Document rBvbzqLLzdMgb0qVbj6paV7yE

LaboratoryReport AnalyticalReport ofData for PFOSA PharmacokineticStudy inRats (Seraand Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester ProjectNo. T-7132.2 TestingLaboratory 3M EnvirorunentTaelchnology& SafetyServices 3M EnvironmentalLaboratory FluorineAnalyticaClhemistryTeam (FACT) 2-3E-09 935 Bush Avenue, St.Paul,NIN 55106 Laboratory Contact Kris Hanser@ Ph.D. Bldg.2-3E-09 P.O. Box 3331 St.Paul,MN 55133-3331 Phone-.(651)778-6018 FAX: (651)778-6176 Requester Andrew SeacatandDeanna Luebker 3M Company ToxicologyServices 220-2E-02 St.Paul,MN I OF6 . ......... Tlusstudywas designedtoprehnmanly assesstheadsorptloannd metabohm by theSpragueDawley ratof theperfluorooctanesulfoanmyilde(PFOSA, CsFl7SO2NH2,CAS # 31506-32-8)T.estanin@ were dosedby oralgavagewith5 mglkg ofPFOSA suspendedin2% TWEEN 80;controlaninmiswere given2% TWEEN 80 withno PFOSA. Subsetsofthedosedgroupand thecontrolgroupwere sacrificeodn day 1,day 4,and day 29 post-dose.Seraand livercollectefdrom thesacrificemdanialswere senttotheEnvironmentalLab and analyzedquantitatinefloyrperfluorooctanse&omte (PFOS, CsFl7SO3', CAS # 2795-39-3)P,FOSA, and perfluorooctanoa(tPeOAA, C7Fl5CO2', CAS # 2991-51-7). PFOS and PFOSA were detectedintheliverosfalldosedarumal& PFOS levelswerelughestintheday 4 group,butevenlivefrromanin@ sacrifice2d9 dayspostdosewere determinedtocontainhighlevelsof PFOS. PFOSA levelsintheliversofthedosed animalswere highestinthegroup sacrificeodn day 1;on day 29,theaveragePFOSA levelwas approxin=ly 2.5% oftheday 1 levelsP.OAA was notdetecteadbove thelu-niotfquanti=on intheliverosfdosedanir@. As intheliverextracts,eraextractcsollecte4d dayspost-doseevidencedthehioiestPFOS levels.Serum PFOSA levelsdecreasedfrom day 1 today 4 today 29;on day 29,serafrom fouroutoffiveanimalsdidnot containPFOSA abovethelimitofdetectiorPlOAA was detectedintheseraofanimalscollecteodn day I and day 4. Screeningstudiesofthedosematerialsuggestthata smallamount ofPOAA was presentinthe PFOSA dosingsolution. PFOSAB, (CgFl7SO2)2NI-L was detectedintheliverosfdosedanimals.Thisamlytewas alsopresentinthe solutiounsedtodosethewiin@. No investigatioonfsPFOSAB intheseiawere conductecl The solutiounsedtodosethetestanimalswas analyzedtoconfirmthetheoreticadloselevels'.[bePFOSA concentratiointheNVEEN 80 solutiownas detemlinedtobe 1330+/-400 gg/mL. PFOS and POAA were alsoidentifiiendthedosesolutionT.he concentrationfPFOS was estimatedtobeapproximately18.5 gg/rnL-POAA levelsareapproximatedat2.5gg/mL. PFOS and POAA datawere collectefdrom a single analysiasnd shouldbe consideretdobeofsc=mng gahty only.A more thoroughcharacterizatoifonthe materialusedtodosetheanimalswas requestedby 3M Toxicologyand was conductedby FredDcroos prior toinitiatioofnthestudy.Resultsofthismore comprehensivecharactcnzadonareavailablferom the requestors. Althoughrigorousqualitcyontrolmeasuresand 3M EnvironmentalLaboratoryStandardOperating Procedureswere foUoNN-etdh,eacquisitioonf tlusdatawas notnecessarilcyollecteadccordingtoapplicable Good LaboratoryPracticesN.eitherthedosematerialnortheanalyticasltandardwsere givena certificaotfe analysisd;osematerialwas charactenzedby NMR and LCMS and theanalyticasltandardswere charactenzebdy NMR. The datapresentedhereisnotsuitablfeordi@bution toany governmentagencyin defenseofproductsintabihtoyr safetyT.his dataisthehighestqualitdyataavailablaetthismm. eceipt On 10/6/99,10/8/99,an1d1/l/99Deanm Luebker from 3M ToxicologyServicesshippedraturine,feces, livera,nd sera,samplestotheFACR group inthe3M EnvironmentalLaboratorys;ampleswere received frozenon dryiceand NN-crsetoredat-20' C. unes Thereisno holdingtimecriteriaassociatedAiththesesamplesforLC/ESMSMS armlysis. 2 OF6 :@MelhdA.d)si.f.v.t.i.c.a.i.i.:.@ ............. Analyticalmethods ETS-8-4.1,Exu=m ofpotassimnPeffluorooctanesulfonoartOetherFluorocheniicaClompowids from Serum forAnalysisUsing I-IPLC-Electrospray&t'Smpectrometry ETS-8-6.0,ExtractionofPotassiumPerfluorooctanesulformolreOtherFluorochcmicalCompounds from LiverforAnalysisUsing EPLC-Electrospray/MassSpectrometry ETS-8-5.1,AnalysisofPotassiumPerfluorooctanemffonatoer OtherFluorochcmicalsin Serum Exn= Using EPLC-Electrospray/MassSpectrometry ETS-8-7.0,AnalysisofPotassiumPerfluorooctanesulfonaotreOtherFluorochemicalon LiverExuum Using BPLC-Electrospray/Nim Spectrometry Sample preparation-BIPLC/ESMSMS: ion-pai@g extrACtion Analyteisextractefdrom sample matrixwith ionpairingreagent[tetrabutayrl=ordum hydrogen sunte (MA)l ina pH-controUedenvironment 71becatior@creagentselectiveltyargetasnionicfluorochcniicals. Once thear@on-TBA pairisformed,theanalyteisftansfein@idntoa non-polarorganicsolvent(methyl-tertbutylether)d,ried,and reconstitutiendmethanol forMS analysis. HPLC/ESMSMS InHPLC, an aliquotofextractisinjecteadnd passedthrougha reversephase liquidchromatographic colunim Based on theaffinitoyftheanalytcforthestatiormqph= inthecolumn relativteotheliquid mobile phase,theanalyteisretainedfora characteristaimcount oftime. For example,ina slmidard solutionPFOS may cluteat8.0minutes.Retentiontimesbetween a standardPFOS solutionand the analyteextractedfrom tissueinthisarmlysiswere matched on theBPLC *,stem towithin1%. FollowingFTLC separafiorE@SMSMS providesa rapidand accuratemeans foranalyzinga wide range of orgaiuccompounds, includingfluorochen-ticaEllse.ctrospraya,n ionizatiotnechr@queused primarilyfor detectionof molecularions,isgene@a& operatedatrelativelmyildtcmpamn=s. Moleculesareionized, and a primaryion,characteristoifctheanalyte,isselected.n@s ionisbombarded with Wgh-mergy gas-, subsequentcollisioncsreatesmallersecondaryionicfragmentsunique totheprimaryior@which are detected. For example,forPFOS (CsFl7SO3)armlysisi,on499 isselectedasthecharacteristpircimaryion. Thision isfragmentedintootherionssuch as 80 amu (correspondintgoS03), and 230 arrm(C3F6SO3).Each of thesesecondarvfragmentsisdetectedand can be usedto differentiaPtFeOS from othercompounds that might have thesame characterist4i9c9 amu prin@ ior4butdifferencthemicalcompositionsand secondaryion fragmentationpattmis. ........... 4.1 Calibration Quantitatioonfthetargetanalytesisbased on linearregressioannalysis(weighted1/x)of two extracted nm= curvesbracketingeach group of samples. Quanutationof each analyteisbased uitheresponseof one ormore specifidcaughterionsusingthemultipleresponse-momtoringmode ofthemstnimenl A rrdd-leveelx,tractedmatrixcalibratiocnheck standardisanalyzedevery5-10 samples tomonitor instrwnentadlnft.Calibratiocnheck standardsarecompliantifinstrumentarlesponseiswithin+/-30'/oof the expectedvalue. 3 OF6 4.2 Blanks Two extractiobnlanks,utlh=g wateras surrogatematrix,areextractedwitheach batchofsamples. Additionallyt,wo samplesof blankmatrix(bothliverand sera)areextractedalongwith each batchof samples and curves. BLuks arecomph= ifno targetarmlyteisdetectedabove thelimitofdetectionfora specifiacnalyte.In thisstudy,allblvikswere complianl 4.3 Surrogates Tetra-hydroperfluorooctanenffoniastuesed as a surrogatem tlusanalyms. Surrogateresponse is monitoredto confim grossinstrumentaflailurei,fnecessary.In thenon-diliaedsamples,the surrogate responsewas acceptable(+/-5(r/of)orallanalyses. 4.4 Matrix Spikes DuplicatematrixspikeanalysesuW=g alltargetanalyteswere preparedand analyzedforone control anunal,With one exceptiorP4FOS recoverieswere withintheacceptablerangeof70-1300/o.One liver matrixspikeshowed a 66 % recoveryforPFOS. AU PFOSA matrixspikerecoverieswere acceptablefor PFOSA- As POAA was nota targetarwyte indw analysisn,o matrixspB= were prepared.Although the recoveryofPOAA from seraand liverhas bem verifiedforothermubes, POAA resultshouldbe consideredscreeningqualityonly. One matrixspikewas preparedforeach of thetargetanalytesinthedoseverificatiosntudy.Spike recovery forPFOSA was 1301/oP,FOS was 1151/oa,nd POAA was 121%. 4.5 Laboratory Control Samples LaboratoryControlSamples arenota component oftlusstudy. 4.6 Sample Related Comments. Otherni=ces subnuttedwith tlusstudywillbe analyzedas needed upon writtenrequestfrom the sponsors.In theeventoffurtheranalysisa,n additionarleportwillbe gencratecl Dose venficationwas conductedby evaluatingdilutedahquotsof thedose againstan unextracted=ridard curve.Triplicatdeilutionosf theTWEEN 80 dose solutionwere analyzedfordeterminatioonfPFOSA; a singledilutiownas analyzedfordeterminationofPFOS and POAA- ................ .... Su)nmary,:: ....... ... . ........... ...................... .......... ...... . ne tableof resultdsetailintghesem analysisisavailablien Attachment A- Resultsoftheliveranalysisare presentedin AnactunentB. PFOS and PFOSA were detectedintheliversof alldosed aninmls.PFOS levelswere highestintheday 4 group,buteven day 29 group aninmlswere determinedtocontainhigh levelsof PFOS. PFOSA levelsinthe liversofthedosed animalswere highestinthegroup sacrificeodn day 1;on day 29,theaveragePFOSA level was approximately2.5% of theday 1 levels.POAA was notdetectedabove thelimitof quantitatioinn dosed anftnals. As intheliverextractss,eraextractcsollected4 days post-doseevidencedthehighestPFOS levels.Serum PFOSA levelsdecreasedfrom day 1 today 4 today 29;on day 29,serafrom fouroutoffivewiin@ didnot containPFOSA above thelimitofdetection.POAA was detectedintheseraofanirrwscollectedon day 1 and day 4. Screeningstudiesof thedose materialsuggestthata smallamount ofPOAA was presentinthe PFOSA dosingsolutiorl PFOSAB was detectedintheEversof dosedanim@. Tbs analytewas aL;opresentinthesolufionused to dosethewiii@. No investigatioonfsPFOSAB intheserawere conducted. 4 OF6 Thesolutiuosnedtodosethetesmt@nws wasanalyzetdoconfirdmoselevelTsh.ePFOSA concentratiinon theTWEEN 80solutiwoansdetmmiinteodbe 1330+/-400gg/mL.PFOS andPOAA werealsoidentifiend thedosesolutiomThe concentratioonfPFOS was estimatedtobe approxmimcly 18.5gg/mL; POAA levels areapproximatedat2.5gg/mL. PFOS and POAA datawere collectedfrom a singlearmbsis and shouldbe consideredtobe of screeningqualityonly. .....@.@:.i@@D :'Oualz .......... lee ves::,Ond ........ No circumstancesexisteduringthepresentstudythatwould have adverselyaffectedthequalityor uitegnty of thedata.The followingdataqualityobjectivewsere followedduringthestudy: Linearit-y The correlatiocnoefficien(trA2)of thestandardcurvewas equaltoor greaterthan 0.98using I/xweighting Limitsofdetectio(ndefineads1/2 theLOQ) - PFOS inserais4.88ng /niL;PFOS inliveris15.3ng / g-, PFOSA inserais2.47ng /mL; PFOSA inliveris6.2ng /g Lumts of quantitanm(definedas thelowestextractedstandardaccurateto wittun30% of theoretical value)-PFOS in serais9.76ng / rnL;PFOS in liveris30.7ng / g-,PFOSA in serais 4.93ng / mL; PFOSA inliveris12.4ng /g Duplicationfrequency/acceptabplreecision-< 30% Spike fiequency/acceptabrleecoverie-s 70% to 130%; PFOS recoverywas 66 % fora singlematrix spikeinliver(seeSection4.4) Use of confirmatorymethods - no confirmatorymethods were used Demonstrationof specifici-tyspecificitwyas demonstratedby chromatograpl@cretentiotnime and mass spectraclharactmmon of a singlqproduction Given theparameterslisteadbove,and assuming spiken=venes form a suitableindicationof endogenous analyterecovery,dataarequantitativteo 301/o.The validitoyf thisa&wnption has not been verifiedby othertechniques. .... ...... ....... .... Attachment A: Table of resultsof seraanalysis Attachment B -T.able of resultsof liveranalysis Attachment C: Sample receipt Attachment D: Screeningresultosf dose verification AttachmentE: Extractionand analyticadlata 5 OF6 ............. . . ...... . ......... ........ ... ................ ........ . ........... .......... LisaClemen, Advanced Chanist lig Date KrisHmsen, Ph.D.,PrincipaAlnalyficaIlnvestigator Date 6 OF6 m LaboratDryReport AnalyticalReport ofData for PFOSA PharmacokineticStudy inPats (Seraand Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester ProjectNo. T-7132.2 Attachment A Tableo.f Results-SeraAnalysis vv 6i-1.99-9099 sq.v vv vvv v vvv v vvv v d x x z z zv z zz z Z.zz'Szzzz v x zzzz;;;;-.$;-!ZZZZZ d vv vvv vv vv v < < <<< ZZ Z ZZ X Z Z x z . ... . d o@ < < < -- --zzz zz - -- <z <z zc <z <z ZZI as <Z Z. < 93 vv v x coon 0 a 92 a comonnomoo u 9 @0 - v 0- O@ v vvv vv vI vv vvv vv 7, 12329 4. 