Document M4EVOGm0Jka704zVOoBgqMEZ9

BACK TO MAIN I Analysis of PFOS in Test Organisms from the 96-Hour Static Acute Toxicity Test with the Freshwater Mussel Laboratory Report No. W2078 FACT Project No. FACT-TOX132 Testing Laboratory 3M EnvironmentalTechnology & Safety Services 3M Environmental Laboratory FluorineAnalytical ChemistryTeam (F'ACT) 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Laboratory Contact Kris Hansen, Ph.D. Bldg. 2-3509 P.O.Box 3331 St. Paul, MN 55133-3331 Phone: (651)778-6018 FAX: (651) 778-6176 Requester Susan Beach 3M Company Environmental Technology & Safety Services Bldg 2-3E-09 . St. Paul, MN 55133 Page I of6 BACK TO MAIN 3M ENVIRONMENTAL LABORATORY ANALYTICAL REPORTNO. FACT-TOX132 This studyW I designed to quantitativelyassessperlluorooctanesulfonatePFOS, C8F17S03-, CAS# 279539-3) levels in fkhwater mussels after a 96hour exposure. Details of exposure conditions, clinical observationsand othertoxicity datawere generated by the m-life testing facility(WildlifeInternational)and are not includedin thisreport.Analyticalresults of the test animalsrepresenting5 dosagegroups and 1 controlp u p arepresentedhere. In each dose group,there were 20 mussels exposed to PFOS. Within each group,10musselswere exposed in one of two chambers labeled A andB. Six of the twenty test animalsper group (3 from chamber A and 3 h m chamber B)were analyzed forPFOS. PFOSwas idmtSed mall test animals analyzed,and most of the matrixmussels and control mussels. Matrix mussels were sacrificedupon arrival at the in-life testing facility,prior to the start of the study. control mussels were housed near the test animalsin water to which no PFOSwas added PFOS levelswere determinedto increasewith each mcrease mdose leveL Refer to attachment D forresults ofindividualmusselanalysis. - Based on matrix spike analysis studies, data genemted in support of this study should be considered to be d-quantitaative with a margin of error of +/-35%. No data was collectedfor d y t e s other thanPFOS. Althoughrigomus qualityumtrolmeasures and 3M EnvimnmentalLaboratoryStandardOperating Procedures were followed, the acquisition of this data was not necessarily collected according to applicable Good Laboratory Practices. Data presented here is the highest quality data available at this time. In-pbase testingwas conductedaccordingto applicableGood Laboratory Practices. The conductof the m-life phase is the sole responsibilityof Wildlife InternationalLfd. See attachmentC for thein-lifeprotocoL Mussel Specimens were collected on 06/01/99 and senttothe EnviroxrmentalLaboratory on 06/07/99. The 3M Environmental Lab received, on 06/08/99, a total of 105 frozen mussel specimens. Twenty specimens were firomgroup 1,20fromgroup2,20 fiomgroup3,20 hmgroup 4,18 hmgroup 5,2 fromgroup6, and 5 matrixmussels. Upon specimenreceipt, a chain of custodywas initiatedand a copy of thisformcan be found in Attachment C. There are no holding time criteria associated with this analysis. Preparatory and Analytical Methods FACT-M-1.1, Extraction of PotassiumPerfEuorooctanesulfonateor Wer FluomchemicalCompounds fromLiver for AnalysisUsing HPLGElectrospray/Ivass SpectrometrySpectromtrywith thefollowing exception:Due to the timeconstraintsandlack