatespikesarenota component oftheLC/MS/MS analyticmaelthod. 5.4 MatrixSpikes Matrixspikeswere preparedforeveryfielsdample (excludinbglanks)ata concentrationf 100 ng/Lusingallcompounds ofinterestM.atrixspikerecoverieasregiveninAttachmentC. Alllaboratormyatrixspikesshowed recoverieosfallcompounds between70-130% Fieldspikeswere preparedon sample MC-201H at a concentrationf 100 ng/Lusingall compounds ofinterestF.ieldspikerecoverieasrealsogivenihAttachmentC. PFOS showed highrecoveryint.hefielsdpike.Allothercompounds showed recoveriebsetween70-130%. 5.5 Duplicates Allfielsdamples(excludibnlganksw)ereanalyzeidnduplicatRee.sultasregivenalongwith thesample resultisnAttachmentB. 5.6 LaboratoryControlSamples Milliwqaterwas spikedwithallcompound ofinteresatt25 and 250 ng/L.Allrecoveriefsorall compounds were between70-130% ineach LCS. Recoveriesaregivenwiththeraw datain AttachmentD. 5.7 Sample Related Comments Fieldblanksamplesconsisteodf empty containers.FortymillilitoefrtsypeIwaterfiltered througha hypercarbcartridgweas added totheempty containearnd analyzedinthesame manner as theothersamples. 6 Data Summaty PleaseseeAttachmentB fora detaileldistinogftheanalyticraelsults. 7 DatalSample Retention Samples aredisposedof one month afterthereportisissuedunlessotherwisespecifiedA.ll electronidcataisarchivedon retrievabmleedia and hardcopy reportsarestoredindata foldermsaintainedby Centre. PAGE40F5 8 Attachments 8.1 AttachmentA- Chain-of-Custody 8.2 AttachmentB:Results. 8.3 AttachmentC: MatrixSpikeRecoveries(Fieladnd LaboratorySpikes) 8.4 AttachmentD: LC/MS/MS Raw AnalyticaDlata 9 Signatures Jo*hngffMF-l.aheftqanagef-operations manager . 4 ./P@ KeviJnLlyrd,Vi@lPeresident Date @q2LA:ti2-cco Date OtherLab Members ContribubngtoData Enaksha Wickremesinhe Karen Smith David Bell PAGE50F5 Cc=ntre Analytical LaboratoriFs. Inc. 3048 Research Drive,State College PA 16801 814-231-8032 FAX 814-231-1253 AnalyticRaelsultWs1979DecatuArl,abama 3M Sample Identification Sample Description PFOS (ng/L) PFOSA (ngIL) MC-201 H MC-203H MC-206H NA MC-207H NA MC-208H MC-284H NA SiteI P/N SurfaceWater Site1 P/N SurfaceWater Duplicate Site2 P/N SurfaceWater Site2 P/N SurfaceWater Duplicate Site3 P/N SurfaceWater Site3 P/N SurfaceWater Duplicate FieldBlankP/N Empty QuietP/N SurfaceWater QuietP/N SurfaceWater Duplicate 23.1J 8.3 J 14.5J 22.0 J < 25 < 25 < 25 108 114 < 25 < 25 < 25 < 25 < 25 < 25 < 25 18.9J 18.1J i -Compound ispresent,butbelow thereportinlgimiotf25 ng/L.The resulitsan estimatedvalue. Method DetectionLimitasre approximatel2y.5ng/LforPFOS and PFOSA and 7.5hg/LforPOAA- POAA (ng/L) 9.2J < 25 < 25 11.11 < 25 < 25 < 25 63.1 57.3 Please referto the reverse side forour standard terms and conditions. Dimction of riverflow @;@j. Deca r Landfill 0 F3 M LIWTP @j ----- ...... -- -------- LIU LI,9P-@ e y Decatu POTIWV emuent Riverwalk 45" Marina Site#2 Riverwalk 2rlIM2 Site#1 Decatur W2ter PliLnt rwalk manna low FlintCmek quietw ter Environmental Sampling SitesforDecatur,AL