7------------ 7 > 9.9 -40 6d > oa > m LaboratD]ryR,epoit AnalyticalReport ofData for PFOSA PharmacokineticStudy inPats (Seraand Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester ProjectNo. T-7132.2 Attachment B Table.oRfesults- LiverAnalysis FACT-TOX-145 Snady productN=bcr(Tmi Subsume) Matrix. M@d,odfR-.=. AnalyticaElquiprnnt System Nmbcr Insoument Softwat(Venion Date or ExwactioWAnalySL Due of AnalysWArWyst Dwe or Dam Redmt3oiVA"Yst Sample Data MX.145 phumacaki-iicsnjdyorPFOSAinP.= T-7132.2 R21 L,@a E-rs-".o .d ETS-8-7.0 SoLq)020199, Armlia 062498 Massty= 3.3 10/13/99,11/04M SEE/RWW/SAL 10/15,99.l(YI9/99MMH. lllOS/99tAS- 11/10" LAS joilim. lot2a", 1I/Ogt99,11111/99LAS/MME Filakum: R-Squwed Vaiw: Slope: Y-WA=PL See Anadufwm See Attachments S- Anach@wm See AUKhments RAT LIVER Grmp ulast Smple 0 PFOS Cldc. Cmc Method Blk maau Bik QC 250 ppb c@p I O.Oms(kg Group 2 O.Omg(kg Group 3 0.0mgikg Group 4 5.Omg/kg Group 5 5@O mgkg Group 6 S.Omg(kg L.mi ofQ@utauon Lmt L..ito(Dewnm (LOD): H20 Bik-II ng" H20 Dik-I1 R20 BLk-2 R20 Bik-2 FLBLI0199-Li@ff Blk-I1 0.00 0.00 0.00 0.00 PBLIG]99-Liver Bik-I I o@oo RBLI0199-Liver BLk-2 RBLI0199-LimBIk-2 1.96 0.00 9RO32.30M. Dayl-MS-1 1 276 9RO3230M, 264 - 9RO3Z35M=-.'2' 226 9RO3235M, Day4-MSD-12 216 9RO3240M, Day29-MS-1 212 9RO3240M. Day29-MSD-2 191 9RO32.30M. Day 1 9RO323 I M. Day 1 9RO3232M. Day 1 0.00 0.00 0.00 9RO3233M.D2yi 9R03234M.Dayl 0.00 O.OD 9RO3235M. Days 0.0() 9RO3236M. Days O.W 9RO3250M. Day4 9R032.38K Day4 9RO3239M. Day4 29,5 22.0 0.00 9RO3240M. Day29 9RO324 IM. Day29 0.00 0.00 9RO3242M.Dzy29 0.00 9RO3243M. 9RO3244M. 9RO3245M. Day29 Day29 Day 1 0.00 0.00 2.3660 9RO3246M.Dayl 3Z260 9R03247M. Day 1 9RO3249M. Day 1 36179 21200 9RO3249M.Dayl 27929 9RO3237M. Day4 9RO3251M.Day4 9RO3252M. D2y4 9RO3253M, DIY4 9RO3254M. Day4 36791 32619 42606 369L45 38268 9RO3255M, Day29 20305 9RO3256M, Day29 20638 9RO3257M. Day29 22025 9RO3251M. Day29 26172 9RO3P11,9.M". .Day29 29867 (LOQ): 26.9 ... IIOSA - 11.1nWg PFOS - 8.45ngig.PFOSA - 3.50@gog ToW Amount of PFOS u <LA)D <LOD <D <LOD <LOD I <LOD <LOD <LOD 921/. 98% 75% 72% 72% 65% <LAJD <LOD <LOD <L.OD @LOD <LOD <LOD om95 <LOQ @LOD <LOD <LOD <LOD <LOD <LOD 23.7 313 36.2 21.2 27.8 36.i-- 32.6 42.6 36@9 33.3 20.3 20,6 22.0 262 1 29,9 Date Enwre&Analyst: 10121/99.lGaZ'99,11/15/99 LAC, I1/08M GML Date Veriftcd/Analyst 11/16/99 GM3. Avwage PFOS olvg <LOD <LOD <LOD <LOD 90-/. 73% 69% <LOD <LOQ <LOD 28,2 37,4 Z3 8 RSD Sid. D@. MS/MSD RPD <LOD <LOD <LOD <LOD 5% 5% 10-/. <LOD <LOQ <LOD 21.7 6.12 9,56 3.58 17.3 4 12 PFOSA Cak.Con& Total Amount of PFOSA nwt 0.00 0.00 uvg <LOD <LOD 0.00 <LOD 0.00 <LOD 0.00 @LOD o@oo <LOD 0.760 <LOD 00313 293 229 215 <LOD 104% 94% 76% 71% 352 119% 330 112% O.OD @LOD 0.00 <LOD 0.00 <LA)D 0.00 <LOD 0.00 <LOD 2.35 -LOD 0.00 @LOD 22.0 0.0220 4.66 <LOD 0.00 <LOD 2-57 <LOD 1.72 <LOD 0.724 <LOD 0.162 <LOD o@00967 <LOD 6021 6.02 7015 7.02 6239 6.24 6657 6@66 8811 981 3523 3.52 3470 3,47 3959 3.96 3454 3@45 4105 4.11 85@5 0.0855 175 0,175 104 0104 142 0.142 303 0303 PFOS PerfluoroocL=aWfonate Awrige PF'OSA olvz <LOD <LOD <LOD <LOD 99% 74% 116% <LOD <LOD <LOD 695 370 0162 PFOSA - PeffluaromuresWf@ide Sampla nwnben my h@ beenmtchod 3237 shouldbe 3250 @' Thm @ples tinybe falselhyigh,due tocaffyovctf@ accidentally sitching32.37and 3250 GMLII/16199 RSD Std. N@. MSIMSD RPD <LOD @LOD <LOD <LOD 1 71/. 7% <LOD <LOD <LOD 16.0 I'll 8@28 0,307 530 00959 - ETS-8-7.0 ExcelV-im 5195 TOX-145-li@a.xls 1113(y" 9:33 AM m I m)ratoiyrepoit AnalyticalReport ofData for PFOSA PharmacokineticStudy inRats (Seraand Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester ProjectNo. T-7132.2 Attachment C Sample Receipt 10/06/1999 IK 3M ENVIRONMENTAL LABORATORY 1 REQUEST FOR ANALYTICAL/FIELD WORK LAB REOUEST NO. W2814 REQUESTOR NAME: DEANNA LUEBKER DEPARTMENT: 0227 PROJECT NO: 0010535009 DATE RECEIVED: 10/06/1999 DESC: PFOSA PK STUDY IN RATS TOX-145 CONTRACT LAB(S): EXP COMP DATE: 12/30/1999 DATE COMPLETED: PROJECT LEAD: KJ HANSEN PHONE NO: 651-778-6018 3M FAX NO: 651-778-6176 220-2E-02,7-1374 -------------------------------------------------------------------------------- SAMPLE DATE CODE DESCRIPTION RESULT MDL or (95% C.I.) -------------------------------------------------------------------------------- -----------1 KJH-SPEC SPECIAL STUDY - KJH UPDATED DATA vI LAC TOX-145 SAMPLES RECEIVED Barbara A. Gramenz 10/07/99 10:08AM ET&SS Lab 2-3E-09 Fax: 778-6176 To: Kari J.Rambo/US-Corporate/3M/US@3M-Corporate Grant A. Paul/US-Corporate/3M/US@3M-Corporate LisaA. Clemen/US-Corporate/3M/US@3M-Corporate KrisJ. H an sen/ US- Corporate/3 M/US@3M -Corporate cc: Subject: TOX-145 SAMPLES RECEIVED On 10/6/99 we received10 Liver,10 Sera,20 Feces and 20 Urine Samples fordays 1 & 2 from 3M TOXICOLOGY. FACT. TOX -1475.LAB REQUEST # W2814. PFOSA PK Study in Rats (T-7132.2). Samples receivedfrozenon dry iceand have been storedin Freezer F-16 at -20+\-10C. Barb Printed10/07/99 [3M Restricted) Page I PFOSA PK STUDY IN RATS TOX-145 LR# W2814 DAY 1 DATE 10/5/99 Gen. MALE POST DOSE URINE ID# 9RO3240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 FECESID# 9RO3240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 LIVER [D# 9RO3230 9R03231 9RO3232 9RO3233 9RO3234 9RO3245 9RO3246 9RO3247 9RO3248 9RO3249 SERA ID# 9RO3230 9RO3231 9RO3232 9RO3233 9RO3234 9RO3245 9RO3246 9RO3247 9RO3248 9RO3249 DAY 2 DATE 10/6/99 Gen.MALE POST DOSE URINE ID# 9RO3240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 FECESID# 9R03240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 TIT E Z, 'f cc 0 (D E C4n) E 0 cn CL E cn Iz CD CD zi Wall 4OB3 ;o siauiezuoo lelo.L (D 0m L) D io'- t -6 OOA HOBN t os4H ONH z OUON A Z' r ry) @n z -t c: 1.0 0 CD cn tv cc (D cmn m cc d) E o L) 0 0>Er 03: w C.) U) rt E E v -z cr ECL) C,4 TOX-145 SAMPLES RECEIVED Barbara A. Gramenz 10/11/99 11:54 AM ET&SS Lab 2-3E.09 Fax: 778-6176 To: Kari J.Ra mbo/US-Corporate/3M/US@3M -Corporate Grant A. Pau I/US- Corporate/3M/ US@3M -Corporate LisaA. Clemen/US-Corporate/3M/US@3M-Corporate Kris J.Hansen/ US-Corporate/3M/US@3M -Corporate cc: Subject: TOX-145 days 3&4 SAMPLES RECEIVED On 10/8/99 we received10 Liver,10 Sera,20 Feces and 20 Urine Samples forday 3 10/7/99 & day 4 10/8/99 from 3M TOXICOLOGY. FACT- TOX -145. LAB REQUEST # W2814. PFOSA PK Study in Rats (T-7132.2). Samples receivedfrozenon dry iceand have been stored in Freezer F-16 at -20+\-10C. Barb Printed10/11/99 (3M Restricted] Page I PFOSA PK STUDY IN RATS TOX-145 DAY 3 DATE 10/7/99 Gen. MALE POST DOSE URINE ID# 9RO3240 9RO3241 9RO3242 9RO3243 9R03244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 FECESID# 9RO3240 9R03241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 DAY 4 DATE 10/8/99 Gen.MALE POST DOSE URINE [D# 9RO3240 9R03241 9RO3242 9R03243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 FECESID# 9RO3240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 LIVER ID# SERAID# 9RO3235 9RO3235 9RO3236 9RO3236 9R03237 9RO3237 9RO3238 9RO3238 9RO3239 9RO3239 9R03250 9R03250 9RO3251' 9RO3251 9RO3252 9RO3252 9RO3253 9RO3254 G)9RO3254 DNE D!-@T Kk3oLl) UW,C44 C@)ae PFCSA PK STUDY IN RATS TOX- 145 LR# W2814 DAY 3 DATE 10/7/99 Gen. MALE POST DOSE URINE 10# 9RO3240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 FECESID# 9RO3240 9R03241 9RO3242 9RO3243 9R03244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 DAY 4 DATE 10/8/99 Gen.MALE POST DOSE URINE ID# 9RO3240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 FECESID# 9RO3240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 LIVER ID# SERA ID# 9RO3235 9RO3235 9RO3236 9R03236 9RO3237 9RO3237 9RO3238 9RO3238 9RO3239 9RO3239 9R03250 9RO3250 9RO3251 9R03251 9RO3252 9RO3252 9RO3253 9RO3254 nn9RO3254 lul -F'4"'2 Np- hdV6.. qRZ:-@@,4 5EZN SPtKPLE5 RDB.-6@2) ZLLT DE@@T KiioLL) CLWIC+;CME CL 2. jCU C, e C13 4) 0 L) CD CD -1 CD - IZ El ii WO;l40" 10 sioullnUO3linoil,o I C).<) CD OOA ,z tD Zu: HOUN VOS'H ONH z OUON ,z tn cr- 0 LL d) E ck cn d) > 0 U) CD a: > cn I 0 ui %j a).2 E U) m ,a - ty CM M le Ln to r@ co CY cn TOX-145 day 29 SAMPLES RECEIVED Barbara A. Gramenz 11/02/99 02:13 PM ET&SS Lab 2-3E.09 Fax: 778-6176 To: Kari J. Ram bo/US-Corporate/3M/ US@3M -Corporate Grant A. Pau I/U S-Corporate/3 M/ US@3M -Corporate Lisa A. Clemen/ U S-Corporate/3M/US@3 M -Corporate Kris J. H a nsen/US-Corporate/3M /U S@3M -Corporate cc: Subject: TOX-145 day 29 SAMPLES RECEIVED On 11/2/99 we received 10 Liver,10 Sera Samples for day 29 from 3M TOXICOLOGY. FACT- TOX .145. LAB REQUEST # W2814. PFOSA PK Study in Rats (T-7132.2). Samples receivedfrozen on dry ice and have been stored in FreezerF-16 at -20+\-IOC. Barb le 4 tle Printed11/02/99 [3M Restricted] Page 1 PFOSA PK STUDY IN RATS TOX-145 LR# W2814 DAY 29 DATE 11/2/99 Gen.MALE POST DOSE LIVER ID# 9RO3240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 SERA ID# 9RO3240 9RO3241 9RO3242 9RO3243 9RO3244 9RO3255 9RO3256 9RO3257 9RO3258 9RO3259 -3>< %Z Z5 CD cy-) C7) CD J.7 Z; E L,@ 2 z i-- u C'lD ) Cl) (a m cn El 1 1 W81 1 4*e 310 rjaullnuo3 INO.L IrD 0 co cc IL E m z OOA HOEN 11 OS114 C ONH 8UON .x.c .0 CD > 4) cc 00) .0 0 l@ L E (D -Z 0 cc 0.2 o cnn 4D EC C) 0 ui E @j i3 E EEE -. 1 E C,4 m e Ln w III 0 LaboratDryRepoit AnalyticaRleport ofData for PFOSA PharmacokineticStudyinRats (Seraand Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester ProjectNo. T-7132.2 Attachment D ScreeningResultsofDose Verification KrisJ. Hansen " /04/9902:29 PM Tel: 778-6018 2-3E-09 Fax: 778-6176 EnvironmentaLlab To: Andrew Seacat/U S-Co rporate/3M /US@ 3M -Corporate Deanna J. Luebker/US-Corporate/3M/US@3M-Corporate cc: LisaA. Clemen/US-Corporate/3M/US@3M-Corporate Subject: TOX145: PFOSA PK, Dose Verification Hi Andrew and Deanna: We have completed our screen of the PFOSA dose inTWEEN. Errorbars are about +/-30%. PFOSA was determined in triplicataend PFOS and POAA from a singleanalysis. I'dclassifythis data as screening qualityand ifthisdata poses any major questions about the interpretationof the tox data, we may need more data pointsfor the PFOS and POAA. However, I did check for the presence of the POAA on two differentinstruments. Also, in one of your voice mails,Andrew, you mentioned concern about photolysisof PFOSA to PFOS. Allof the data that I'veseen indicatesthatthere may be photolysisof PFOSA to POAA (not verifiedyet),but there isno evidence of PFOSA photolysisto PFOS. Since the photolysis experiments were conducted under very strenuous conditions,I don't thinkyou have much to worry about with your samples (atleastnot fora few dozen years!). In TWEEN 80: PFOSA recovery 130% PFOS recovery POAA recovery 121% 133.26 % of expected dose of 1000 jig/mL 185 % of expected dose of 10 pg/mL 115% 1330/ig/mL 18.5pg/mL 2.5 jig/mL spike spike spike Let me know ifyou have questions. kjh Andrew Seacat 10/27/99 02:53 PM 3M Medical Dept.ToxicologyServices Andrew M. Seacat Ph.D. 3M Center 220-2E-02 SaintPaul,MN 55144 Tel: (651)575-3161 Fax: (651)733-1773 To: cc: Subject: Kris J. Hansen/US-Corporate/3M/US@3M-Corporate Fred L. DeRoos/US-Corporate/3M/US@3M-Corporate Deanna J. Luebker/US-Corporate/3M/US@3M-Corporate Sue Chang /US-Corporate/3 M/U S@ 3M-Corporate PFOSA dosing solution Kris, As we were discussing in our lastFriday's meeting,we would liketo have the PFOSA dosing solutionchecked for PFOSA concentration, and for PFOS and PFOA, which may under certain conditions arisefrom photolysis.We leftthe dosing solutionwith you. I understand there is a problem with the Tween 80 concentraton being too high to allow sufficientdilutionfor analysis of some PFOS concentrations. Given that the startingmaterialhas approxmately 1% PFOS in itcould the dosing solution sample be analysed to see ifthere issignificantlmyore PFOS in there? Ifnot possible,then perhaps we could ask Fred Deroos to analyze the dosing solution? The dosing solution was prepared as follows: Stock PFOSA in acetone was made up at 52mg PFOSA/0.52 mL acetone = 100 mg/mL This was dilutedinto 51.48 mi of 2% Tween Finalconcentration of PFOSA = lmg/mi Final conc of acetone 1 % Finalconc Tween 80 -2% 80 to acheive the dosing solution: Thanks, Andrew ui Us En 05a z Study Date Analyzed File# Instrument PFOSA in2% Tween 80, Sample TN-A-3046 File# 10299013 10299014 10299017 Mean Standard Dev. %RSD TOX145 10/29/99 102999a Soup 020199 % Recovery ofDose Recovery ofDose amt (ppb) 132.64 265.27 134.31 268.62 132.83 265.65 133.26 0.917 0.688 266.51 1.83 0.688 .e4V"@"A 7-D0 rr"' ve r_ovlaIio- Z14cl" PF6SA i-r Sf PFOSA dosing solution Andrew Seacat 10/27/99 02:53 PM 3M Medical Dept. ToxicologyServices Andrew M. Seacat Ph.D. 3M Center 220-2E-02 SaintPaul,MN 55144 Tel: (651)575-3161 Fax: (651)733-1773 To: cc: Subject: Kris J. Hansen/US-Corporate/3M/US@3M-Corporate Fred L. DeRoos/US-Corporate/3M/US@3M-Corporate Deanna J. Luebker/US-Corporate/3M/US@3M-Corporate Sue Chang/US-Corporate/3M/US@3M-Corporate PFOSA dosing solution Kris, As we were discussing in our lastFriday'smeeting,we would liketo have the PFOSA dosing solutionchecked for PFOSA concentration, and for PFOS and PFOA, which may under certain conditions arisefrom photolysis.We leftthe dosing solution with you. I understand there isa problem with the Tween 80 concentraton being too high to allow sufficientdilutionfor analysis of some PFOS concentrations. Given that the startingmaterial has approxmately 1% PFOS in itcould the dosing solutionsample be analysed to see ifthere issignificantlymore PFOS in there? Ifnot possible,then perhaps we could ask Fred Deroos to analyze the dosing solution? The dosing solution was prepared as follows: Stock PFOSA in acetone was made up at 52mg PFOSA/0.52 mL acetone = 100 mg/mL This was dilutedinto 51.48 mi of 2% Tween Finalconcentration of PFOSA = lmg/mi Final conc of acetone 1 % Finalconc Tween 80 -2% 80 to acheive the dosing solution: Thanks, Andrew /1. /000 co-^-* &/ 16 6 0 16 Co-e, /0 0 tK6 o. -o-7softL- 0 Printed11/04/99 o /,%o".L ,4 1 d S- [3M Restricted] o*17' 5D ape /DSL- rAL IDW teC Page 1 ac/. 