of controlmaterial,standard c u ~ ews ere preparedm methanol insteadof h m musseltissue. PFOS lot 171was used as refereke material ETS-8-6.0, Exhction of PotassiumPerfluomomnesulfonateor Other Fluomhemid Compmds from Liver for P d y s i s Using HPLC-Electrosprayh4assSpectrometry with thefollowingercepfion: PageZof6 BACK TO MAIN 3M ENVIRONMENTAL LABORA TORY ANALYTICAL REPORTNO. FACT-TOXl32 Due to the time constraints and lack of control material, standard curves were prepared in methanol instead of fiom mussel tissue. PFOS lot 171 was used as reference material. FACT-M-2..1,Analysis of Fluomchemicals in Liver Extracts Using HPLC-Electrospray/Mass Spectrometry ETS-8-7.0, .Analysisof PotassiumPerfluomoctanedonateor Other Fluorochemids in Liver Extracts Using HF'LC-E1eclrosprayMas.s Spectrometry The characterizationof the reference material (PFOS, lot #171), with respect to purity, stability,and homogeneity,was not complete on the date thisreport was issued. Once the characterizationis coelete, a copy of the report will on file in the 3M EnvironmentalLab archives. Sample preparation-ion-pairingextraction On July 01,1999,l .O mL of each mussel homogenate (six specimensper group) were extractedfollowing method FACT-M-1.1 which utilizes an ion pairing reagent [tetrabutylammoniumhydrogen sulfite (TBA)] in a pHantrolled environment The cationicreagent selectively targets anionic fluorochemical. Once the anion-TBA pair is formed,the analyte is transferred into a non-polarorganic solvent,dried, and reconstituted m 1.O mL.of methanol forMS analysis. Samples of the test matrix fiom Group 4 animals were spiked with PFOS and extracted according to FACT-M-1.1 on July 01,1999. Samplesof test matrix fromthe control group were spiked and extracted following ETS-8-6.0 on July 22,1999 and August 2,1999. Although two different extmctionmethod numbers were used for these specimens, the extractions were performed ;isdesmkd in method ETS-8-6.0. For example, the July 01,1999 extraction followingmethod FACT-M- 1.1used methyl tertbutyl ether solvent as statedin method ETS-8-6.0, instead of ethyl acetate as stated in FACT-M-1.1. HPLC/ESMSMS: for detailed quanitative work On July 07,1999 the mussel extractswere analyzed using tandemelectcospraymass spectrometry (ESMSMS:),analytical system``Soup020199"according to FACT-M-2.1, with the followingexception. Because large amounts of blank matrix were not available, analyte levels were evaluated versus a solvent curve insteiid of versus a &we extractedh m matrix. Extra matrix spike studieswere conductedin order to validate this action. Results of these matrix spike studies were good (extraction efficiency greater than 65%), therefore, these sample results are considered to be acceptable. In this analysis,a 10 pL aliquot of extract is injected and passed througha reversephase liquid chromatographiccolumu Based on the f i t y of the aualytefor the stationaryphase in the cohmrn relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. For example, in a standard solutionPFOS may elute at 5.0 minutes. Retention timesbetween a standardPFOS solution and the d y t e extractedh m mussel in thisanalysiswere matched on the HPLC system to within2%. Following HPLC separation, ESMSMS provides a rapid and accurate means for analyzing a wide range of organic compounds,including fluomchemids. Electrospray, an ionizationtechniqueused primarilyfor detection of molecular ions, is generally operated at relatively mild tempera-. Molecules are ionized, and a primary ion, characteristic of the adyte, is selected. This ion is bombarded with high-energy gas; subsequent collisions create smaller secondary ionic hgmentsunique to the primary ion, which are detected For example,for PFOS(Cp,,S03] analysis, ion499 is selectedas the characteristicprhaiy ion. ?his ion is hgmented into other ions such as 99 amu (correspondingto FSO33, and 230 amu (C&Sa]. Each of these secondary fragmentsis detectedand canbe used to differentiatePFOS fhm other compounds that Page3of6 BACK TO MAIN 3M ENVIRONMENTAL LABORATORY ANALYTICAL REPORTNO. FACT-TOXI32 might have the same characten.stic 499 amu primary ion, but different chemical compositions and secondary ion fiagmentatim patterns. After analysis on July 07,1999, it was determined that dilutions were required for extracts firom group 2-6 test animals. Dilutions were prepared and analyzed on July 09,1999 using analyt~caslystem "Madeline 040198" according to methodFACT-M-2.1. The diluted samples were withinthe caliirationrange. 5.1 Calibration For quantitative determinations, a mid-level, unextracted methanol calibration curve vedication (CCV) standardwas analyzedevery 5 to 10samplesto monitor instnrmentaldrift. calibrationw e verification standards;irecompliant if instrumentalresponse is within +/- 30% of theexpectedvalue. In this study, all ccv stan<lards were compliant. Quantitationofthe target d y t & is based on linearregression analysis (weighted ILK)of two curves prepared in methanol, bracketing each group of samples. Quantitation of each analyte is based on the response of one or more specific daughter ions using the multiple response-monitoring mode of the instrunlent. Analyseson OWOU99 and08/03/99 containedpoor calil~ratimcurve response; these data were not reported 5.2 Blanks Four extractionblanks, utilizingwater as surrogate matrix, were extracted with eachbatch of samples. Blanks are compliant ifno target analyte is detected above the limit of quautitation for a specific analyte. In this study, all blanks were compliant 5.3 Surrogates Tetra-hydro perfluorooctane sulfonate is used as a surrogate in this analysis. Surrogate response is monitored to confirmgross instrumentalfailure, ifnecessaxy. Surrogate response results were acceptable. 5.4 Matrix Spikes Four matrix spikes at 100ppb and four matrix spikes at 1.Oppm were extracted and andyed u t h h g all target adytes for which quantitativedata is presented Samplesof the test matrixh m Group 4 animals were spiked with PFOS and extracted according to FACT-M-1.1 on July 01,1999. Spikerecoverieswere erratic, probably due to exceptionally high endogenous levels of PFOS, the matrix spike studieswere repeated on July 22,1999 and August 02,1999. Spikerecoveries h m the July 22,1999 extraction at 100ppb and 1.0ppm were within analytical acceptance criteria of 65130%. As the matrix spike data collected July 22,1999 was acceptable, data collected b m analyses of the August 2,1999 extraction were not included m thisreport 5.5 Laboratory Control Samples Laboratory control Samplesarenot a component of thisstudy. 