460M 3) :OTfeEy iEf 33"awDk : 3%% iBNt: i ih 0 [of iy hyig AE an Ey (ED) i 0J i]i iHlRl i i Si | I i iil J i i i = iT = 3 on 2% 1 FACT: Daic Data Analyst. FACT Study 4@ I-A s -ro A I9@@ Ntatrix(Timepoints:7@.- -o c@ Simple List: -/oz@f f Sct-upAnalysis Date/Analyst: /z f,/f Instrument: -72@,/,rf DA'I'A REN,'IENN SLiNItNIAMI tUX@ti JA@S Data Rcview Sign-Off Analyst Review_ Name / Date: Tecbnical Review Name / Date: QuaLityAssuranRceeview Name /Date: Data Entr-y: Conments Jusdncations: Analyte: 7@6AA er-H I AcceptableLinearRuge- LOQ: OL)"AA /cop"02 -7TF-xbwtion BW& R^2: ()@@f-7171 Matrix Bbmic /hq CalibratioCnhecks: NIS/MSD: de ,DataStiLtus: !ga bw- i Analyte: tOF05 CCH2- AcceptableLinew Range: /12/;@-12@ /-7/&24 LOQ! ExwactedBlani,-NA R^2:. Matrix BlaniL AIA CalibrafioCnhecks: MS/MSD: .Data Status: &1# 7@- -7A s 0,2 ye p z- 0 iL4 /15S 30 '>/- 7@e la 1 v -cc Analyte: ?FO,5x rc,43)0 AcceptableLincar Range: > LOQ! R^2: /a. /OFP@ 0 -ff-7-7.,l ExtractedBlank: Matrix Blank: ,IIA 74. /.7/ C.alibradonChecks: ed-lekel- MSIMSD: 03 idata Satw: Date Data Analyst. @Z4 6 FACT: DA'I'A REv'IEW SUi*vIINIAR@k UF..,Ni -r*5 Data Rcyiew Sign-Off r Analyst Review Name/ Date: 70-'5 Y/,//tt FACT Study 4: --TojcrY@5- Niatnx@Timepoinu-:7i@..e-o ei Ci 41 1-0- Sample LAt: Z I f-P4-- Set-upAnalysi3 Date/Analyst: Enstrument: P/, f /f i@o .5 TechnkalReview Name /Date: Quahly Assurance Review Nune /Datc: Data Entry- Comnwnts /Jugd&ations: Anslyte: AcceptableLincirRAnSc- NA LOQ AIA R^2: IVA CalibratioCnheck& tyra M&INBD: idataStatus: Analyte: AcceptableLinearRange: LOQ: R^2: Calibmbon Checks: MSMSD: idataStatus: ExbmctionBWnic AIA NU= BW& NA ExtractedBl&nL- 7@7 Matrix BlanL- /lp u li-rp 14X 6s as -6 s 7,/L, Analyte: AcceptableLinearRAngc: LOQ: R^2: C.,baIrliLbtroa/dnon =it ecks: msims 1D Satus: ExtractedBlank: Matrix Blank: Qu&ntify Ccapou-d S-- ROP"@ TOX14LS-t@an 80 dose confir@t@on for po", pros, & POAJL- "t- Sampla Listt Lastt rwdi ia:d: M 2 hod: t @dified: " Job Coda: C: \KA-SSLYM\soup02Ol99 1 -P-\s=WlaDB\102999& P i o@t 29 10:23:59 999 C:\M"SLYNX@souV020199.pro\1NatbDB\102999. "on Nov 01 06:21:40 999 Print*d: No. Nov 01 06:47:34 1999 10/29/99 i&B ccupound 1: POKA 0 N1- 99001 OZ9 102999002 3 102999003 10,999004 5 0 9999005 1 1l@2'99 006 10,99900, 89 il@ll@99900'8 9 10,99901 0 11 1OZ999011 1: 10,999012 1 *1 101999013 1' 10,999014 15 101999015 1 17 102999017 18 10,999018 19 10,999019 .3 10299902C 11 102999021 102999022 -3 10,999023 2 45 11002999024 2 10 1999015 2_6 10 1999999026 7 2298 10;19990@8 - - -9 (Chl) S lEalist T-t ME'OWH ..o Ik .E-lk FCMI H 99086-43-1, FCMix-99086-43-:,3 FCMix-99086-4 -3, F-@M@x-99086-43-4, F@-Mix-99086-43-5, Fcm@x:9908.-43-6 -x 99086:43:7: , FFCC.M4@ 99086 43 8 FcMix-99086-43-9. lppb- 9/10/99 RWW 5ppb- 9/'-0/99 9 RWW 10ppb 9.'-0/9 RWW 25ppb- 9,'0/99 RWW 50ppbIOUPP.25OPPb 500ppb 750ppb- 9 @0/99 9 RWW ;@@0/99 RWW -9 99 Rww 10 9 RWW 9/10/99 RWW MEOH Elk ICX145:PFOS/PO / TOX145 AA FCM,x-99,08P6FC-S43-4P,C) MEOH B k 'mXld5-PFOSA in in Tween-dose-2ppbTee.1---4ppb- -25ppb- 9/10/99 Tw::n-dose-200ppb- 10/29/99 10/29/99 RWW 10/29/99 IAS IAS I.AS TOX145-PFOSA , 5 n-W-30_ 0p b- 9 10/29/99 -99086- i3-n7,IV 2 Oppb 9/lpo/9 RWW FMEcOmH Bik Fcmix-990 6-@13-1, lppb- 9/10/99 RWW FCM@x-990:6-43-2, 5ppb- 9/10/99 RWW FCM,x-99086-4 loppb- 9/10/99 RWW FCMix-99086-4,-,@ @-4 25ppb- 9 /10/99 RWW F ix-990 6-43-5. FCM 90:86-43-6, F CCMM@X-9990 6-4 3 -7, FCM,,-99086-43-8, 50ppb100p b 250pp pb 500ppb- 9/10/99 9 RWW 99 /10/9 9 /10/9 9 10//99 RWW RWW RWW FCMix-99096-43-9. 750ppb- 91110 99 RWW IAS Typa Standard Standard Sta dard Standard Standard Standard St. dard Standard Standard oc oc standard Standard St@ rd Standdaar d st@dard Standard St ndard Standar d Standard std Co= 1.00 5.0@ 10 .00 25.IC 50.20 100.00 251.00 502 00 752:00 25.10 251.00 1.00 5.02 10.00 25.10 50.20 100.00 251.OC 502 .00 752.00 RT 7.154 77..01828 7.10'9 7.0', 7.08; 7 0834 7@.2, C)3 7 .I23 77 .11479 7 152 7@134 7 .147 7.131 7 160 7:128 7.110 7.169 7.174 7.180 7.129 7.130 7.179 .154 7.129 Ara4! Flag& - bb 16 53 12 08 4 4714 981. 2481 5 25@ 54 l@ 22 40 259 MM mm bb bb bb bbX bb bbX b@bX mm mm mm bb 12 MM 231631 MbMb 13 67 113 27 5 31 102ai 23 38 4210 5411 mm MM mMmM bb mm bbX bbX bbX COnc. 3.66 %DSv 1.0: 4.72 10.223.74 46.43 97.28 2 6 . 70 4243 as 55I.;-l o. 1 67 2 -6 2 -5 -8 -3 --16 -27 IC 3@51 25.32 1 0.70 0.6. 234L . 97 -6 0.73 6.15 10.71 26. 61 53.45 101.52 232.52 418.9@ 538.7- -@7 23 7 6 6 - -7 _17 28 Soup 020199: gu@titated and printad kyy i" on 11/01/99 Quantify Compound Summry Report TOX145-t@on 80 doze confi@tion for POAA, Pros, r POAA- SA@le LiSt: L&3t modified; L&St modified: Job Code: Printed: C:\XASSLYNX\souPO20199.pro\SanpleDB\102999& Fri Oct 29 10:23:59 1999 C:\MASSLYNX\zoup02Ol99.p@.\Ktb=\102999. Man Nov 01 06:21:40 1999 Non No@ 01 06:47:34 1999 t. 10/29/99 i&S Compound 2: PFOS (Ch2) I Name i 10299900@ 2 10299900.' 3 102999003 4 102999004 5 102999005 6 IC299900@ - il:999OC-1 1 :@2999009 i: @C-19990-3 I- 102999oi1- 1029990@Z 10-1999013 1. 102999014 15 10.1999015 16 102999016 17 102999017 19 102999018 i9 102999019 .10 1029990,10 ZI 10299901@ 22 102999OZ2 23 1029990.3 .1. 102999014 25 102999OZ5 26 102999026 '7 102999027 25 lo2q99028 29 '.02999029 Samplelist T"t MeOki Bl@. MEOH Blk FCMix-99086-43--, FCMIX-99086-43-, FCM,.-99086-43-3, FCMix-99086-43-@, FCM@x-990Bb-4'@-5, FCM@.-99086-43-., FCM@x-99086-43-7, FCM,x-9908@-43-8, FCM,x-99086-43-9, MECH Blk TOX145-PFOS/POAA TOX145-PFOS/POAA FCMix-99086-43-4, M@OH Blk TOX145-PFOSA in IOX145-PFOSA in FCMix-99086-43-7, MEOH Blk FCMix-99086-43-1., FCMix-99086-43-2, FCM@x-99086-43-3, FCM@.-99086-43-4, FCMix-99086-43-5, FCMix-99086-43-6, FCM,x-99086-43--,, FCMix-99086-43-8. FCM-x-99086-43-9, lppb- 9/10/99 RWW 5ppb- 9/ID/99 RWW loppb- 9 '-0/99 RWW 25ppb- 9/:,0/99 RWW 50ppb- 9,110/99 RWW 100ppb- 9@10/99 RWW 250ppb- 9,'10/99 RWW 500ppb- 9,'10/99 RWW 750ppb- 9/10/99 RWW in Tween-dose-2ppb- 10/29/99 IAS in 7Veen-=-4ppb- 10/29/99 IAS 25ppb- 9/10/99 RWW Tween-do.e-200ppbTween-=-300ppb- 250ppb- 9/10/99 10/29/99 10/29/99 RWW IAS ZAS lppb5ppt>- 9/10/99 9/10/99 Rww RWW loppb- 9/10/99 RWW 25ppb- 9/10/99 RWW 50ppb- 9/10/99 RWW 100ppb250ppb500ppb- 9/10/99 RWW 9/10/99 RWW 9!10/99 RWW 750ppb- 9/10/99 RWW TYPO Standard Standard Standard Standard Standard Standard Standard Standard Standard QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Co= 1.01 5.03 10.00 25.20 50.3C 101.00 252.00 503.OG 755.00 25.20 252.00 1.01 5.03 10.00 25.20 50.30 101.00 252.DC 503.00 755.00 RT 7-315 7.295 7.226 7.291 '.240 7.266 7.248 7.246 7.27'@ 7.265 7.289 7.309 7.313 7.340 7.331 7.338 7.314 7.32'7.313 7.295 7.272 7.330 7.335 7.342 7.29@ 7.313 7.363 7.314 7.291 Area 202 1 42 48 476 913 2108 4162 8473 22878 41708 56477 170 424 619 2284 63 373 398 22863 15981 530 989 2289 4761 8949 22364 42068 55588 I'lags bb bb mm MM MM bb bd bd bbX bbX bbX mm bb bb bb mm mm mm bb bb bb bb bb bb bb bb bbX bbX bbX Conc. '.-56 0.00 0.93 4.74 9.8@ 23.71@ 41.57 97.61 265.05 483-87 655.48 1.18 4.13 6.40 25.75 0.00 3.55 3@83 264-S! %Dev -8 -6 -5 -3 5 -4 -3 2 5 1.04 5@37 10.70 25.80 54.53 103.19 259-08 488.05 645.14 3 7 7 2 8 -15 page 2 soup 020199: Quantitated and printed by ias on 11/01/99 Quantify Compound Summary Report a co@fi@tion TOX145-tween 80 dos for POAJL, PIPOS, & FOAA- Oxt. 10/29/99 ias S&Mle List: Last modified: Method: L.ast @dified: Job Code: C: \VASS LYNX\ SOUP020199 -PKO\SAUW'&DB\102999& rri Oct 29 10:23:59 1999 C:\KKSSLYNX\soup02Ol99.prO\K*thDB\102999& No@ Nov 01 06:21:40 1999 Printed: Mon Nov ol 06:47:34 1999 CorcVound 3: PFOSA (Ch3) # N@ 1 102999co,- 102999002 1OZ999003 '02999C)04 @0299900@ 1029qgOO6 E 102999008 9 IC2999010 1029990'1 :Z 1029990'.: 1OZ999014 15 1-0-1999015 l@ .0:999016 .7 10-999017 13 102999018 19 102999019 Z3 1OZ999020 2: 1029990,1 io29990-1: 23 102999OZ3 @4 io2999014 :5 102999025 2@ 102999026 '7 '.,2999027 :3 102999028 29 IC2999029 SmMlelist T"t MEOH Blk MEOH Blk FCM..-99086-43-1, rcmix-99086-43--, FCM,.-99086-43-3, FC:M@x-99086-43-@, FCMix-99086-43-5, FCM,x-9908@-43-6, FCM@x-990S6-43--, FCMix-9908o-43-8, FCM,x-99086-43-9, Ippb- 9/@0/99 RWW 5ppb- 9,:0/99 RWW loppb- 9,"@0/99 RWW 25ppb- 9/10/99 RWW 50ppb- 9@.0/99 RWW 100ppb- 9,'10/99 RWW 25oppb- 9/'0/99 RWW 500ppb- 9/-0/99 RWW 750pp.- 9/'-0/99 RWW MEOH Blk TOX@45-PFOS/PDA,;, - T@-@-d..e-2ppb- 10/29/99 IAS T@,Xl45-PFOS/POA.A In T@"@---4PPb- 10/29/99 IAS FCM,x-99086-4-@,-4, 25ppb- 9"0/99 RWW M.CH Blk TOX145-PFOSA In Tee n-dose-200ppb- 10/29/99 IAS TOX.45-PFOSA in Tween-- -300ppb- 10/29/99 IAS FCMix-99086-4i3-7. 250ppb- 9/10/99 RWW MEOH Blk FCM,x-99086-43-1. FC M@x-99086-43-2, FCM.x-99086-43-3, FCM,x-99086-43-4. FCM@x-99086-43-5, FCMix-99086-43-b, FCMix-99086-43-7, FCM@x-99086-43-8, FCM,x-99086-43-9. lppb- 9/10/99 RWW 5ppb- 9/ID/99 RWW 10ppb- 9/10/99 RWW 25PPb- 9/10/99 RWW 50ppb- 9,'10/99 RWW 100ppb250ppb500ppb750ppt- 9/10/99 RWW 9,'.3/99 RWW 9/10/99 RWW 9,'0/99 RWW Type Standard Stands rd Standard standard Standard Standard standard Stan dard Stan dard cc QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Co= 1-01 5.03 10.10 25.10 50.30 101.0() 251.00 503 .00 754.OC 25.lC 251.00 1.01. 5.03 10.10 25.10 50.30 101.00 251.00 503.00 754.00 RT 7-833 7.79C 7 741. 7.809 7.803 7.805 7.766 7.809 7.85"7 7.895 7 .941 7.982 7.920 7.969 7.994 7.989 7.943 7.950 7.964 7.990 7.947 8.003 7.988 7.948 7.942 7.965 7.99: 7.989 @9i7 Area 18209 835 1102 1881 2710 6408 10741 21634 68915 139095 199487 IAC 7@1407 73318 8797 596 72510 105109 75327 870 783 1994 3433 8204 14786 30309 76998 140797 20'774 rlag. MM MM mmx mmx MM MM mm MM MY. MM bL@ PWI bb bb mm Mll. bd db MM MM 19-L% 14tLK MM MM MY, M Ml-, MM MM cone. %Dev 66.1@ '.3 3.30 6-16 9.-,. 2@1.80 38.71 78.74 25,'.44 510.2S 73Z . 15 7...' 2:1 23 -9 -9 -2', -3 26S .27 268. 62 31.51 26 i.44 265.61 385.42 27@.00 .45 2.13 6.58 10 111 31 i- 29.39 1- 53.58 7 110.61- .C 28--l.4 1-1 516.53 740.5@ Vag. 3 Soup 020199: ou@titated and printed by is. .. 11/01/99 ouantify compound Summary Report TOX145-t@en go dos. confir@tio. poM, pros, & poAA- ext. 10/29/99 i&S for Sample List: Last modified: Method: Last modified: Job Code: C:\MMSLYHX\SOUP020199-Pro\SaMlODB\102999& rri Oct 29 10:23!59 1999 C:\MXssLy=\soup02Ol99.pro\NzbDB\102999& Mn N- 01 06:21:40 19 9 Printed: M.. so@ ol 06:47:34 1999 CorWourid 4: IS (M4) N- 2 @0299900: 3 -02999,10-@ 4 10299900d 5 102999005 1.0299900@ io:999028 1-@2999003 io:9993c, .@2999@:. .@:9993i: '.3 1.02999013 1. 10.1999014 'S 1OZ999015 i@ 10'999016 17 1029990'7 18 10 z 9 9 9 0 18 19 io2999019 102999023 2i 1029990-1. 