5.6 Sample Related Comments The levelof PFOS msamplesof mussel tissue was determinedby comparison with a standardcurve prepared msolvent Typically,PFOS levels are determinedversusa curve extractedb m tissue inorder to more acamteIyassess any matrix effects. ~ x t r ama& spike studies were conducted morder to validate thisaction. Resultsof thesematrix spikestudieswere good (extraction efficiencygreater than 65%), therefore these sample results are considered to be acceptable. Page4of6 BACK TO MAIN I 3M ENVIRONMENTAL LABORATORY ANALYl7CAL REPORTNO. FACT-TOXI32 I 1 PFOS was detected m the test animals analyzed.Refer to Table 1for a summary of averagePFOS levels in mussels by dose group. Please refer to the attached spreadsheetsfor individual test animalresults. I Assuming spike recovery studies form a suitable indication of endogenous analyte recovery, data are quantitiativeto f35 %. The validity of thisassumptionhas not beenverified by other techniques. 1 The estimated limit of quantitation (LOQ) for PFOS is 25 ppb (ng/mL) for the July 09,1999 analysis and 5.0 ppb (ng/xnL) for the remaining analyses (July 07,1999 and August 03,1999). 1 The LOD and LOQ values are stated as ng/mL since the extracts were evaluated versus a solvent curve, not an extracted mussel m e . I This report reflectsthe most accu-rate data availableat thistime. Table 1 Analysis Resdts-Mussel I Group/ Average Conc. I Dosage PFOS in Mussel 0.0808 A: <O.O174pg/g Cuntrol I I I Group3 I 12 ppm B: 0.0502 A: 3.41 B: 3.96 A: 4.83 B: 5.61 Group 4 20 Ppm 1 Group 5 41 PPm 1 Group6 79 ppm A: 8.07 B: 6.58 A: 11.2 B: 12.5 A: 91.2 B: 86.4 I I I 1 Matrix =Mussel specimenswhich were sacrificed upon arrival of all mussel specimensat the in-life testing facility and not exposed to control or dosed water. I A =Specimensstored mChamberA. B =Specimens stored in Chamber B. 1 Spechens and exfnctswill be retained for a minimumof one year for hture evaluation, ifnecessary. 1 I PageSof6 I x i" .'Lc I BACK TO MAIN 3M ENVIRONMENTALLABORATORY ANALYITCAL REPORTNO. FACT-TOX132 8.1 Attachment A Analytical Report Addendum 1 8.2 Attachment B: Wildlife International Protocol 8.3 Attachment C: Extraction and Analytical Methods 8.4 AttachmentD Chain of custody form(s) 8.5 Attachment E: Complete Analytical Results 8.6 Attachment F: Extraction and Analysis Wonnation , 06/dY/H Date 1 I II I I I 1 c Page60f6 BACK TO MAIN 3MENVIRONMENXL LABORATORY ANALY'nCAL REPORTNO. FACT-TOXl32 AnalyticalReport Analysis of PFOS in Test Organisms from the 96-Hour Static Acute T-oxicity Test with the Freshwater Mussel Laboratory Report.No.W2078 FACT Project No.FACT-TOX132 Attachment A Analytical Report Addendum 1 BACK TO MAIN . 3MENVIRONMENTAL LABORATORY ANALWICXL REPORTNO. FACT-TOXI32 ADDENDUM I AnatyticalRqortAddendum 1 Analysis of PFOS in Test Organisms from the 96-Hour StaticAcute T-oxicity Test with the Freshwater Mussel Laboratory Report No. W2078 FACT Project No. FACT-TOX132 Testing Laboratory 3M Environmental Technology8z Safety Services 3M Environmental Laboratory Fluorine Analytical Chemistry Team (FACT) 2-3E-09 935 Bush Avenue St. Paul, MN 55106 Laboratory Contact Kris Hansen, PhD. Bldg. 2-3E-09 P.O. Box 3331 St. Paul, MN 55133-3331 Phone: (651)778-6018 FAX: (651) 778-6176 Fagelof4 BACK TO MAIN 3M ENVIRONMENTAL LABORATORY ANALYTICAL REPORTNO. FACT-TOX132 ADDENDUM I This study addendumwas designed to quantitativelyassessperfluorooctanesulfonate(PFOS,C8F17S03-, CAS # 2795-39-3) levels munexposed, W w a t e r `'matrix"mussels. Matrix mussels were sacrificed upon anid at the m-life testing facility,prior to the start of the study. In the on@ study,the samplesof matrixmusselswere determined to containanaverage of 0.0808 ug/g of PFOS. This levelofPFOS in unexposed mussels was unexpected,so furtheranalyses were conducted. The resultsof the reanalysis,reportedin this addendumindicate that PFOSlevelsmthe samples of matrix mussels are less than0.0174 pg/g. It is likely that the origiaalsamples of mussel matrixthat were analyzed were contaminated during sample prep. Although rigorousquality con@ measures and 3M EnvironmentalLaboratory Standard Operating Procedureswere followed, the acquisitionof thisdata was not necessarilycollectedaccording toapplicable GoodLabratory Practices. Datapresented here is the highest qualitydata availableat thistime. Mussel specimens were collectedon 06/01/99 and sentto the EnvironmentalLaboratoryon 06/07/99. The 3M EnvironmentalLab received, on 06/08/99,a totalof 105 frozen mussel specimens. Onehundred and five specimenswere received; 5 of these were matrix mussels. Uponspecimenreceipt, a chainof custody was initiatedand a copy of thisform canbe fouudmAttachment C of the finalanalyticalreportPOX132). There are no holding timecriteriaassociated with thisanalysis. l?reparai!!ryand Analytical Methods Please refer to the analogous sectionmthe MIanalyticalreport. 14.1 Calibration For quantitativedetermmations, a mid-level, unexhctedmethanol caliiration curve verification(CCV) standard was analyzed every 5 to 10samplesto monitorimtmmental drift. Caliition curveverification standardsare compliant if instrumentalresponse is within +/-30% of the m v h . Inthisstudy, all ccv stsuldards were compliant Quantitation of the target analytes is based on linearregressionanalysis(weighted lhr) of two curves prepared mmethanol, bracketing eachp u p of samples. Quantitation of each analyteis based on the BACK TO MAIN 3M ENVIRONMENTALLABORATORY ANALYTICAL REPORTNO. FACT-TOXI32 ADDENDUM I response of one or more specificdaughter ions using the multiple response-monitoringmode of the instrument 14.2 Blanks Two extractionblanks, utilizing water as m g a t e matrix,were extractedwith each batch of samples. Blanks are compliant if no target analyte is detected above the limit of quantitationfor a specificanalyte. In this study, dl blanks were compliant 14.3 Surrogates Tetra-hydro perfluoIooctane sulfonate is used as a surrogate in this analysis. Surrogate response is monitored to confirmgross instrumentalf a h e , ifnecessary. Surrogateresponseresults were acceptable. 14.4 Matrix Spikes Two matrixspikes at 50 ppb were extractedand adyzed for PFOS. The matrix spikes showedrecoveries of 119%and 75%, withinthe acc-eptablerange of +/-30??. 14.5 Laboratory Control Samples Labomtoq control Samples are not a component of this study. 