1029990Z-' 23 102999023 24 10-.99902.A 102999025 26 102999026 2- 10-1999oz:8 10:9q9lzs 29 '02999229 SampleliSt TeXt MEOH Blk MECH Blk FCMI.-99086-43-1 FCMIX-99086-43--@, FCMIX-99086-43-3, FCM@X-99086-43-4, Fcmlx-99086-4',-@ FCMIX-99086-43-6. F,-Mix-99086-4@-7, FCMIX-99086-43-- FCMix-99086-43-9. MEOH Blk TOX145-PFOS/PCAA TOX145-PFCS/POAA FCM,@H-9a9l0k86-43-4, MeO TOX145-PFOSA in TOX145-PFOSA in FCM-x-99086-43-7, MEOH Blk FCM,x-9908b-43-., FCM --99086-43-., FCM@.-99086-43-3. Fcmlx-990B6-43-4, FCMix-99086-43-5, FCM,x-99086-43-6, FCM@x-99086-43-7, FCM@.-99086-43-8, FCM@x-99086-43-9, '@PPb- 9/10/99 RVr.4 5ppb- 9 10/99 RWW loppb- 9/10/99 RWW 25ppb 9/10/99 RWW 5oppn- 9/10/99 RWW 100ppb- 9/10/99 RWW 25oppb- 9/10/99 RWW 500ppb- 9/'0/99 RWW 750ppb 9/10/99 RWW in Tween-doze-2ppbin Twee@-=-App.- 10/29/99 IAS 10/29/99 IAS 25ppb- 9/10/99 RWW Twee@-do.e-200ppbTween-= -300ppb- 250ppb- 9/10/99 10/29/99 IAS 10/29/99 RWW IAS lppb5ppbloppb25ppb50ppb- 9/10/99 9/10/99 9/10/99 9/10/99 9/10/99 RWW RWW RWW RWW RWW 10oppb250ppb500ppb750ppb- 9/10/99 RWW 9/10/99 RWW 9/JC)/99 RWW 9/10/99 RWW Type Stan dard Standard Standard standard Standard Standard Standard Standard Standard QC QC St andard Standard standard Standard Standard Standard standard Standard Standard Std Conc RT 7-170 1.00 1.00 1.00 i.00 1.00 1.00 1.00 _.oo 1.0() 7.082 7.147 7-095 7.099 7.104 ".101. ",.128 7.120 7.145 1.00 7.169 7.150 7.163 1.00 7.147 7.1511 7 .146 1.00 i.oc 1.00 i.00 1.00 1.00 1.00 1.00 1.00 7.127 7.163 7.168 7.174 7.145 7.147 7.174 7.146 7.146 Area 15 rlags bt 4292 4'@89 4424 4486 4446 4093 2630 1993 1842 bb bb bb bb bt) bb bb bb bb 2613 bb 1041 bb 2305 bb 2529 bb 1016 bb 1991 bb 2320 bb 2361 bb 2396 bb 2274 bb 2435 bb 2181 bb 2059 bb 1934 bb 181 8 bb Conc. %DS@ 0.01- -99 1.48 1.49 i.s: 1.54 @.53 i.di 0.91. 0.69 0.63 48 48 sz 534 4: -9 -31 -37 0.90 0.36 0.79 O@87 0.3@ 0.69 0.80 0.81 0.83 0.78 0.84 0.75 0.71 0.67 0-63 -10 -64 -21 -13 -65 -31 -20 -19 -17 -16 -@15 -29 -33 -37 Page 4 soup 020199: N@titated and printed by ias on 11/01/99 Method Report Me thod file: Last modified Compound Printed: C:\KASSLYKX\SOUP020199.pro\MethDB\102999a.mdb Mon N., 01 06:21:40 1999 1: POAA (Chli Mon No@ 01 07:36:09 1999 Compound Name Intnernal Ref.. Q ua@t@fy T@:c Con . 0, St ndards; U::r RF.Value rgp:tek FaC or: UCIhn@ te r windtow Factor: o@togr@ mass window: POAA (Chl@ 'None] Tc Conc. A 1 000000, D-.bled @000000 I .ooo 1-0000D. R:t.ent., T-etl@l@ 1 0' ion T RR-7' te ' ereR.@eete' Time fwindow (mins): Peak Selection: 7 173, -d O@000, EDni&sb&lbld (None] 0.312 Nearest R:spons:,Type: R spons Polyntomifal Type Po'n 0, F We 0 gh @tn1l 1 )LIxisTrIanst o@tion: Extemal Are. 5 Li ear Fxclude 1/X None Unit.: Peak-to-peak amplitude: 90 Smoothing: window size (scans): Number of smoths: Smoothing ethod: @nabled I Join valley threshold: Re.du e pe . llng! i.e bas:@,tnel-.-: 30.00 200.00 5.00 Dratwecvtertica threshold: D@ ., shou IdIee.rs Sh l@ler thr hold: 90.00 Dis.a00bled 30 Relative h:lght Abesolute @ght R h r:a Abs'oaltut'e r 1 50, D@:abl:d O@00, D@ bl d 2.00, D..abled 0 00. Di bled r,4 5 /.@ Page Method Report Method file@ Last -d,t@@d Compound: Printed: C:\KASSLYNX\soup02Ol99.pro\methDB\102999&.mdb mon Nov 0- 06;21:40 1999 2: Pros (ch2 Mon Nov 01 07:36:09 1999 Compound Internal Quan-ify Conc. of Name: Ref, Trace@ Standards: User RF Value: User Peak Factor: integrate window Factor: Chro@togr= mass window@ PFOS (Ch2) (None] TIC: Conc. B 1.000000, 1.000000 2.OOC) '.OOOOD. D@sbl.d Retentior. Time Relative Retention P7 Reference. Time wind.. Time Peak Selec-ion: 7.434, C.000, [N..@) 0.345 Enabled Disabled Nearest Response Type, Re.p.ns@ Polynomial Typ@: Point of Origin Fit weighting: Axis Transto @ tion: Units Externa'Areas Linear Exclude 1/X None Peak-to-peax amplitude Smootning, W.ndow size (scans Number of smooths: Smoothing method: jo,@,-v.alley threshold: Reduce peak tailing: Raise baseine maximum E)@.. th@@sh.1d@ Detect shoulders Shoulder threshold: Relative heigh@: AZS@'.,@te height: Relative area Abso'@u-e area 88 Enabled 2 30.00 200,00 5.00 90.00 Disabled 30.00 1.50, 0.00, 2.00, 0.00, Disabled Disabled Disabled Disabled Qu@tify Calibration TOX145-t@en 60 doss Report C-nf'@t@o' for POAA, PROS, & POM- "t- 10 /29/99 ias !Comp hl) ICoefficienotf Determination:0.997121 ICalibratiocnurve:10.0347 * x + 5.23213 !Response type:ExternalStd, Area ICurve type:Linear,Origin:Exclude, Weighting: 1/x,Axis trans:None 7.55e37 Response-@ 0.0 100.0 200.0 SouP 020199: Qu@titat.d and printed by J" m 11/01/99 300.0 400.0 500.0 600.0 700.0 Conc Quantify CalibratiOn RGPO- TOX145-t@on 80 dose C--t@@tiO- f-@ POAA, PROS, & POAA- "t. 10/29/99 ias lcompound2 name:PFOS (Ch2) ICoefficienotf Determination:0.996935 ICalibratiocnurve:86.0577 - x + 68.0228 IResponse type:ExternalStd,Area ICurvetype:Linear,Origin:Exclude,Weighting:1/x,Axis trans:None 6.5Oe4 Pago Response-, 0.0 SOUP 020199: Quantitated 100.0 200.0 and printed by L" on 11/01/99 300.0 400.0 500.0 600.0 Conc 700.0 Qu&ntify Calibration Toxl4s-twon 80 doze ROPOM confirmation for POAA, PROS, - ext. 10/29/99 ias & PQJLA ICompound3 name:PFOSA (Ch3) @Coefficienotf Determination:0.997261 ICalibratiocnurve:272.189 - x + 203.159 lresponse type:ExternalStd,Area !Curvetype:Linear,origin:Exclude,Weighting:1/x,Axis trans:None 2.05e5- Fag. x x Response@ x X// /X 0 X 0.0 100.0 200.0 9-p 020199: Qu@titatod and printed by i@ on 11/01/99 300.0 400.0 500.0 600.0 Conc 700.0 Quantify Calibration ROPOTOXI&S-t@on 80 does CO-fir=tiO- poAA- *xt. 10/29/99 ias fO@ POAA, Pros. & ICompound 4 name: IS (Ch4) IResponse Factor:2904-16 IResponse type:ExternalStd,Area ICurve type:RF 4.49e3- Response: Page 4 x x x x x x x 0 0.0 0.1 0.2 0.3 Soup 020199: Quantitated and printed by ias on 11/01/99 0.4 0.5 0.6 0.7 0.8 0.9 Conc 1.0 0 LaboratDryRe-poTt AnalyticalReport ofData for PFOSA PharmacokineticStudy inRats (Seraand Liver) LaboratoryReport No. FACT-TOX-145 (W2814) Requester ProjectNo. T-7132.2 Attachment E Extractioannd AnalyticaDlata ExtractioWnorksheet ETS-8-6.0 Study #7r-iv- I-YJ- Surrogate Std Matrix24Lt 'L,V"- Approx. ppm Box# ]g.@ 4qq-Xc)i@) WK/Day d* I @ i Actual ppm #q4o%-13-11 Date @piked/Analy-st ?- RBLI0139-250ppD-CCV-11-1to4 5 uL 9R03230M.Dyi.Control-250ppb-MS/1Dl 5 uL 9R 03235M.Dy4,Control2.50pob-MSID 12 5 uL FC Mix FC Mix approx.0.5ppm approx.5ppm actual ppm actual ppm #qSo&-.47-2. # ggob-*-,4 lo I?-V 10 uL 10 uL 10 uL FC Mix approx.50ppm actual PPM Comments VerifiedBy tu/A RBLI0139-H20 blk-11&12 RBLI0139-Liverbik-11&12 RBLI0139-5ppb-11&12 RBL10139-10pob-1 1&12 RBL10139-25ppt)-11&12 RBL10139-50ppb-11&12 RBL10139-100ppb-I1&12 RBLI0139-250ppt@-I1&12 RBL10139-500plob-11&12 FCI-_I,LlRBL10139-750ppb-11&12 RBL10139-1000ppb-1 1&12 9R03230M,Dyl.Contmi 9RO32 31M.Dy 1,Control 9R03232M. Dy 1.Control 9R03233M. Dy 1,Control 9RO3234M, Dy 1.Control 9R03245M,Dyl.5mg/kg 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 2 uL 4 uL 10 uL 20 uL 40 uL - 10 uL 20 uL 30 uL 4 uL -A MiA 9R03246M,Dyl,5mgikg 5 uL 9RO3247M,Dyl,5mgfkg 5 uL 9R03248M,Dyl,5mg/kg 5 uL 9R03249M,Dyl.5mgikg 5 uL 9R03235M,Dy4,Contmi 9R03236M,Dy4.Contml 9RO3237M,Dy4.Contmi 9R03238M, Dy4.Control Blank - -Rp-66 -,t L,,v,c.LiverExtractionMethod 5 uL 5 uL 5 uL 5 uL Std# Iqu3@, -/3 ETS-8-6.0 amount =j .12_ mi 3-91mi .................... Date & Initials Vortex 15 Sec. IQ, L%- qvi PipetteMatrix,spike with appropriatesurrogate or FC-Mix Pipette1 mi of0.5 M TBA, pH 10. pH= ju /o-13-'Yf Pipette2 mi of0.25 M Na2CO-,/0.25M NaHC03 buffer Dispense 5 mi ofmethyl-t-butyelther-- Volume L? Std. Std.# YYOA(, TN-A-.21,/t, mi rV- 0 9 Nil 9cl 1 Shake 20 min Shaker speed: 3vo Centrifuge20-25 min. Centdfuge speed:_i Remove a 4 ml aliquatof organiclayer Put on NitrogenEvaporator to dryness Temperature: BQgnijAmp, Add methanol Volume_L_.Q_ml TN-A-_21YL_ Vortex 30 sec. Fiiterusing a 3cc B-D syringewith a 0.2 um filteirntoan autosampler vial a-@,t@ct F &" L)av*tt'I'AAk, LAvro-@k@ C&eiV-4"" @,ft,lov-A4-,41 L L)( iCW c f or, r P@-) I'l C@D LU @zd v q "IL 6 ee @3 L 6@. so - 10/12/99DraftAttachment A ETS-8-6.0 Extractionof PFOS from Liver Form Compiption VerifiedBy 2i*@q ExtractioWnorksheet ETS-8-6.0 Study # -TC)-x- it4 s- Matrix L.;v Box q(-4?oo_ WK/Day @-@4 1 DateSpiked/Ana iyst 9RO3239M.Dy4.Controi 9R03250M,Dy4,5mg/kg 9R03251M,Dy4.5mg/kg 9RO3252M,Dy4.5mg/kg 9RO3253M.DY4,5mg/kg 7@R03254M,DY4.5mgfkg Surrogate Std FC Mix Approx. ppm approx.0.5ppm Actual ppm actual ppm ctqobf,-13-11 I-)V 5 uL 5 uL 5 uL 5 uL 5 uL 5 UL FC Mix approx.5ppm actual ppm FC Mix approx.50 ppm actual PPM Comments VerifiedBy N I P. Std# amount =-LL) mi gvml Liver Extraction Method ETS-8-6.0 Date & initials Vortex 15 Sec. /n. ; q,? Pipette Matrix, spike with appropriate surrogate or FC-Mix Volume =J 0 mi Pipette 1 mi of 0.5 M TBA, pH 10. pH= io 9&0@ac Pipette2 mi of0.25 M Na2CO,/0M.2N5aHC03buffer Std. # - 3-/ # --"A-q)qodo&q--oi Dispense 5 mi of methyl-t-butyelther Shake 20 min Shaker speed: 3oo Centrifuge 20-25 min. Centdfuge speed:_ILDO Remove a 4 mi aliquatof organic layer Put on Nitrogen Evaporator to dryness Temperature: Room T@mp, Add methanol Volume J.0 mi TN-A-@ o -lq Vortex30 sec. Filterusing a 3r-c B-D syringe with a 0.2 um filteirnto an autosampler vial /4 'iO -13-7f c;@-- 10/12/99 Draft Attachment A ETS-8-6.0 Extraction of PFOS from Liver Form Com Verified By LLtlqq Prep Date(s):10-12-99 ,Xnaivst(s)S:EE Sample '*12trixR:at Liver ,%Icthod/Revision:ETS-8-6.0 Target Anslyte(s):PFOS. PFOSA Sample ID 9RO3230M.Dvl.Control 9RO323 IM.Dy 1,Control 9RO3232M,Dyl.Control 9RO3233M,Dyl,Control 9RO3234M.Dyl,Control 9RO3245M.Dyl,5mg/kg 9RO3246M,Dyl,5mg/kg 9R03247M,Dy I,Smgfkg 9RO3248M,Dyl,Smgfkg 9RO3249M,Dyl,5mgfkg 9RO3235M,Dy4,Control 9RO3236M.Dy4,Control 9RO3237M,Dy4.Control 9RO3238M,Dy4.Control 9RO3239M,Dy4,Control 9RO3250M,Dy4,5mg/kg 9RO325 1M,Dy4,5mg/kg 9RO3252M.Dy4,Smgikg 9RO3253M.Dy4,5mg/kg 9RO3254M.Dy4,5mg/kg Summary ofmethod: Notes: Sample Weights/ Volumes Initial Weight grams t) 9 9 t, oirq 400400 0.997S /. 6/.? 1) /.C)1-71 I. 0 0 7q /,o / C7)- Study Number: TOX- 145 Equipment inumber: 0222-0900 FinalSolvent& TN Number: McOH /TN-A-2945 Matrix Blank/identirierR:abbitLiver Box: 99-200 Homogenized By: VerifiedBy: Comments I P, Used forMS/D II - I /k4t,4/-12/all" 1\)A/ I ooiq I. eap(oll I Li Used for MSID 12 IV)4 g@o 11'7 o /41-7 1:21 fly _cel- Rcvicw Date RtlIO139 Form Approved byfdate: Form Compi 1 VerifiedBYe- ir@, l,mPa.StLadudComa-T.@ P,.p A..Iy,l(,) S..rA. SEE R.. L.@@, ETS-" (I Target A..Iyoo,): F,.Nl,- Bo. N..t.,: C),)2.00 S,.dy r4..b-: TOX-145 Eq.ip.-I N..b-. 02-12,PgW F,..lSi.-t & TN N..b-. PAOKITN.A.2945 FC Mi. Sid Appr... 0 5OU pp.: FC %iiiSid App-.. 5 Ot)pp@: FC Mi% Std Appmi. 50 0 ppm: S.-.g.t.SidApp-.. 100pp.: lIX96-47--l 1)086-47.1 119095-33 9')086-13-11 ActualCmc@trusms PFOS Sid Cmc uWmL 05000 05000 05000 05000 050()0 5 ODO 500() 5 OOD 5000 ofswduds in theFC Mix PFOSA PFOSEA Std Conc Std C-c uW.L 0 $005 05050 05050 05050 05050 5 ()05 5005 W@L 04997 0 499' 04997 04997 04997 4997 4997 5005 5005 4997 4997 PFOSAA Std C@ ulVmL 04999 04999 04999 04999 04999 4999 4999 4 9" 4999 Ri..k li,-i.i4Wd-sity ig)far EIFOSE-OH Std C@ uWmL 0 5w5 05005 05005 05005 05005 5005 5005 50()S 5005 M556 Std C@ UWML 05010 05010 05010 05010 05010 5010 5010 5010 so to All A.'t Spiked mL 0002 0004 0010 0020 0040 0010 0020 0030 0004 0 163 1000 AU D@sty it 0163 0 163 0163 0 163 0,163 0 163 0 163 0,163 0.163 AU Vol mL 1 000 1 000 1 ODO 1 000 1 ODO 1 000 1 000 1 000 1,000 Cal@latedC@@ms PFOS Std C@ -ws 6 13 12 3 30 7 613 123 307 613 920 122' 1 ofSu.Ww& in s..Pi.@. PFOSA PFOSFA Std C@ Std C@@ ng/g 6 14 nsis 6 13 124 310 620 1.14 307 12,3 307 613 123 307 614 613 921 9120 1228 1226 ' PFOSAA Std C@ wg 6 13 123 307 613 IZ3 307 613 920 1227 EtFos"H SW C@ -gig 6@ 14 12.3 307 61 4 123 307 614 921 1228 MS% sw c@ nwg 6.15 12.3 307 61@5 1 307 615 922 1229 Srmpts StdCom. ghL 100 Srrepto FinalC@, nwB 3077 AD Am-t Spiked ML 0005 1 Calculated Con=@ons PFOS FinalConc nWmL 1 00 200 5()0 100 200 500 100 ISO 1 20() 1 ofstandmds PFOSA FinalC@ ngiml 1 00 202 505 10 1 20 -' 501 too 150 200 in the 1 0 mL finalsol@t wlme PFOSEA FinalC@. PFOSAA FinalC@ ngi-L 1@oo ngiml 100 200 2.0() Soo 500 too 100 200 200 500 500 100 100 ]so 150 1 200 1 200 ---- FAFOSFIOH FinalC- nl/mL too 200 501 too 200 501 100 150 200 MS% SW C@. n@VmL 10() zoo 5@01 100 200 501 too 150 200 SmpicuwdforMS/MSD MSIMSD cl@. In PFOS Fir.jC@. .g,g 301 30i 9RD3Z30KDyl IniuaiWL PFOSA FinalC@, S/g 301 301 Control (s) 0 996 PFOSEA F'uudC@ ngig 301 301 PFOSAA FinalC@ agig 30 30@ -r InitiaVl*i@ (@,L) 5 00 FinalCnlvg 10 3011 Std C@. nlvg 302 302 S. p SW C@. UW-L 100 5 ..