14.6 Sample Related Comments The level of PFOSmsamplesof mussel tissue was determinedby comparisonwitha standardcurve prepared m solvent Typically,PFOSlevels are determinedversus a m e extractedh m tissue in order to more accurately assess any matrix effects. Results of matrix spike studies conducted in the original study and d e s c r i i in the fiual analyticalreportvalidate the choice of using an unextractedcurve. The results of the reanalysis, reported in this addendum indicate that PFOS levels m the samples of matrix mussels axe less than0.0174 pg/g. It is likely that the originalsamplesof mussel matrix that were adyzed were contaminated during sample prep. Assuming spike recovery studiesform a suitable indicationof endogenousanalyk recovery, data are quantitativeto f 35 %. The validity of this assumption'hasnot beenverifiedby other techniques. Specimensand extracts will be retainedfor aminimumof one year for future evaluation,ifnecessary. Page3 of4 17.1 None. BACK TO MAIN 3 M E " R O N M W A L LABORATORY ANALYTICAL REPORTNO. FACTTOXI32 ADDENDM 1 FACT-TOX-132 BACK TO MAIN Study: Roduct Numbmest Substance): Matrix: MethodlRcvision: Analytical Equipment System Number: Instrument SofhvarJversion: Date of Extlaction/Andyst Date of AnalysidAnalyst Date of Data ReductidAnalyst Sample Data 96 Hour Static Acute ToxicityStudy with the FreshwaterM w c l PFOS Freshwater Mussel Filmam: ETS-86.0, ETS-8-7.0 R-Squared Value: Amlia 062498 Slope: Masslynx 3.2 09/14/99 RWW Y-htcrcept 09/19/99 MEE 09/20/99 MEE See Attachments See Attachments See Attachments See Attachments Gmnp Dose Method Blk QC - lOOppb, Sooppb 36417 Matrix clean mussels b u l p1 Control Sample # H20 Blk-1 H20 Blk-2 1A-10-100 ppb-1 1A-10-100~ b - 2 1A-1O-5ooppb-1 1A-10-5OOppb-2 MATRIX-1-1 MATRIX-1-2 MATRIX-1-3 MATRlX-I4 MATRIX-1-5 1A-6 IA-IO 1B-3 1B-6 Coacentration of PFOS nslg CLOQ (0.0347 uglg) <LOQ (0.0347 uglg) 105% 110% 99% 9o.h CLOQ (0.0347 ~glg) <LOQ (0.0347 Uglg) CLOQ (0.0347 uglg) <LOQ (0.0347 Uglg) <LOQ (0.0347 &) CLOQ (0.0347 uglg) cLOQ (0.0347 uglg) cLOQ (0.0347 uglg) 0.0663 Mean PFOS Odk! <LoQ 1 OPh 95% <LoQ <LOQ NA RSD Std. Dev. MSrmSD RPD NA NA 5% IWO NA NA NA NA NA Date Enterrmy: Date Verified By: 09/21/99 LAC 12/13/99 GML FACT-M-2.1 Excel version 5/95 5/24/00 5 2 7PM 1 FACT-TOX-132 BACK TO MAIN Study: Roduct N u m e s t Substance): Matrix: Method/Rcvision: Analytical Equipment System Number: Instrument SofhvarcNmion: Date of ExtmtiodAnalyst: Date of AnalysislAnalyst: Date of Data RCdUCtiOdAnal)*1: SampleData . 96 Hour Static Acute Toxicity Study withthe Freshwater Mursel PFOS Freshwater Mussel Filename: ETS-84.0, ETS-8-7.0 R-Squared Value: Amelia 062498 Slope: Mwlynx 3.2 9/22/99 MCH Y-IntercCpt: 09/24/99 IAS 09121/99 IAS SeeAttachments Set A t t a c h & See Attachments See Attachments Gronp Dose Method Blk Qc-5oPPb at.9/22/99 M.M. clean mussels Sample # Concentration of PFOS H20 Blk-9 u%e <LOQ (0.0174 udg) H20 Blk-10 <LOQ (0.0174 udg) MATRIX-1-3-MS-9 11Yh MATRIX-I-3-MSD-IO 75% MATRIX-1-1 M A m - I -2 <LoQ(0.0174 udg) <LOQ(0.0174 udg) MATRIX-13 MATRIX44 MATRIX-1-5 CLoQ (0.0174 udg) <LOQ(0.0174 udg) <LoQ (0.0174 ug/g) Limit of Quantitation0P: FOS =0.0174 ug/g Date EntcredlBy: Date Verified/By: iomww LAC 12/13/99 GML Mean PFCS oglg <LoQ 97% <LoQ RSD * Std. Dev. MSMSDRPD NA I , 45% NA NA FACT-M-2.1 Excel venion 5/95 5/24/00 5 2 7 PM BACK TO MAIN 3M ENYIRONMENTALLABORATORY ANALYTICXL REPORTNO. FACT-TOXI32 ADDENDM 1 I I I Analysis of PFOS in Test Organisms from the 96-Hour Static Acute Toxicity Test with the Freshwater Mussel - Laboratory Report No. W2078 FACT Project No. FACT-TOX132 Attachment E Complete Analytical Results FACT-TOX-132 BACK TO MAIN I I -.pJ 12 pp" Cp.20 ppn -.pS 41 ppm -.ps 1-7EZ DueEntaodlBy: Due vaifiedl By: ZB-7 . ZBlO 3A-7 3.4-8 3A-9 3BS 3E-7 3BIO 4A-5 4.4-8 4A-IO 4Bl 4E-2 4E6 5A-7 SA-8 SA-9 5E4 5B-7 5B-9 6A-1 6EI MATRIX-1-1 MATRIX44 MAm-1-5 3.15 5.47 4.85 5.76 3.88 5.11 5.75 S.97 6.91 10.2 7.07 8.06 4.79 6.88 13.1 10.9 9.55 14.0 14.5 8.92 913 86.4 0313 0.0434 0.02s I 33.2 3.96 1.31 19.5 4.83 0.940 8.00 5.61 0.449 23.2 8.07 I .m 23.2 6.58 1.66 16.1 11.2 1.79 24.8 125 3.10 NA 1.8 . 0.0537 ' 0.0937 ' I10 0.103 TOX-13tMd.xL ywoo k2l PM FACT-TOX-132 BACK TO MAIN Study: Product Number(Test Substance): Matrix: Method/Revision: Analytical Equipment Syskm Number Instrument Softwdersion: Date of ExtractiodAnalyst: Date of AnalysidAnalyst: Date of Data ReductiodAnalyst: Sample Data 96 Hour Static Acute Toxicity Study with the FreshwaterMussel PFOS Freshwater Mussel Filename: ETS-86.0, ETS-8-7.0 R-Squared Value: Amelia 062498 Slope: Masslynx 3 3 Y-Intercept: 09/14/99 RFKW 09/19/99 MEE 09/20/99 MEE See Attachments See Attachments See Attachments See Attachments Group Dose Method Blk QC - 100 ppb, :500 ppb 36417 Matrix clean mussels Group 1 Control Sample # H20 Blk-1 H20 BIk-2 1A-10-100 ppb-1 1A-10-100 p ~ b - 2 1A-10-5OOppb-1 1A-10-5OOppb-2 MATRIX-1-1 MATRIX-1-2 MATRIX-1-3 MATRIX-14 MATRIX-1-5 1A-6 1A-10 1B-3 1B-6 Concentration of PFOS uglr <LOQ (0.0347 ug/g) <LOQ (0.0347 ug/g) 105% 110% 99% 90% <LOQ (0.0347 ug/g) <LOQ (0.0347 ug/g) <LOQ (0.0347 ug/g) <LOQ (0.0347 Ug/g) <LOQ (0.0347 ug/g) <LOQ (0.0347 ug/g) <LOQ (0.0347 ug/g) <LOQ (0.0347 ug/g) 0.0663 Mean PFOS uplg <LoQ 108% 95% <LoQ <LoQ NA RSD Std. Dev. MSlMSD RPD NA NA 5% 1 0% NA NA NA NA NA Date EnteredlBy: Date Verified By: 09/21/99 LAC 12/13/99 GML FACT-M-2.1 Excel version 5/95 sn4/00 521 PM ,, FACT-TOX-132 BACK TO MAIN Study: Product NumbeQest Substance): Matrix: MethoMsion: Analytical Equipment System Number: Instrument SoftwareNersion: Date of ExtractiodAnalyst: Date of AnalysidAnalyst: Date of Data ReductiodAnalyst: SampleData . % Hour Static Acute Toxicity Study with the Freshwater Mussel PFOS Freshwater Mussel ETS-84.0, ETS-8-7.0 Filename: R-Squared Value: Amclia 062498 Masslynx 3.2 9/22/99 MCH 09/24/99 IAS 09/27/99 IAS Slope: Y-Intmept: See Attachments See Attachments See Attachments See Attachments Group Dose Method Blk QC-50ppb ext. 9/22/99 Matrix clean mussels Sample # H20 Blk-9 H20 Blk-10 MATRIX-1-3-MS-9 MATRIX-1-3-MSD-1 0 MATRIX-1-1 MATICE-1-2 MATRIX-1-3 MATRIX-1-4 MATRIX-1-5 Concentration of PFOS udg <LOQ (0.0174 ug/g) <LOQ (0.0174 ug/g) 119% 75% CLOQ (0.0174 ug/g) <LOQ (0.0174 ug/g) <LOQ (0.0174 uglg) <LOQ (0.0174 ug/g) <LOQ (0.0174 ug/g) Mean PFOS udg <LOQ 97% <LOQ RSD Std. Dev. MSlMSD RPD NA 45% NA NA Date Entmd/By: Date Verified/ By: 10/W99 LAC 12/13/99 GML FACT-M-2.1 Excel Version 5/95 TOX-I3 2 - M ~ ~ ~ ~ l . x l s 5/24/00 5:27PM