*PC. F-umd C@ ng/mL 5(r AU A.1 Spiked ML 0005 Apprm Std C@.. S.DD ugiml Amt Spkd (mL) 0010 D-ty 0166 Smple umd forMS/MSD MS/MSD cl@ Inwi@-t PFOS FinalC- -tv 9 500 Soo 03230M. Dy I Control InitialWL Ig @. 0 996 P OSA FisdC- PFOSEA FinalC-c. wg -Wg 50 1 so 0 50 1 Soo PFOSAA FinalC- nwe 1500 00 In,t,V@.i1@ (mL) 5 00 ETFOSE-OH m FinaCl- StdC- nwg -Wa so I 1500 50 I Appm@ Std C@ 500 ug/mL Am't Spiked(mL) Fnal Vol 0010 1000 4-r%)b )@Nrt-",-k.Aa S@ple used forMSIMSD MS/MSD caic.In@x PFOS FinalConc nWg 301 301 9RO3235K Dv4. @mi ln.biWLig@ 1001 PFOSA PFOSEA Fin&JC@ FinalC@ nwg nwg 301 30: 301 30 P OSAA FinalCmc -Wg 1 10 , InitiaVlol@ t FinalC@ wg 301 301 (mL) 5 00 SW Cwg 33@0' Approx Std C@ 5 00 LLWML A.'t$Mkod (.L) D@ty 0010 0 167 S=PieuwdforMS,MSD 03235?@1,Dy4,,wuoi %iS/MSD calcin IV-, InitiWail A) I DOI PFOS PFOSA PFOSEA FinalC@ F,@.iC- F.njC- nwg nwg -nwg Soo 50 0 500 00 so 0 Approx Std C@ 500 uWmL 500 Ain'tSp-kedI mL) FinalVol PFOSAA 1 0010 1000 FinalC-c FinalC- StdC- e%L nwg wg 550 0-6-T 1.0 nws t, soIso I l@ Par Std E@u*aw Sheet h..) (Ali191 732' UE Ca C71, kA r_ cc C:r, C) C) C) C) C:) w bo bo Cko m w E E E E E EE E E r7 = = I I g@ cc a, a, c@, a, a, c@, a, 0001Go LL > E I lz ExtractionWorksheet ETS-8-4.1 Study 14 r Matrix tSt.@ Box # WK/Day d,, k,LA DateSpiked/Analyst TBS10199-25OPPt)-CCV-11-1 to 4 RTS10199-250ppb-MS/D-1 1 RTS10199-Serum Blank-11&12 RBS10199-H20 bik-11&12 RBS10199-Serum blk-11&12 RBS10199-5ppb-11&12 RBS10199-10ppb-1 1&12 RBS1 0199-25ppb-1 1&12 RBS10199-50ppb-1 1&12 RBS10199-100ppb-1 1&12 RBS101 99-250ppb-1 1&12 RBS10199-500ppb-11&12 RBS10199-750ppb-1 1&12 RBS10199-1000ppb-I 1&12 9RO3230M, Dy 1,Control 9RO3231 M, Dy 1,Control Surrogate Std Approx. ppm Actual ppm #Ctq,-@t,13-it lo-tr,-Yq -u E--- 5 uL 5 uL 5 uL 5 uL t)uL 5 uL 5 uL 5 uL 5 uL 5 uL b uL 5 uL b uL b UL 5 uL FC Mix approx.0.5ppm actual ppm #-asSL-tLq 7--@ FC Mix approx-5ppm actual ppm # 99(,riL4)-1 FC Mix approx.50ppm actual PPM #grtcq@- 33 - - 5 6L 5 uL 10 uL 20 uL -5 UL 10 uL 20 uL 5 uL 10 uL 15 uL 20 uL Comments AIIA 9R03232M, Dy 1.Control 5 uL 9R03233M, Dy 1,Control 5 uL 9 R03234M, Dy 1,Control 5 uL 9RO3245M,Dyl,5mg/kg 5 uL 9RO3246M,Dyl,5mg/kg 5 uL 9R03247M,Dyl,5mg/kg 5 uL 9R03248M,Dyl,5mg/kg 5 uL 9R03249M,Dyl,5mgikg 5 uL 9RO3235M,Dy4,Control 5 uL 9RO3236M, Dy4, Control 5 uL 9RO3237M,Dy4,Controi 5 uL 9RO3238M,Dy4,Cog,rol 5 uL Blan Serum Extraction Method Std# CtciW -A.3 Ci ETI&-4.1 amount= I-C) ml Date & Initials Vortex 15 Sec. kQ- Q Pipette Matrix, spike with appropriate Surrogate or FC- ix Volume I. C3 mi Pipette 1 mlofO.5M BA,PH 10. ph=lg- I&dlql95 Std. # q Pipette 2 ml of 0.25 M Na2C@O@0.25 M NaHC03 buffer Std. Dispense 5 mi of methyl-t-butylether TN-A- Shake 20 min Shakerspeed: Centrifuge 20-25 min. Remove a 4 mi aliquatof organic layer Put on Nitrogen Evaporator to dryness Add methanol Volume J Centrifuge speed: aiiial" I emperature: Room 0 TN-A-zZq TEMD Vortex 30 sec. Filterusing a 3cc B-D syringe with a 0.2 um filterinto an autosampler vial VerifiedBy N WA ioliqlq@ r-I A: lilirlo 114 It I rYI,4 JulIt I)k It,I)t)i i IIgigok, Cont. Cal. Verificationsused same matrix as for std curve. (P--" 10 1 k-I- 1,-t S--@ , . tv SL@- " 10/12/99 Draft Attachment A ETS-8-4.1 Extraction of PFOS from Serum Form Completion Verified /y, 41 ExtractionWorksheet ETS-8-4.1 Study#-jt@A lq"Matrix Box # I WK/Day Date Spiked/An aiyst 9RO3239M,Dy4, Control 9R03250M,Dy4,5mg/kg 9R03251M,Dy4,5mg/kg 9RO3252M,Dy4,5mgikg 9R03253M,Dy4,5mgfkg9RO3254M,Dy4,5mg/kg SurrogateStd Approx. ppm Actual ppm #1110t, 13 1, 5 uL 5 uL 5 uL 5 uL 5 uL uL FC Mix approx.0.5ppm actual ppm FC Mix approx.5ppm actual ppm FC Mix approx.50ppm actual PPM Comments 1 VerifiedBy Blank-kaAA,, t Serum Extraction Method Std# 9 clC4.,7 ETS-8-4.1 amount =--Lla-ML- Vortex 15 Sec. PipetteMatrix,spike with appropriateTurrogate or FC-Mix Volume==,L=Q Pipette 1 mi of 0.5 M TBA, pH 10. pH=_LLZ__/f@./ fPipette 2 mi of 0.25 M -Na,-CO-JO.25 M NAHCO, buffer Std. 12a&, I Std.# 222@-,Y-a Dispense 5 mi of methii:i@butylether TN-A- 924/(@, Shake 20 min Shakerspeed: 'Z Centrifuge20-25 min. Cent Remove a 4 mi aliquatof organic layer Put on Nitrogen Evaporator to dryness mperature: -Room Temp. Add methanol volume I L) TN-A-_2_y t@ ,Vortex30 sec. Filterusing a 3cc B-D syringe with a 0.2 um filteirntoan autosampler vial Cont. Cal.Verificationsused same matrix as forstd curve. Date & initials 10/12/99 DraftAttachment A ETS-8-4.1 Extractionof PFOS from Serum Form Completion Verified IBY PrepDatei!i1@0:/19/99 Angly3t(S):SEE Sample Matrix: Rat Serum Method/Revision: ETS-8-4.1 Target Analyte(3):PFOS, PFOSA Sample ID 9RO3230M,Dvl,Control 9RO3231M,Dyl,Control 9RO3232M,DYI,Control 9RO3233M,DYI,Control 9RO3234M,Dyl,Control 9RO3245M,Dyl,5mgfkg 9RO3246M,Dyl,5mgtkg 9RO3247M,Dyl,5mg/kg 9RO3248M,Dyl,5mg/kg 9RO3249M,Dyl,5mglkg 9RO3235M,Dy4,Control 9RO3236M,Dy4,Control 9RO3237M,Dy4,Control 9RO3238M,Dy4,Control 9RO3239M,Dy4,Control 9RO3250M,Dy4,5mgikg 9RO3251M,Dy4,5mglkg 9RO3252M,Dy4,5mglkg 9RO3254-1 M,Dy4,5mg/kg 9RO3254-2M,Dy4,5mg(kg Summary of method: Notes: SampleWeightsV/olumes Initial Vol. mL Ci r@nL. Study Number: TOX-145 Box: 99-206 FinalSolvent& TN Number: McOFirM-A-2945 Matrix BlankfidentirierR:abbitScniffv99062-39 Rat Scrunv'99062-88 VerifiedBy: Comments Review Date Rts10 199 Form Complct VcririedBy:@ ici im f-airStandud p "P M.,..: M,lb.VR-m.: 1 41SEE R.,S-. ETS-" ; PFOS. PFOSA st.dy TOX-145 Eq..p-, -4..b@, F,._i Sel@# & T14 Nomb@: MeOWrN-A-294S Mask TamwAdelifier. RAbbitSerum/99062-39 Rat Swumt99062-39 FC Mi. Std App-.. 0 $00 PP-: FC Miz Sid Appmz. 5 00 PPm: FC M,. Sid App-.. 50 0 pp@: s.rr.g.o@SidApp-.. loopp.: 9%86.47-2 99096-47.1 99095-33 99046-13-11 ActualConcmuwjNu PFOS Std Conc .g/.L 05000 0 5000 5000 5000 5000 5000 5000 5000 5000 of Standuds in theFC Mix PFOSA PFOSEA StdCugml 05005 05005 5005 StdC@ ug,.L 04997 04997 4997 5005 4997 5005 5005 4997 4997 5005 4997 5005 4997 5005 1 4997 Mask @m iniewvW*w 4=L) (w m@: Fi" -1-t .I.-f.L) PFOSAA SidCo- uvj.L 04999 04999 4 99Q FIFOSE-OH Std C@ @W.L _ 0,5005 05005 5005 M-4@% SidC@. uWmL 05010 05010 5010 AU A.'t Spiked L 0010 0 MI 0005 AU nitlaiVokum @L 1015 1,0125 1.010 4999 5005 5010 0010 1015 49919 5005 5010 0020 1.025 4999 5005 50 10 0005 1.010 4999 5005 so 10 o@010 1.015 4999 50.05 5010 0.015 1.02() 1 4999 1 50.05 1 so 10 1 O@020 1,025 C.1-I..dC@@ PFOS StdC@ ng/mL 493 976 24 & 493 976 248 493 735 976 ofSt..Wd. PFOSA Std C@ V).L 4 93 9 77 24 A 493 977 249 493 736 971, d. -OW @ PFOSLA sw c@@ mw'ml 492 975 247 492 97 5 247 492 735 975 PFOSAA Std Cow nWmL 4,93 975 247 493 975 247 493 735 975 LLSFWOSCFoO@H p)mL 493 977 249 493 977 243 493 736 1 977 SW*LC-@-% nWmL 494 973 24,3 494 978 248 494 737 1 973 Sarrepte Sid C@. uWmL lot S. u FiW C@@ agtl 496 AN Am-t Soked OLL 0005 Calmlawd C@=@m PFOS FinalCmc nWn,L 500 too 250 500 too 250 Soo 750 1000 of Smndwds PFOSA FinalC- nWmL 501 100 2.5 D 50 1 100 250 501 751 1001 m &a 1 0 -L ruW FFOSXA FinalC- n Soo 100 250 500 too m 500 750 999 wilmt "ime PFOSAA FinalC@. WML 300 too 250 Soo 100 250 Soo 750 1000 ETFOS"H Fi.W C@. -.WML 5.01 msu StdC-, W.L 5@ol 100 100 250 25 1 50,1 so I 100 too 250 251 Sol Sol 751 752 1 too' 1 1002 S.ropt@ StdC- UW-L 101 Swrepte Fi" C@ *WmL 503 Ain'tS*.d L 0005 too 100 AU F"W Vol. L 100 too 100 100 1,00 100 100 1@oo 100 Sa.pi. .d fw MSIMSD P@ -=I -.@.99062-" MSTMSD Co.@.inth -pi. @ PFOS FinAlC@. PFOSA Finalc@ PPOSLA FoW Co - nW.L 2 ngtml 249 241 DWML 27 2417 S-pic md fm MS/MSD RAt @1.1 5 ..SM9062-38 MS/MSD Cmc, in thefinal$Wv-t-- ?FOS StdC- PFOSA SidC- SidC- u!VmL uwml uw.L 250 250 250 250 "15'.0 I..u.V]oi-. (.,L)100 PFO FinalC@ FinalC@. 1"336 stdr@ 4ML NWML RWML 247 242 243 247 1 249 249 Iniu.V1on- (.L) IW Std C@ u.J.L 250 m StdCuWmL 250. stw -W-L 1 21 Appm. StdC@ 30 0 ugial Am@t Sinked Vol.(mL) 0,005 Appm. Sid C@. 50.OuWmL -431,%6 &- 4).@ 6 Amt Spked Vol,(.L) 0005 FinaiVoi.(mL) 100 -P,.,.nk.Lj RU10199 F@ C@plet Venfied By CD :zl 0 tri ct Z rE . cc ...... .. .. If I C> CD 0 0 0 w@ ocl 0 E w co bb E E g E E @p 0E0 @ap 0E0 E E m m00 r_ 0 e- f7 10 00 C, c:@ f-4 @j ") -1 Q CD 0 a 14 '1 C,4 C4 In -1 C> = ce w ce c@ CY. i iL Extra,:tioVnVorks@ieetETS-8-6.0 Study Matrix Box 5;@;- 2 41 Surrogite '-Std FC Mix FC Pvlix FC Mix com ents VerifiedBy Approx @)pm al@orox.0.5ppn-. @ip@)rox.p5pm approx.50 ppm ACtual/vt ppm iactual ppm !actual ppm actual pprn WK/Day Date S piked/Ana lyst z15 -F12OBlk -LiverBik-6ppt@-I 2ppt@-1 30ppb-1 -60ppb-1 -120ppt>-l -300ppt@-1 -900ppb-1 -1200ppb-1 5 0 ul 5 0 ul 5.0 ui 5.0 Ul 5.0 Ll 5.0 u@ 5.0 ul 5,0 ul 5.0 ui 5.0 ui 5.0 ul 2 ul 4 ul 10 ul 20 ul 40 ul 10 ul 20 ul 30 ul 4 ul BlankLiver ExtractionMethod_ Std# t I@i-t5-60 amount Vortex 15 Sec. Pipette Matrix, spike with appropriate surrogate or FC-Mix Volume PipeFe 0-1f ml 0.5 M TBA, pH 10. pH= 7,) le-7,@-,ZTLpIiC,y@l Std. Pipette 2 mi of 5.29 9 Fqa,U,576-25-M NAHCO@ butter Dispense 5 ml of methyl-t-butyelther Shake 20 min Shakerspeed@ J,2 D Centrifuge 20-25 min. Centrifugespeed:-LL21a Remove a 4 mi aliquatof organic layer Put on Nitrogen Evaporator to dryness Add methanol Volume it o mi iemperature@ t@oom Iemi) ,Vortex 30 sec. IFilterusing a 3cc B-D syringe with a 0 2 LIM fitteri,,taon autosamrier vial Cont. Cal.Verificationsused same matrix as fc,stc curve mi mi -941- gimi Date & initials fglAA109 10/12/99 DraftAttachment A ETS-8-,3 <t,action of PF@DE froi,.Liiver Form Completion VerifiedBy.2& 1012 Ion PoirS'tandarCdurves-*Tis3ucs P,.p D.I.Nsi: lor_sily) Analy2flS): RWW S..pie Matrix: Rabb,t L,@er M@ihod/R-ision: ETS." 0 TargetAnslyle(s):See below Box Number: 99-206 FC Mix Std Approx. 0.300ppm: FC,Mix Std Approx. 5.00ppm: FC Mix Sid Approx. 50.0ppm: SurrogateStd Approx. 101ppm: 99086-44.3 99096-44.2 99096-t4-1 990346@ 13.11 Ac@l Comentmoons PFOS Std Conc. ug/mL o@5004 05004 05004 05004 0.5004 5,004 5.004 5.OD4 1 5004 1 ofStandardsm theFC Mix PFOSA ETFOSF-OH@ StdC@ Std Conc ugml ugiml 0500() 05000 05000 05000 05000 o@5000 03000 05000 0,5000 0.S" 5@000 5.000 5,000 s.ow 5.000 5.000 50,00 1 50,00 S,M556 d Conc ug/mL 0.5000 0.5000 0.5000 0,500() 0.5000 5@000 5.ODO 5.000 50@oo CjdculateCdommusu@ PFOS Std C@. ng,g 6.14 12.3 307 61 4 123 307 614 921 1229 of Sundardsin the@ple =t= PFOSA ETFOSE-OH StdCom. Std C@ nwg ngg 6 13 6.13 12 3 12.3 30,7 307 61.3 61.3 123 123 307 307 613 613 920 9r2O 1227 122'7 1 MS$6 StdCmc. agig 6.13 12.3 30.7 61.3 123 307 613 920 1227 Study Number: TOX145 Eqwipment Number: Final S@l,.ni & TN Nuber: Rabb,t LiverPNOS&13-5 MtOHfTN-A.MS M570 Std Conc. u@VmL 0,5000 05000 05000 0.5000 O."W 5.000 5.000 5.ODO 50.00 M570 Std C@@ nwg 6.13 12.3 30,7 61@3 123 307 613 920 1227 Blank livtirnitidaelnsity(g)form"n: Finalmimi "ionic(mL)form-u: MEFOSE-ON Std Conc. ugiml 0,5000 o@5000 o@5000 0.5000 0.5000 5.000 5000 5.000 50.00 POAA Std Cmc. ugiml 0.5000 0,5000 0,5000 0.5000 0.5000 5.000 5.000 5.000 50.00 PFHS Std C@. upVmL 0.50DO o@5000 0S" 0.5000 0.5000 5.000 5.00() 5.000 50.00 0 163 1 000 All A.'tSpiked mL o@002 O.OG4 0010 0.020 0,040 0.010 0.020 0.030 O@004 All Des,ty 9 0.163 O@ 163 0.163 0,163 0.163 0.163 0.163 0.163 0.163 All Vol mL 1000 1,000 1,000 t00() 1.000 l@000 1.00() 1.000 1.000 MEFOSE-OH StdC@. ng/g 6.13 12.3 30.7 61.3 IZ3 307 613 920 IZ27 POAA SidCmc. nWg 6.13 12.3 30.7 61.3 123 307 613 920 12-17 PFHS StdC@. nwg 6.13 12-3 30.7 61.3 12.3 307 613 920 1227 Surropm Std C@. ugml 101 Surrogate FinalC@. nwg 8 All Ain'tSpiked InL 0,005 CalculateCdoncentrationosf Sbumiardsinthe 1,0aiL fiawsol@ntwi=e PFOS PFOSA ELFOSE-OU M536 FinalC-@. FijW C@ FinalC@. Fmaj Cmc. ngiml 1.00 ng/mL 1 00 ngtml 1.00 ng/mL 1.00 2,00 2.00 2.00 2.00 5,00 5.00 5@oo 3.00 10.0 10.0 10.0 10.0 200 200 20.0 20.0 500 50,0 50.0 50.0 too 1()0 100 100 130 150 150 150 200 1 200 1 200 1 200 1 M570 FinalConc. ag/mL l@()O 200 500 10@o 20.0 50.0 too 150 200 MEFOSE-OH Std Cmc. ngi 1.00 2.00 500 10.0 20,0 30.0 100 150 1 200 POAA StdC@. nwml 1.00 2.00 3.00 10.0 20.0 5t0o.o0 150 200 PFHS StdC@ ng/mLL 1.00 2.00 5,00 to 0 200 50,0 100 150 200 Surrogate Std Cmc UW-L 101 Surrogate Fin.]Con@. agiml 505 All Am*t Spiked mL o,oor- Smplc usedfor.V&MSD MS/MSD caic.Inmatrix PFOS FinalCom. nWg 300 300 No MS/MSD InitiWatl (s):1.000 PFOSA ETFOSE-OH FinalCom. FinalConc. agig agig 300 300 300 300 M536 FirW Cmc nwg 300 300 S@pic u@d forMSIMSD MS/MSD calcI.n wi@t PFOS FinalConc. ngig 50 50 No MS/MSD ImnalWt, (g):1.000 PFOSA ETFOSE-OH FinaJConc. FinalConc. ngig ng/g 50 50 50 50 .4356 FinalConc nwg 0 "0 InitiaVlolume (mL): 5.00 e FinalConc. Std Conc. ngig -gig 300 300 300 300 lmtialVol@c (mL): 5.00 M570 MeF SE FinalConc. Std Com. ngig ng/g 50 50 50 50 6.00 Std C@. 08/8 '30.0 600 AA Std Conc. ngig 50 50 Approx. StdCooc.:5.00ug/mL Ain'tSpiked(mL) PFHS Std Conc. 0,010 ng/g 300 300 D@ity 0,167 Approx.StdConc. 5 00 ugiml Am'tSpiked(mL) 10 Sid Conc nwg 50 50 FinalVol. 1.000 IPSE-10259L@@-99096-44-1.@i, ExtractiVoVnorkstieeEtTS-8-4.1 Study x Matrix Box WK[Day DateSpiked/Analyst -H20BIk - P -SeraBIk- 1 -5ppb -/ -10ppb - I -25ppb-50ppb -T--100ppb, -250ppb-- 1 -500ppb 1/ 750ppb SurrogateStd Approx PPm Actual ppm .@:Cmix arprox.0.5 pprn I@ctual ppm FC klix FC Mix approx. 5 ppm approx.50ppm actual ppm actual PPM vf,-2- 5@O 5 ul 5.0 u! 5@O ui 5.0 ul 5.0 u! 5.C)Lli 5,0 ul 5.0 ul 5 0 ul 5.0 ul K)iA 10 ul 20 VOIA 5 ul 10 ul 20 ul JA 1%)Ig lie 5 ul 10 ul 15 ul 20 ul Comments VenfiedBy Blank::@i .9.t= @lr2 Std# TA4,4-,Z ETS-8-4.1 Vorte1x5Sec. PipettMeatrisxp,ikewithappropriastuerrogaotreFC-Mix amount Volume r,, mi mi PipeFelmlo-fo.5mTBA,pHlO. pH=Le PipeFme-21 of0.25M Na2CO3/0-25 M NAHCO, Dispense 5 ml of methyl-t-butyelther- putter Std@ 2EOL-/4t-P TN-A- Shake 20 min SriaKer speed: Jc@'c Centrifuge 20-25 min. Centrifugespeed@_j @.,Oc) Remove a 4 mi aliquatof organic layer Put on Nitrogen Evaporator to dryness iemperature. EDDm-TgmiL Add methanol volume7-@@ @-TN-A- Vortex 30 sec. Filterusing a 3cc B-D syringewith a 0 2 L;m filternto an autosameler vial Cont. Cal.Verificationsused same matrixas fc,s,,2curve. Date& Initials 10/12/99 DraftAttachment A ETS-11--4 i ictionof PF--,S Irc)rSierL]M Form Completion VerifiedBy -@- lo i S,.Iff lmPaiSrtandarCd@c@Flu,ds Prep D.I.4.1: A..Iy.,(.): S..Pi. matrix: .MethocltR"ison: ILV25/" RWW Rabbit ETS-8-4 I T.rZet,%nalyiels): Below B.. 99-206 FC,Mis Std Approx. 0.500 ppm: FC Mi. Std App,..@ 5 00 ppm: FC Mix Std Approx. 50 0 PPM: Surrogate Std Approx. 101 ppm: 9909&44-3 99096-44-2 990$F II I 99096-13-11 AcnW Conccnwwons PFOS Std Cmc ug/mL 0 50DO 0,5000 05000 5000 5,ODO 5 DDO 50.00 50.00 50.00 50,00 of Standards m the FC %iix PFOSA Std Com ug;ml 05000 05000 0 50DO 5000 5,000 5.ODD 5000 50,00 50.00 50,00 ETFOSEOH Std Com ugtml 0,5000 0.50DO O@-SODO 5@000 5000 5,00() 30,00 50.00 50.00 50.00 M536 td Cmc, ug/mL o@5000 0.50DO o@50()O 5@ODO 5.000 5.000 50.00 50.00 50.00 50.0(7 CalculatedCoacmtmtiom PFOS Std Cmc. ng/mL 4VALUE' 4 93 976 24 8 49.3 97.6 248 493 735 1 976 1 of Standards0 the $=Pie n=u ETFOSKOH Std C@ rngiml #VALUE'--- Std Conc. nghml WV-@IUE! 4.93 9@76 24,9 493 97,6 249 493 735 976 4.93 9@76 24.9 49.3 97.6 249 4913 735 1 976 M536 Std C@- ag/mL #$VALUE! 4.93 9.76 24.9 49.3 97.6 248 493 735 1 976 Study Numb@@: TOX IAS Fquipmmt Number: F-,.aSiolvent& TN *..@b., M@OIIITN-A-2945 Blank T"asueAdentifter:Rabbit SerwTNA-2392 Blank mmm initiavlolume ImL) forCu"=: too Finalwivmt volume (mL) for"ma: 1.00 M570 Std C-., uWmL 05000 O,M 0,5000 5000 3,0()0 5@000 5000 50.00 50.00 MEFOSEOH Std Conc, ug/mL 0.50DO 0.50DO 0.5000 5.000 5.000 5.00() 50.00 50@oo 50.00 POAA Sid Com. ug/mL 05000 0,50()0 0 50DO S.ODD 5,000 5.000 50.00 50.00 50.00 50-00 1 50-00 1 3000 PFHS Std C@ uWmL 0.5000 o@5000 O@50DO 3,000 5.ODO 5.000 50.DO 50.00 50.00 50.00 All Am't Spiked mL 0.010 0.020 0005 0.010 0.020 0.005 0.010 0.015 0.020 All initiaVlolume mL O$VALUE' l@015 1.025 1.010 1.015 1.025 1.010 1.015 1.020 1.025 All Final Vol. L l@000 1 000 1.000 1,000 1.DOO 1.00() I.ODO l@000 1.000 1.000 M570 Std C@. ng/mL #VALUE! 4,93 9.76 248 49,3 976 248 493 735 976 MEFOSEOH Std Conc. 01@ZUEL! 4,93 976 24.8 49@3 97.6 248 493 735 976 POAA Std C@. 0 ogi-L VALUE! 4.91, 9@76 24.2 49@3 976 242 493 733 976 PFHS Std Cmc. ngtml #VALUE! 4.93 9.76 24.8 49.3 97.6 248 493 735 976 Surrogate Std Cwc. ug/mL 101 Surrogate FinalCom, ng/mL 499 All Am't Spiked mL0005 CalculatedCmccnmwons PFOS FinalC@. .g/mL OVALL;E! 5 00 10.0 2.50 50,0 too 250 500 750 IODO OfSuu2dw& PFOSA FinalC@ ngi-L AVALUE' 5,00 100 25@O 500 100 250 500 750 IDDO m ft 1.0mL fi0fiwdi@mt volume ETFOSEOH F" M55C6onc. Fumd Cooc. ngi-L $IVALUE! nwml $$VALUE! 5.00 5.00 10.0 Z5.0 50.0 100 250 10@o 25.0 so@o 100 2.50 500 Soo 750 730 1000 1000 Fuu-j45C7o0w ng/mL $$VALUE, 500 100 250 500 1()0 250 500 750 1000 MEFOSEOH S @rL $$VALUE! 5@oo 10@o 25,0 so@o 100 250 500 750 1000 POAA Std Cooc. ngtml #VALUE' 500 100 25,0 Soo 100 2.50 500 750 1000 PFUS Std Conc. ngtml #VALUE! 5.00 lo,o 25.0 so,o IDO 250 500 750 1000 Surrogate Std C ug/17 101 Surrogate FiradConc. nWmL 505 All Am't Spiked ML0005 Smplc @d forMS/MSD: No VLVWD MSIMSD C@. inthe@pi@ um PFOS Final Conc@ ng/mL 249 249 PF SA F" Conc. ng/mL 249 249 S=ple used for MS/MSD No %iS/MSD ,MS/StSD Conc. in the fumd solvmt PFO Std Com. ug,ml SidC-, uWmL 250 250 i5o 250 F-uW Cmc. ng/mL 248 249 Std C@. uWmL TO InitiaVlolume (mL): 1.00 a EOH FinalCoric. FinalConc. Std Conc. ng/mL nWmL ngml 248 248 249 248 249 249 2.00 POAA Std Conc. nWmL 248 248 lmtialVol@e(mL): StdC-, uWmL 250 250 Std Coug'ml 250 250 1.00 SEOH Std Conc. ug/mL 250 250 2 00 POAA Std C@, ul;;.L 250 250 Approx- Std Coac-: 50 ug/ml Std Cmc. ag/mL 248 249- Am't Spiked Vol.(mL) 0005 Appro. Sid Cmc Std Com. ugiml 250 230 50ug/mi Ain'tSpiked Vol.(mL) 0.005 FinalVol,(mL) 1,00 ir4a d nj 10% 6, IFSE-10259Su-99096-44-1 %is ioii ['repI)atc(K): SAmple Nlgtrix: Sample ExtractionSheet StudyNumber: 7@)ctlc, Equipment 'Number: Notebook# and Page: Final iolvent: fiwy ;rAl-A Procedure Detail 9'0 k)Aj 77-.,, tAd d iio IJ /-, 74.41161al-Ac* A "."E M".Q@ FOA-*ZPr6S -r@5 7-2) N,09'4 -13-Yl J61 gp. 7bA* 3@'/ca 7)@e-IC?aA.4 (..,4w w., -L11, At., I ARA., >c /,ooo A., y A)o,!, K 6 ./,oo 2!. 1- )&(.41;" 4 7Z. MS777). E\traction-TIeniplate Re@iewDate- EmporeExLractionP3.xis Page It)l 1'rtp Sample %intrix: .%Icthod/Revision: 'FargetAnjilyte(s):?@;'$/tftAA F- P;:;21^ @-o54 .A0.4 Sample ExtractionSheet Study Number: 74K /Yg Equipment Number: Notebook# and PaLe: Finalsolvent: -XA-Zft-? Procedure Detail 'I'S"C.@ d(I IL liwl 0.44 VeA^4.c 6-1 4.@57/,s A a.@-A Li 44. 7( 7r, IA --tld IJ-ffZ 0./-/00 Yr," Z&A_A OCO 31'r -x n.166AmL ftl 1,3 F.xtractioiIiT-emplate Revic%@ Date Empt)rcExtnctionP3.xls PageIof*_ Prep Dsf@il): Sarnple Matrix: 7-k@-,- rsrget %nalyteis)F:-Y";.4 Procederv D*tgil ?';:7-.!;A 5ample ExtractionSheet SomiJy '4*tnber, Equipment '4wmber* @14atabookO and Page Findl Saiven(: ir,)--A - LM-F .2 i,a- clp 7T- ee,, -7/.o 'PC-I JPllA -A/'IV l@b" io -L Ats 4 071 /604g@ x O.Z,70-t- x 0- Vo-z-_ .72 Zoo 4.L All 4, /,00 -7i@lf E%tractium-1 Tcmpiatc Rc@,c- Da(c Ectr-iction%Is Forr.n-kpprovedby,L)ate ExtractionWorksheet ETS-8-4.1 Study Matrx fLIL-$= agLA-q.CL-= WK/Day Day 29 Date Spiked/Ana lyst -@BSl1039-25OPPtl-CCV9&10 C- RTS11039-seraBik-9&10 Fw-i@-fTTS-11039-250ppt@-msg RTS11039-250ppb-MSDiO RBS-1 1039-H20BIk-9&10 RBSI 1039-SeraBIk-9&10 RBS1 1039-5ppt>-9&10 RBS11039-10ppb-9&10 RBS11039-25ppb-9&10 RBS1 1039-50ppb-9&10 RBS11039-100ppb-9&10 RBS1 1039-250ppb-9&10 RBSI 1039-500ppb-9&10 RBSI 1039-750ppt@-9&10 Fti RBS11039-1000ppb-9&10 9R0324OM-0-Day 29 9RO3241M-0-Day 29 9R03242M-0-Day 29 9RO3243M-0-Day 29 9RO3244M-0-Day 29 9RO3255M-5mgfkg-Day 29 9RO3256M-5mglkg-Day 29 9RO3257M.5mgfkg-Day 29 9RO3258M-5mglkg-Day 29 9RO3259M-5mgikg-Day 29 Blank: Rabbit Sera Seru Extraction Meth2d- Surrogate Std Approx.100ppm Actualictppm #2EP@@ FC Mix approx.0.5ppm actual c- ppm # C@@- q @,A FC Mix approx.5ppm actualc.r- ppm # 1117,1"3(-,q -7-1 FC Mix approx-50ppm actualc@@c:ppm 'lqOq5 - 3 @5 .,> VLAbf 1 10;14@ 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL Std#-o-ilo to 10 uL 20 uL - 5 uL 10 uL 20 uL - - amount 5 uL 10 uL 15 uL 20 uL mi Date Comments LA ;Ilo; i 4@@ & Initials Vortex 15 Sec. PipetteMatrix,spikewith appropriatesurrogateor FC-Mix Volume i.0 ml la", Pipette1 mi of0.5 M TBA, pH 10. pH= Ir) Iliitg Std. Pipette2 mi of0.25 M Na2CO310.25 M NaHC03 buffer Std. os Dispense 5 mi of methyl-t-butyelther Shake 20 min Centrifuge20-25 min. TN-A- 6uqL,2 Shaker speed: 300 Fm- peed: 3500 mm Remove a 4 mi aliquatoforganiclayer Put on NitrogenEvaporatorto dryness Add methanol Volume'.U Temperature: Room Temp. ml TN-A- Vortex 30 sec. Filteursing a 3cc B-D syringewitha 0.2 um filteirntoan autosampler via[ Cont. Cal.Verificationussed same matrixas forstdcurve. VerifiedBy r@ila 1, 1131; @J I x@, FN-1: The MS/MSD and associatedsera blanks were taken from controlratsera TCRCIQC@'I -5C @O lc t%cec\ ctflel( Ct 10/12/99 DraftAttachment A ETS-8-4@l ExtractionofPFOS from Serum Form Completion VerifiedBy lotiPairStandardCumes.-Scrum Prep Date(.): 11/03/99 ,knalyst(s):MCH Sample,%Iatni: Rat Sera Niethod/Reviswn: ETS-84 I Tartet Anslytgls): PFOS. PFOSA Box Number: 99-208 Study Number: TOX 145 Equipment Number: FinalSolvent & TN Number: McOH TN-A-2997 Blank Tissue/identirser:Rabbit Sera TCR99062-94 FC Min Std Approx. 0.500 ppm: 99086-47-2 FC Mix Std Approx. 5.00 ppfn: 99086-47-1 FC Mix Std Approx. 50 0 ppm: 99095-33 Surrogate Std Approx. 100 ppm: 99096-13-11 Blank serum initiavlolume (mL) forcurves: F-inalsolvent volume ImL) forcurves: 1.00 1.00 Actual Concentrations of Stanct2ri inthe FC bkx PFOS PFOSA PFOSAA ETFOSE PFOSEA M556 All All All Std Conc, Sid Cmc. Std Conc. Sid Conc. Sid Conc. Std Conc. Am't Spiked InitiaVlolum Final Vol. ug/mL ugiml uWmL ugml uWmL ug/mL mL mL mL 0.5000 0.5005 O@4997 0.4999 0.5005 0.5010 0.010 1.015 1.000 0.5000 0.5005 0.4997 0.4999 0.5005 0-5010 0.020 1.025 1.000 ti 5.000 5.005 4.99', 4.999 5.005 5.010 0.005 1.010 1.000 5.000 5.005 4.997 4@999 5.005 5.010 0.010 1.015 1.000 5.000 5,005 4.997 4.999 5.005 5.010 0.020 1.025 1.000 50.00 50.05 49.97 49.99 50.05 50.10 0.005 1.010 1.000 50.00 50.05 49.97 49.99 50.05 50.10 0.010 1.015 1.000 50.00 50.05 49.97 49.99 50.05 50.10 0.015 1.020 1-000 50.00 50,05 49.97 49.99 50.05 50.10 0.020 1.025 1.000 Calculated Concenn=on3 PFOS Std Conc. ng/mL 4.93 9,76 24.8 49.3 97.6 248 493 735 976 of S--'-@ds PFOSA Std Conc. ng!ml 4-93 inthe smple matrix PFOSAA Std Conc. mg/mL 4.92 9,77 24.8 49-3 97-, 248 493 736 9r 9.75 24.7 49@2 97.5 247 492 735 975 ETFOSE Std Conc. ng/mL 4.93 9.75 24@7 49.3 97.5 247 493 735 975 PFOSEA Std Cone. ug/rmL 4.93 9.77 24.8 49.3 97.-7248 493 736 977 Nt&% Sid Conc. ngtml 4.94 9.78 24.8 49.4 97.8 248 494 737 978 Surrogate Std Conc. ug/mL 101 Surrogate FinalConc. ngiml 498 All Am't Spiked ML 0.005 Calculated Concen"6ons PFOS Final Cooc. ng/mL 5,00 10.0 25.0 50,0 100 250 500 750 1000 of Standards inthe 1.0 mL finalsolventvolume PFOSA Final Coac- ngtml PFOSAA Final Conc. ag/mL ETFOSE FinalConc. oF/mL 5.01 5.00 5.00 10.0 25,0 50,1 100 250 501 10@o 25.0 50.0 100 250 500 10.0 25.0 50.0 loo 250 500 751 750 750 1001 999 1000 PFOSEA FiiW Conc. ngtml 5-01 10.0 25.0 50.1 100 250 501 751 1001 M556 Std Conc. ag/mL 5.01 10.0 25.1 50.1 loo 251 501 752 1002 Surrogate Std Conc. ug)rrLL 101 Surrogate Final Conc. nWmL 505 AU Am't Spiked ML 0.005 Sample used for MS/MSD: TCR99062-30 MSIMSD Conc. in the sample matnx PFOS PFOSA Final Conc. Final Conc. ng/mL 248 248 ngtml 248 248 Smple used for MS/MSD: TCR99062-30 MSIMSD CGnc. inthe finalsolvent PFOS Std Conc. PFOSA Std Conc. ug/mL 250 250 uzml 230 250 PFOSAA Final Conc. ngVmL 247 247 PFOSAA Sid Conc ug/mL 250 250 lniualVolume (mL): I.DO ETFOSE PFOSEA M556 Final Conc. FinalConc. Std Conc. ngml agiml ng/mL 247 248 248 247 248 248 InitiaVlolume (mL): 1.00 ETFOSE PFOSEA M556 Sid Conc. Std Conc. Std Conc. ug/mL 250 ugiml 230 ugiml 251 250 250 251 Approx. Std Conc.: 50.0 ug/mL Am't Spiked Vol.(mL) 0.005 Approx. Sid Conc.: 50.0 ugiml Arn'tSpiked Vol.(mL) 0.005 FinalVol. (mL) I@oo h' 1 1/0 Toxl45 LL ro C, C, C, cli cq CL co C60 w u co CD 2,@ E@ E E E W) r- co a, cq r4 r4 In r-n rn rn w ce iz ExtractionWorksheet ETS-8-6.0 cl@., , ,* . , /- Study #_IOX-145 Matrix Rat Liver Box 99-211 WK/Day Day 29 Date S piked/Anaiyst -CCV-/-/-I/-L- -msMSD-H20SIk-1&2 -LiverBik-1&2 -6ppb-1&2 -12ppb-1&2 -30ppb@- &2 -60ppb-1&2 -120ppb-1&2 -300ppb-1&2 -600pp 1&2 -900ppb-1&2 -1200ppb-1&2 Surrogate Std Approx. ppm Actual/#,p/pm lilflf,5-@.se 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul FC Mix approx.0.5 ppm actual ppm FC Mix approx.5 ppm actual ppm FC Mix approx.50 ppm actual PPM 10 ul 10 ul 10 ul 2 ul 4 ul 10 ul 20 ul 40 ul 20 ul 30 ul 4 ul Comments VerifiedBy Sample numbers and weights noted on a separate page - add TO ul surrogate to allsamples. ----------- Z) Z@i 1711( Blank-/2,@), Liver Extraction Method- Std# 5;'7e) ETS-8-6.0 7/_7-_r amount ml gimi Date & Initials Vortex 15 Sec. ivjr? ip Pipett atrixs,pike withappropriatesurrogateor FC-Mix Pipefte1 mi of 0.5 M TBA, pH 10. pH= Pipette2 mi of 0.25 M Na2CO3/0 NaHC03 buffer Volume @@mi Std. #_?hZZLtyyl 7901-L 42,=dy llljelq,? -Z,. Dispense 5 mi of methyl-t-butylether Shake 20 min Shaker speed:_I.,Q_,@) Centrifuge 2G-25 min. Centrifuge speed: -J -@-0t) Remove a 4 ml aliquatof organic layer Put on Nitrogen Evaporator to dryness Temperature: do2mjl= Add methanol Volume_LL) ml TN-A- Vortex 30 sec. Filterusing a 3cc B-D syringewith a 0.2 um filteirntoan autosampler viai Cont. Cat.Verificationsused same matrix as for std curve. )if@ I \V UN 10/12/99 DraftAttachment A ETS-8-6@O Extractionof PFOS from Liver Form Completion VerifiedBy@t/tj 11 Prep Date(s):1113/99 Anmiystl3):RWW Sample Matrix: Rat Liver Method/ReVi3iGn* ETS-8-6-0 TargetAnalyte(s):PFOS. PFOSA Sample ID 9RO3240/M[Day29/Control 9RO324i/MfDay29/Control 9RO3242/M/Day29/Control 9RO3243/MfDay29/Control 9RO3244ftvVDay29/Control 9RO3255/M/Day29/Smg/kg 9RO3256/M/Day29/5mg/kg 9RO3257/MtDay29/5mgtkg 9RO3258/MfDay29/Smgfkg 9RO3259/MfDay29/5mgikg Sample Weights/ Volumes Initial WL 9 2- ?c:2 @j @/,/ 0 MQ Water mi 5 mi 5 mi Smi 5 ml 5 mi 5 mi 5 in[ 5 mi 5 in] 5mi Study Number: TOX145 Equipmeot Number: FinalSolvent& TiN Number: MQ Water Matrix Blank/ldentirteRra:bbit LiverM"86-13-5 Box: "-211 VerifiedBy: Comments ell Summary ofmethod: Notes: Review Date FoffnApproved by/Date: Weight Volume Sheet-101299.xls Form Completion VerifiedBy: ktLt41-1It,14 ion ?airStaredwdCurves-Tassucs P,.p D.I.I.): Analyst(s): Sample.@striz: t,ion: T.rg" Amlyt02): Box Number: 1R114/99 ww /"tL' Rabbit Liver ETS-8-6 0 See bCiO- 99-211 FC Mix Sid Apprei. 0.500 ppm: FC Miz Sid Appmx. 5.00 pprn: FC Mix Std Appmz. 50.0 pprn: Surrogate Sid Appmz. 101 ppra: 99086-W3 99066-U-2 99026-9& 1 9908&13.11 Actual Concmtmtions Pros Sid Cmc ugiml 0.3oD4 0.5004 0.5OD4 0.5004 0.5004 5.004 5.004 5-004 50.04 of Standards in the FC Mix PFOSA ETFOSE-OH Std Conc uWmL 05000 Sid Conc. ug/mL 0.5000 05000 0.5000 0.5000 0.5000 0.5000 0.5000 0.-%" 0.5000 5.000 5.DW 5.DDO 5.000 5.000 5@000 50.00 50.00 M556 Std Conc. uWmL 0.5000 0.3000 0.5" 0.5m 0.5000 5.000 5.ODD 5.000 50.00 CalculatedConcentrationsof Standards in the @ple matrix Pros Std Cow PFOSA Std C@. ETFOSFOH Sid Conc. MS% Std Conc. nwg 6.14 agig 6.13 ows owg 6.13 6.13 12.3 12.3 12.3 12.3 30,7 30@7 30.7 30.7 61,4 61.3 61.3 61.3 m 123 123 IZ3 307 307 307 307 614 613 613 613 921 9r2O 920 gr2O 1228 1 1227 1 IM7 1 1227 Study N@mbr: TOX145 Equipmmt Number: FinalSolvent & T74 *4umber: MeOHfM-A-2997 Rabbit Lier/9908& 13-5 M570 Std Conc, ug/mL 0.5000 0.30DO 0.5000 0.50DO 0.5m 5.000 5.000 5.ODO 5().00 Blank liveriribaldeni@ty(g)form"n: Finalwi@t volume (mL) forcumes: MEFOSFOH Std Conc. ug/mL 0.5000 O.SODO 0.50DO O.-IIOW 0.5000 5.000 5.000 5.000 50.00 POAA sw CORK. ugtml o._im 0.5000 0.5m 0.5000 0.5= 5.000 5.ODO 5-000 50.00 FFHS Std Conc. ugiml 0.5w 0.50()0 0.5000 0.5000 0.5m 5.ODO 5.000 5.000 50.00 0 163 I,ODO All Am't Spiked mL 0.002 O@004 0.010 0.020 0,040 0.010 0,020 0,030 0.004 All Density 9 0.163 0.163 O@ 163 0.163 0.163 0.163 0.163 0.163 0.163 All Vol, mL 1,0()0 100() 1.000 1,000 I.DDO 1.000 1.00() 1.000 1.000 M370 SW Conc. awg 6.13 12.3 30.7 61.3 123 307 613 920 1227 MEFOSFOH Std C@. ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1 1277 POAA Std Conc. PFELS Std Conc. nwg 6.13 ows 6.13 12.3 30.7 61.3 123 307 613 920 1 1227 1 12.3 30.7 61.3 123 307 613 920 1227 Surrogate Std C@. UWML 101 Surrnatt Final Conc. nwg 3098 All Ain'tSpiked mL 0.005 CalculatedCowzwmow Pros FinalC@. ng/mL_ 1.00 2.00 5.00 10.0 20.0 50,0 100 150 1 200 1 of Standardsin the 1.0mL fiiw solventvolume PFOSA FiaW C@. EtFos"H FuW Conc. NS% F=W Cooc. ag/iLL 1.00 ng@-L 1.00 OW-L 1.00 2.00 5.00 10.0 2.00 5@oo 10.0 2.DD 5.00 10.0 20.0 50.0 too 150 200 20.0 50.0 100 150 1 200 1 20.0 50.0 100 150 200 1 M570 Fuud Cow. ng/mL 1-00 2.00 5.00 10.0 20.0 50.0 100 150 200 M&FOSF-OH Std Conc. POAA Std Conc. PFHS Std Cow. DW-L 1.00 2.00 5.00 10.0 20.0 30.0 100 150 1 200 aw-L 1.00 2.00 3.00 10.0 20.0 50.0 100 ISO 1 200 UBI-L 1.00 2-00 5.00 10.0 20.0 50.0 100 150 1 200 Surrogate Std C@. UWML 101 Surrogate FinalC@. nW-L 505 All Am't Spiked ML 0.005 Smpic used for MSIMSD: MS/MSD catc.In m-niv Pros FinalConc. nwg 295 295 Smplc used forMSIMSD@ MSI.MSD calc.In wivmt FZC.O.S ngtg 50@o soo__ 9RO3240 Wtial WL (g): 1.TB PFOSA Final Conc@ ETFOSE-OH I" Cow. nwg nwg 295 295 295 295 M556 FuW Conc. nwg 295 295 InitiaVloi=c (mL): 3.00 K570 NEFOSE-OH Fuud Conc. Std Conc. aws nwg 295 295 295 295 9RO3240 ltW Wt. (g):1.020 PFOSA F-uw Cooc, nIV; so,o ETFOSE-OH FuW Cosc. owg 30@o 0. M356 FinalConc. r4ig 0 0 InitiaVlolume (mL): 5.DD M570 FinalConc MEFOSE-OH Sid Cone. nWg 50,0 ngig 50@o 50,0 50 0 6@00 POAA Std Conc. ngig 295 295 600 POAA Std Conc. ngig so@o --50@o Appro@ Std C@.: PFHS Std Conc. wg 295 295 5.00 ugtml Am't Spiked (mL) 0.010 Density O@169 ApproiL Sid Cmc.: PFHS Std Conc. nwg 5.00 ug/mL Ain'tSpiked(mL) 0,010 FinalVol. 1.000 0. IPSE-10259Liv-99086-44.1,xis CL@ E 0 r,4 z Ew t lw rA 6 do ba co co EEEEE C.4 C4 C-4 C4 r-z Em @o - " " CIA C,4 eq rA 09 m @% m m In 0 0 0 0 0 C71, C, cr" FACT: DATA REVIEW SUMIMARY FOIINI DALC@ DaLaAnalyst FACT Study Matnx/Timepoints; --DL@ 1 Sample LASL /0/?ffb Set-upAnalysis DateAnalyst /If JfNAI Instrument a Ann": 0 7oAA (CNI) AcceptablLemearRange-. AfA See e. ni@s LOQ: AIA R^2: AIA CalibratiCohnecks: tVA N4S/MSD: 641- ,DataS Exbwdm BLaaL AIA MatrixBlanL- NA CAL LAr@ D2t& Ik-yiewSign-Off AnalystRevkw Name /Date: TechnicalReview N./Daw: 4r::C QualitAymurance Review Name /Daw: DataEntr3- LA C, Conunents /Jusdfkations: (D 4 ipl:Ll@i AA, L/ -i*c J @'CaAL* I/ AltS-et@Jstle- llte4t#--4,,f4Ec Analyte: (Chl-I AcceptablLeinearRange: LOQ: -7eitZ I R^2: 0 71ovy@(7 CalibratCihoencks: MS/MSD: 1E)ataSUttus: E.Itd BW& lel., Mtri. Blnk. Z-1,@ D Qnimolis aler- (ou 5- d /t.,/ po 4L c.,,e Analyte: PF05,q (e4ii) AcceptablLeinearRange: @(X3 4@ @(y342@ LOQ: 1/yi ExtractedBl&nL- R^2: 0. MatrixBlank- C:alibmfiCohnecks: MS(MSD: Data Satus: eA@J4 10),Iilii zo /4(2 LAL 7,r-S-A . PO A A444a*.$ C6%4 ou ont S UAIA riL,Al-tk^ hA A. 101?.Ol" Date: Data Analyst: -1:@s* FACT StudyN: Matrix/Timepoints: Sarmic LixL- /0 17 f11. Set-upAnalysis DateAnalyst: Instrument. FACT: DATA REVIEW SUMMARY FORNI Data Review Sign-Off 'Analyst Review Nune /Date: TA6 -'Z@C Technk:aiReview N. /Do.: QuaHty Axmmuce Review Nam /Date: PC-e- Data itatrr[.Ac,Io a i)Iq Cormnenb IJusdfkations: Analyu: @rs AcceptablLeinearRAngr. AIA LOQ7. A4et R^2: HA CalibrationChocks: A(A NiS/NSD: IDataStatus: E-ct=tion Blank-- 4A Mau= BWi@- -IA Analyte: AcceptableLinearRange: LOQ: R^2: CalibratiCohnockL ExtractedBl@z/- Data Sbdw: An2lyte: AcceptableLin LOQ: R^2: Calibm* Checks: i D*:' taSann: ExtractedBi&nLMatnx Blank: LAC,[DI211%9 Qt,@tity compmad p@rY." T=45-rat @a, "Y do&,- @. 10/19/99 1= samle List: : l@t moditied U.tbod: J::t modified: C@d.: C: UDSSLTUX@ @p-r&ts -vm% Sam,.=% I algggb U" Oct 20 07:37:33 1999 c:%IWSLTNZ%.Oup-rats.p"\Ntwm\loiggsb @d Oct 20 07:36:45 1*99 Printed: W" @ 20 09:08.10 1999 CO.P-W 1: POA& (Cbl) SI N@ 19012 2 'o" 11.@3 3 100119999014 4 101999015 5 101999016 6 101999017 7 101999018 8 101999019 9 101999020 10 101999021 11 101:990022 12 101 99 23 13 101999024 5 14 1019:90026 1156 10011:9999900221a 17 1 a 199 9 0 2 9 1,9 1. 1 91,.1 . 10 101999031 2 1 10199903 2 1 0 1 9990 3 23 22 1 1 3 23 101:99034 24 101 9 999035 25 101999903076 26 101 3 27 10199903: 289 10199903 2 0 101999040 10 3 1 0 19990g4o1 42 3 2 1 0 199 33, 110011999999004443 3 5 1 0 199:045 36 1 0 1 9:9046 3378 1001199999G408&479 39 1 01 99 ')o50 40 101999051 Al 101199909502 12 101999053 43 101999OgSo4 5 14 10199 5 45 101999056 46 101999057 47 101999OSS 48 101999059 49 101999060 50 101999061 51 101999062 52 101999063 53 101999064 54 101999065 55 101999066 56 101999067 57 10199906B 58 101999069 59 101999070 60 101999071 61 101999072 62 101999073 SaMialist T@ IBlta'nk-'k MOB Ma'@o Blank K7-0038CL45S-_FRLZBSS@1@00119"99-_H5200 a BI.,.k-11, SEE :,:Ik-11. S21 7ToVXX1I4S-RTSIO'99l-gSge_rS.e 4S-RTSIO @k 11 S Blank 12 SEE 7 45-ItBSIO!99-Spp b-11, TOXI 4S-RBSIO!99-'-O ;b-11. lUn TOX145-SR_BISL1B0S1,9_901-9295pp_bS-o1pp1. - VE S SEE SEE TOn pb TCn4S-RRS10199-100 p 7=45-RBS10199-25GpPb-11. "b-l 45_RBSIOJ99_Sooppb-1,1: 199_750ppb-11 ?= 45-RASIO olgg_loooppb-11, 'MXI 4S-RBS1 Taomn Blank TOX3.145-RTS: :.I@3..: 1: TOX2,5-RTS R03232M Dyl 9103232M Dyl 7= T?O=n TOn 4 S-RTS 4,S-:RTS., 9103233m , Dyl , 9103234.M Dyl SRBSI0199-250ppb-CCV-11-1. SZE S9 SZZ SIM CAt al -10/19/:: Cotr ral :-10/1 cot@.1,-10/1 Co-t ol C..t,.01:--1I.../.I"t:: SZZ SZE En SRI SIR MOOR 4B5_ .k T 9R0323 DY4 c ut.:l -10/199/:9 TMoXl1a15- R TS, 9R03236. TOn 45:RT @ 9ROO332 ID)Y4y, Coontr 1:-1011 / 9 Control.-10/19/99 TOM145 RTS TUXI&S-RTS. S' :,: Dy4&. ntrol,-10/19/99 9RR03:239m-.4- oy , Cc.ontrol.-IO/19/99 TDXI&5-RBs 10199-25^.ppb-CCV-11-2. SRI N.OR Blank sag SZE SI&Z 3S2I9R TC=&S-RT 99:250; b-KS-11, 10/19/99 SRZ 7=45-RTSSIIOO'9-9 :505;.,4Pb-M D-11, 10/19/99 SIM TCn4S-RTS, 9RO3Z. . DY,-1 5 elk 10/19/99 SIR 9 T= 45:RTS , 9RO12464. Tonts RTS. 9103247M. Dy@@ 5 No/ko 10//1,9/:9 SZZ Dyl, 5 g kg 10 1 SIR TOX.145-RDS10199-250ppb-CCV-11-3. SEB N*QH B5latnk TOX: TS. RTS, TT"CC'Xxi 45-RTS , X145 -R@ 7c n1 15-ItT S. TC X'453-I&tnSkSS; 9;t 2 4489:.: Dy'@@ 5 .9//k9 10//199/9/91, 9RO3.' 991Rt@12SOM 9R -01235:2SYI.M: Dyl , DY4 Dy'. Dy4. 5 mg / kg 5 .9 kg I lalk" 5 w kg 10 / 1 9/99 10G/ 1 9/99 1 0,1 /" I1 9-25c;pb-CCV-11-4. SEE :22 ZZ 533 S. Szz Y.C 1 TCX'.T TCX-.'SS:RRI S :.5-RB '.0.. DYy4l'. 5S wog/ikkgg pb -ccv-ii-i, SZE SEE l1o0/ 1199//:99 SZE T@UcX. S 7ToCX145-RBSIOk'99-ico TCX14$-ROSI@*99:S@r: SEE Bl.nk:ll,. SEE TCXX145- RIrIST'@099 3- S:r. :1.@k-11 - SSZEEE M'l 15:11BS'O@ '? I-Sp:r b-l,, kSZE - 15-"S 1. 9-IC SEE TTO.Xi 45-RD 10 :11. szrz 'TC=;ZXlI.15-RISSSIO '99 --5O;p:p;b. 11, S 9 xt4s-Raslo.91,999'-slooppb:ll: SEE ITCCX'4I5-RBS10'.99-250;p 11 SEE @x,.45:RBS1019)-Socppb-11, SIR ,x,,s-RRslol99:750rpb-11. . SZE 'U 5 RBS10199 1000ppb-11 SEE 2"- standard SStandard t---@d tad&rd S tandard standard Standard 9 t..d..d standard oc oc oc oc oc SStandard Standard Standard ---Ed S.S tt--@d Standard tand@d Standard Std C- wr 1.00 1.00 1.00 1.0000 1. 00 7 7 3 7 .1,2,1 7 .08 2 7 A 7.111 7.109 7.1 0 7.1102 l' 00 1, 00 11.*00 1.00 7.1 10 7.1 11 12 7.1 7.01910 7. 11 1 7. 00 0 7. 6 7.113 7.089 1.00 1.00 7.133 7.112 7.12 7..1110 92 76 7.105 7-132 7.123 7.090 7.111 7.112 7.107 1.00 1.00 1.00 1:110 1.00 1 .0 I 00 1.000 1.00 1.000 1. 7 1094 7@O 0 7.10083 7.1 10 7 7:1113 7.110 7.113 7.111 7 109 7:.129 7 110 7.091 I 7.1 3 7:131 7,111 7 .126 7.111 7.111 7.107 7.110 LA c Fla. C- %a- 37 NK 384 M 3 a NK 3 5 mm 3 2 bb 4 3 bb 342 bb 39 bb 39 bb 51 m &2 bb 60 m 307 NK 3 bb 3 2 bb && 3, UmM 1m 29 bb 37 MM 34 NK 33 bb 30 NK so NK 56 NK 35 bb 300 bb 425 bb 360 bb &2 bb 291 bb 3 1 0 bb 200 2 609 bb 2 31 bbbb 24: bb 23 9 bb 3 bb 2: MM 3 bk. 21, bb 43@ M 37 M 34 m do mg 37 M AS mm 37 Mm S3 bb 6& bb 0.3981 0 @al I 0.83 0.99 01.7070 -12 -9 11 9 -170 -2-31 0.92 -0 0.93 -1a 1.21 21 1.00 0 1.41 41 00 .71 0 .:7 5 1:0 10.(8102 1 -293 -1 -150 -2 -19 O0 .:g -32 -.11 -11 0:.772 -1293 -284 0.96 - 1 32 0:83 1 7.256 _32 17 6286 09.052 1.00 97052 -0 1 97 4@93 6 is 0 73 S7o.11 397 393 sis -27 5 5:',', 0 92 4 -8 0 696 :34 00.6a6 -3141 1 .73 00.87 O.el 0. a 5 1:@,1 o@87 1.26 1.51 -@7 -13 -19 - -5 12 _I 7 23 516 8@p 020199: Qu@titiod &ad Printed Ly Las = 10/19/99 o@tif Comp@&ud guxmwt @4s-yvat @a, "Y I & A. @-I & a...- azz Sm,ple A&t: L@t IMMdLfied: Method: Itd: &..t Odi Job Co"; C:%KiL3SLVMX@s@p-ra@s.p_ks.Mi.DB%1019$Sb Wed Oct 20 07:37:33 1999 C:\KASSLVIM\@p-rats.pm%motb=%10199gb vftd Oct 20 07;36:48 1999 U@d OCt 20 09208'-10 1999 COMPM--A 2: PVOS (Cba) 1 91012 23 l11o001"9991910.1.& A 10 999015 5 1011999016 6 10 999017 7 1011,9:,@@l9, 9 10 199 10 1011999020 9021 11 101::9022 9023 12 1011999024 i15d 1i0ol::9025 10199:026 176 10199990027 1. 1019 'go21, 19 1019 2 20 1019990930031 21 10199 9032 10119919033 23 1." 9034 24 10 1;:9035 25 10 1 999036 26 101999037 278 1011999038 101:99039 29 9040 30 I'1l9 99 41 31 10 19999042 32 10 1999043 33 10 1999044 34 10 1999045 11 36 1o,l,:9:.900.4,76. 1. 01"l1o 49 3490 1'0011919199015.1'10 41 101999052 2 101999053 4 443 11 019990SA 1,56 1,001119999990055o65 101999OS7 4,78 1 01 99go589 19 1 1 @19999@:o 50 10 1999061 51 101999062 52 101999063 5) 1 0 1999064 54 1 0 1999065 55 1*1999066 56 10199906-7 S7 11 019990:89 I"@ :::*70 610 110011999990701 9072 62 1011999073 SM&*OMHI:Ililsltk T"t K*OH a l@k K&OIK'SlWtk SEE Tolox"@ -"-IllIl9.l.-H:@.l.11..k-11, MXI,5-xa s 10 @ e 6 ank-11 SZE x -RTSJO0 I-::Eer@@ :1..k:ll, S:E 7,ox@lll-.1s1@ 11.9_!.,"_ll@kl:12. 5 t wx 45-" SSE I'OX145-" S 10 TOX"45-Rs'slol11 P-;b-11. Z.. TIC)X!45-FLBSSIO'@@9--10;=tb 11, SEE MX145-ILBS 101'9-' pp b SEE TOX145-RDS101999-210500;pb:-l1l1:' SaZZ TOX'45-PJLS10199-SC- b 11 s TOX145 RILS101999-750ppb-11, SZE TCXJAS:RRS101 9-IOQOVpb-11, SZE MIC I'l@* TOX" RTS Tooxxids-"S: MX 145-RTS, TOX 145:RTS: 14S ITTS :R 1230M. DyYI Ccontrol -10/19/99 szs R033231.n.Dyl1,: Cc.t.rtooll:-100/19 9 s 9R03232M. /19/99 522 9R03233M, Pyl, Can t, -10/19//99 szz 9R03234.4. Dyl, Can 1: 9 99 six 7V 115-RBS10199-250ppb-CCV-11-1, *1szz-l)/l HTCe)x@C.1 4'S51-k TC I'S -:TS, 9-13321511: DYA: C.@trol:-10/19/9,9 s Ts gRo z 3 6m Dyd . control -10/19 99 SZE Tmlx&5 -RTS: DY4 control 7VZ145-RT . 9,@3 31 DY4. C ontr : -,0o,',, ZI To,.@,4 s - RTS . 9-:3:, .m,Dyt, Contraol , -10/ 191 9 9 szx TCX'@ S-RES 10'-@)-Z.'-:Ppb-CCV-11-2. 1 Z-31 1 9 NECH Al TT,OoXxI,.@A,5S_-R-TklO'99:Z!C;.Pb-KS-11. lo/:9/99 SZE TIOX,.,S_R S RTTSS l. o-9--S033 Dyll: TO@. '45-RTS, 9' 33:;,:1. Tll..14S--@,@9 ;.10324 7 -4. Dy'@, 5 ://1k0/g191/09/919,/S9UZ9 SSEtEz kg 10 1 9/9 9 5 9 sts s lO@', 1 MTl*'c4'44 52-'RTS, l@l I TC)-' 5-RTS, 9R'3-': @:1 Dy 5 lkg 110,11:1:: SSEE kg 1 0/19//99 s 7T@c:'"144S5:RRTTSS,, 99 -",!:-".! Ily4l.I lglk lo'l,", S 1 Dy . 5 g kgg t TC@..45-RTS, 0 9F33 -': 1.b DY4. 5 .9/kg i10/119/99 ssME TI::'IS-RBS1 -cc-v-il-4, sn Me-I 4 TC - B@ l,,,.', 9 ---:@ im. Dy,4. s .9//k lo//19//99 SEE Tr :,45:R-.5S, 9 2M. Dy . 5 .9 k" 10 19 99 szz S-,.S,@ cpb-CCV-11-', SZEg TM@,- -i4,5glnk T: ll:R. 1 1 mlk SEE -'l' TC: 45-RTS.0' TCC., 45-_RTB,51l0o,_ 91- :11: SEt: BI-K-I SEE s r T@ 45-RB lc..)-: ;@b-I'@,SSEE TC:@745-RBSIC"@-'@--b-l@ Er loi-4:5);pb-ll,,SZE TD@ "IS:RR:S , 1 rI- -4 _RB '0, @p@pppbb_ :llll.SEE b 11. SEE TTCI: "1.455-RB'S110."--@.;pb-11, SZE TC-:.4S-RBSIO'.--@-'-:^.Ppb-11, SZE Type Standard Staod&rd s t---@d standard S tand&rd s5 tandard t&md&rd oc oc oc oc oc tandard Sttand@d St and@d Standard tandard S t..d"d Standard Standard Btd Conc A 93 2 9 .760 4 .a30 979 .60 241.001. 495.00 79711.-00 2,2.00 2&8.00 248.00 .00 248 248.00 :.93 24:20 49.30 97.60 2493.000 719,-(0. 3 6 000 97 7.2 RT 74 7.2:9 7.24.87 7.2 7.26'0o 7.2 50 7.2 7.246 7 2540 7 2 40a 72 7.25,2 7-2 9 7.2 51 "7.-2I.9131 7.2 7.2773 7.2 2 7.270 7.247 7,274 7.2,350 7.2 2 77 7 .227,41 7.:2738 7 26.7 7 7..266 7 .21S2o 7.2 7 .2 63 7 .25S0o 7 .2 51 72 7 21g7., 7.2531 72 7.2128 7 .2t 7 .250 7 .252 7 294 7.250 7..227921 72 5 7.292 7 28 9 7:2 5 9 7 252 7.2,2 2,1 7 35 9 77 .2615 7.251 7-211 7 7.'224a96 1P." 2 AT" Flog, 134 m c@ %D0.00 31 bb 0.00 3: bb as m 1.01 1 5 5 NK 0 00 0 bb 0.000 09 UK 0.00 178 bhX l@71 -65 316 bb 1 724 bb .983 -20 2375.8 0 4 3541 bb 9 3. 2 9 225 0 bb -:7 -19 12123 2. ' 93 3 bbd '516769:*@8'7 11 -2 208020 bb 915.47 -6 0.0 &S bb UK 0.000 LkL 7: m Am 1.01 ..,Ilbb 0 00 36 bb 2710*603 11 30 M 4 9 bb O'c' a bb o@o'O 3 2 bb 0.00 37 bb 00 Al bb '840 bb 1o: 203.20900 -16 34 M 53 8 bb 231.204 11257.I 1 6916 , bb 3 141.11 4e&a i;-@D 4,0821.19 1 a3 0& bb 1'3137,.0"! 11 9 6611 bb 27 4 3 36 bbdb 7 57B9 bb 0 3165.816 761 6 bb 79647 bk, 3369. 30 3478. 8 Ck I;SL) 76820 bb 3397 1133840, bb 5017 :56@ 61 'S9 bb 266.30 7 .21 9. 1 96 MbMb al27A55l bb 399 16@':2. . L 1.50 A 6 , bb '1299 bb 2.: 09 16 0.00 0 00 12662 MbMb o@.o0o 0 .00 130 m 213 MM 368350 nbmbx @.2 0 .."8 -111 24.19 -1-2 1351 bb 53.71 9 2168 bb $9.88 1267131,6 bbbb 264.84 7 556.0a5 13 @6227 bd 7 12 3 -3 20551 bKKb 904.-45 -7 Mmp 020192: 90--ti!4*d and priiti: by ias an 10/19/99 Q@tify copou" su...,y 24=45-." s@a, day I & 4, LO/19/99 smpl a LL;t: c: %KASSLT31m\s@, -rats. pm%sawploz*%LOI*tvb L"t @" Lod u" Oct 20 07:37:33 '999 nothod: tied: C:%I@SSLTIM%"u7....r3a-s.ao"1%NMtbDS%IOLgggb &-t DdL U" Oct 20 0 :A 999 Job Cc": IP@int.d: U" Oct 20 09:OE:10 1999 CCOVOUnd 3: Vvo&L (ch3) #I ...I. 19012 2 l@ 111.@3 3 110011999999001145 5 67 1100119999:90001176 a 110 19990i9s 91 109 1l0a19999900201 11 10 19 990222 123 i10o1i19')99023 1, 1019999024 15 101,9902: 02 99'027 16 10119 'o a 1l7a 1019:9029 2 19 101;:900301 2 0 1 0 1 99:03 21 1 0 1 99903 2 22 10 I9990 33& 23 10 1 3 24 10 1:9:0035 25 10 1 9:9036 26 10 1 37 27 10 1 21 1 @:::003'9a 29 1019::040 30 101:990041 331 1100119g91g1,0o4&23 3 2 101 ...0:1 33 35 101 999046 36 1019990&7 37 101 999043 38 101 999049 39 101 9990SO 40 101 999asi 41 101 999052 423 101999053 1019990554 ,@,:990" 46 101999057 47 1019 9'0 &,ag 110011999999,005589 0 so 1019:90:01 52 1019999006623& 53 1 01999065 545 1o 199 9066 6 01':9067 5 7 1109199068 5 8 0 999069 5 9 1 0 1 991070 5601 11011999999007712 62 1011999073 S@l:IiSt T@t TY" "K*@C"HK .B1'.-.'k k MCK 145 I..k TC'- ,45:RBS@O T7C@:.14S-RTS10@ TC.@, 45-RTS TCI .45 -RBS@@.', '4 S.@_ .:Zl-aa s@z . a $22 lank-11, SEE :1&.k-ll-, Sao It -12, S ..SkEE TC S-RBSIII' SZEE TC:1-445-RRS10' --",pb-ll. S E TC::'. a S-RBS'3.- 1:@-=Pb-11 SZE T0.1 5-P.B io,-@3 @ppb-11. SEE TC)Xld5-R"lols3 53ppb- IL: 332 TO:@l&S-RSSIO !@.PPb-ll SZE TOX114,5-RDS101@@:7$Dppb-11, SRI TOX 5-RJLS101@) 1030ppb-11. SRI K.:H ll"k TC)Xl4S-RTS, 9r@3,333-"ON: Dyl: C t@ 1 9 2'-Lm DYL C"t@o "Sam TCNI:1 S-RTS: 9;z33232M. DIyyLl...Coonn ro1l.--I1O/L1I/99 SZE TTcc*)@x115S-RTS . 9RO3233M, TC::id5:RRTTSS, 9AD3234M. mtr 1 -100/11/19 SZE DYL, cCocttro 1 /L9/99 an o5l92 NeC4,a5lank TC -RTSS.. r7-,"1'14-5.TS, _RTS. s- @332 .Sm 9@, :@64: 9-:3:-'M@ : --- DDYy4&., C*.tr -10/191/:9 SER C.@tr*.'1: -1 /19 9 Sn DyA: C t@.I.-IO/19/9, Sao vy , C:ntral.-IO/19/99 393 TC::.-.5-RTS, '9 I---,.1. DY&A control 10/19/99 3= T' '15-FLBSIO* ppb-CCV-11-2, Sit- M.-.i Blank TC .*1445 -RTSJ101 ppb KS -11. 10/19/99 SITZ TC 1 S-RTS 0' 9-KSD-11. 10/19/99 SZZ T@ @. S.RTS 9 5-.4,Dyl 5 .9/kg 10/15/99 SIX TC:::45-RTS, 9- '3:*,M. DYL: 5 .9 //kkg 10/19 99 :zg TI@ :'@.545:RTSi@l9@F.;32 7.p'4. g 71: : .1R.I.S pb-DCyClV 15 1-3. Saam10 19 99 IM M, i k 1' :@455:,RtTS: 9,- 3 -.@M: Dyl, T@ TS --,:'.-^@3 Dyl. 1S 1mg91/1k;g 111./111999 "/:I1g SSIZ.II.Z 1155:R T , 9- ':---,M:DY4. i - RTSS. :3 Dyd, 15 1.91,k1.9 I.'/lill1/19 SZE 'r ;S:RR B'SSI'09' @3: :;;PbDYC4C'5 -0/kg 10/19/99 St -nd-rd Standard Standard Standard SS t&vA@d tand@d standard standard standard QC oc oc oc T' .45-RTS, 7- i.-S-RBSI@: a 3: @:LK. DyA. 5 2 Oyd, 5 P.Mb'Cll-l gs//1:: 11.00//1199/19999 SSaool g ::.55_-1RRBBSSIJCO-'_ -D 51a-k -11. Sao :11, SEE T- ':S-RTS11-- 311@.@*k 11. SSS T- -;5-R-.SIOL -E 51-k-12. T- 1 55:;.t.SBS :b-11. SZE _ zp b so -115-RgSICC'- @_5, bb:_1lI1lI,. SZZ T-' @.'S_-RFBLl'B5 1l0o'*., _:@:ppb_l Sax @5_Rg JC S T SE" '@@'S-RB 10: @45-RA "S10' TO @1.5-Ra sio'. @p pb 11 Ss ZE @ppb:ll 91 ')Oppb -11. Sao oc SS tt&VA"d SS tandard Stta&n@dd@- d Stand@ d d sS tandard st andard tandard *td o@ .93 .77 249 .80a 4979.730 248.00 493.0C0o 736 .00 977 21.. 248.00 2to.oc 00 248. 248.00 49_.7973 so 26. 49 9.30 1.70 1.0.0 736',0000 177 7.11, 7.1106 7.053 7.833 7.:329 7.a2, 7. a 3a 7. $3.3 7*,810 7,8$0142 7, all 7*809 7*01& 7: 7 OL3 7 :77 7:. 834,6 7.831 70 7 7-:37 12 7..85 7 7.8564 7.83 7..88552' 7 7.85@8 7.806 7.875@i 7. .8.13 7 791 710 7* sit 77*. 809 7 7 .:0 7951 7, 810 7, sot 7.:871549 7 .856 77.813 7 .789121 7. 7 .$85574 .851 7 .833 77..885194 7 7 .813 7.511 7.:13 7:.Ol 7 7 .791 7.88161 7 A@ rise 27259 M 53 , MM" 21,l I 1 54 m S9 mm 1 45 m 1174 NK 2 36 NK 5 0 16 mm 9 1 15 UK 165 41 M 49 79 100 6 39 NK 117&aOL OU 149225 =a 9:3 UK 3233 M 6 147 : 150 m 112 M 0341 MM 1 12 m I6"8 16,7 m 1 @61 M 431165 MmM 'a 315 m 521:L M 8750 5 5111 & dd 499046 m 3834 NK 6575 072 dk) 1255 0 m I15,,S?o,:dmd A612S Mm 1 ., nm 12128395 "bdM 50283 mm 348 mm its NK 126 120 MNK" 143 1139 NK 2063 mmmm 1 5615 mm ooti nK 10298 UK 1 NK 12213304A MM 133 3 MM C- %D13.20 2.2: 1.011 00 ..36 0 .392 .3 II 25 54 I3 47 .'9o - 7 217 1 503 11 2 585 80 -2 744 71 -240 4.55 1.41 00 .72 0 .33 0 -31 3 2441.*47 -1 0 .15 43 00.:29 0. 43 32 2150.. 27 1, 13 -13 17 213 . 32 2.@ 260.064 423564.5812 248.730 1.51 0 334.30 277.07 65 1.30 :31 7@ 28 232 -6 ,3 60.1 18.9 25D1..6379 0.322 0.1 3 0.3 9 5.2 9.1. 27.63 49.73 $9.61 254.60 83 499.43 1 7609.42& 6S. 3 -227 00%&p 020199: Q@tif @,d .d pr t by I- - 10/1,/g, a@ ify emmpc%Lnd T=45-r&t Bar&, "Y 4. Bawl* List: t@t nodified: N.th.d: L@t nodified: j.b o*": C:\MUSLYNX\20,: %led0= 20 07:'-:23 1999 C:\M&SSLY=\Sc@; -razs.p"\Moth=\lOI992b U" Oct 20 07:3':48 1999 prisktod: Mbd oct 20 Oa:C-;lG 1999 cc.p.oad 4: xs (ch4) a x@ 1 lol999012 2 101999013 1 lol99golA 4 lol999ol5 5 loL999ol6 6 lol999ol7 7 101999018 saMlelLSt Te.,t Ron Blank N*OM Blank IG&OR Blank Tox.145-kBslIo, ToxiA@-Rss @: TIDX24 RTS'@@^ Tumi&@5. -R-_;T,51.I- @-H-D.Bl-*-Ill sSzazm @-s-f -S@r. BI..k-11. SEE :Seab_ aIl..k-12, SEE a9 l10o1l9999990o2l09 io lol999o2l 11 IDo19:9D22 123 1o19990o23 1 1 19 9 24 145 lol999o25 1 101999026 16 101999027 17 10o199902: 11 1l.ll,"9I,,o23. 2 1999031 22 Ilooltg9 9Q32 lol9 990333 23, 1o 19'9903 4 256 1 01 999o 3: 2 10 1999ool7 2 78 1101199,903839 2 1019 90 29 101999o4o 0 lol999oAl 33'. 101999012 2 101999043 33 101999o44 34 lol999o45 5 101999046 36 101999904,7 37 10199 90 8g B lol99 o 39 lol9999o5o o lol9 9osi 421 ljol:999052 o53 434 1019999054 145 1019 9 9055 16 l1o0l1999990o5576 47 1019999,0589 489 ioi9 9 9 os 0 150 101 9 06 101999061 512 110199990626 ',3 1'0199191'ol' 54 lolI999o65 55 lol999066 5 6 IlDo1999067 7 99)990689 ss io 6o 59 lol9g99g9g0oo7 1 60 61 1019990772 62 101999073 71V=XI '--R:@.o iloTOXI.'5@_-RRBBSSI@::! -;iltlI- Sg I SEIE '-!:ppb-11, Sol TTooXxii.@ 5_-RRBBSS,I.C:-:-)):_ :-'.GOppo-pb mxl.- S_R&Slo: @_ '- @@OpPpb-11: $So ToxIZ5_RoSlo. 3_7,_ )opb-ii st z ppb-ii, szz TM.lOnHl -Blank TO=45:RTS : s- 3-!?M, T=45 RT's 9 11323-M. DYI, Control.-ID/19/99 Dyl. r Toxld5-RT I 1322MM: I)y1. cC *,t * -,o, SEE T=243-R-S.s, @7)32'@3 Dyl, coo.,rol.-LO/19/99 on TIOXI!5:@RTS.o@ 13^'4'Mp; Dyl,_C ntr 1,-10119/99 TOXI. BS1 1-:::, b-cev ii-l'osix NEOH 431.R@k TOXI Toxi -I7t@-, 70xl-'- S: Toxl. _@7L ,mn 41-RBS'@: @3--6m vy, oyt: CCcaonntntt0rr*..'l:-l,o9O/"119"s"g9',9 -M,. -Y4 : C..@1.1 ..4 Ily" r 1 -:1l0o,119",g9": Izxxz 3 'Y C..tr I lo I sn b-CCV-11-2, TKO.XOIH 3187.1 TOoXIi.:3R7IZt._- xi TOX145:,RTL. TIox.14 3 ,-s, 7OX145 ESI IMOR 3 Toxl.@ R-1s, 70%1. RT@. 7loXI4 TO X.1 @ :R7S MX,@@ RS: : ---,PPpPbb-KS-11, 10 9/ -KsD-11, la/19/99 su :3:,*5M. DYL: 5 no//kg 10/191/99 SU Dyl , 5 kg la 19,99 mm I)Yl 5 ::Ikg le 19 99 SEX @--@3PPb-CCV-11-3. SEE 2,14 Dyl, 5 q/kg lo/19/99 sn @4@. Dyl, 5 @gkg loO/19199 S :--', DYA 'kg o,/,9",g s . @'-'M. Dy4, 5 @glkg 10119/11 SIM -:.--rpb-CCV-11-4, SEX NoH TID XI TOXI-4 Tom 1 ------ @:lM. Dyt. 5 mg//kg 10/19/99 SEE SEE 2M. DyA, 5 .9 kg lo/19/99 'Ppb-CCV-11-1. SZE @C 1 TollH ., TOX14 MTwaxi.* XIZ 7axi@ R _iz Toll.@-R: : ToXI@@-RE-IC: T= ,:-R7-l@ To XI TIDLI.@ _aR-B :S"IOc_ 7=1 ? :..Bl -11, scl 8..1:",k:lllS.EE. 1 nk 1, s Blank-12. SEE 1. SEE Pb-ll. pb-11, s.1l.IEF b '',pPp-1i,i,-"rE.' --@@ppbb--ii. sEEE - ')pp b-11. SZE :__:j)oppb -11, SEE ppb-11. SEE ?"a Standard Sg tandard tandard tand&rd standard ss tandard taadard standard standard oc QC Qc oc oc Stand" Standard 3 t,@-@d Standard st standard ss tt...."dr-d d standard std c@ mr l.Ooo I i.* oo '1-.o.o, 1.0o0 1.coa I. i.oo 7.oso 7.094 7.093 7.063 7.079 7.111, 7.1 95 77.-a@.07 7.lGS 7.1o0s 7.1 6 7.106 I.OD 7.0l8o4 7. 5 7.1003 7.1 & 7.107 7.105 ao 1. I.oo 7.104 7.10a7 7.1 o I 7.1 o6 7.1 0 7.0 9 7.1015 7.1 7 7:*1.13 7 lo5 7 lo26 7 @..o. 7.o9e 7.lo6 7.103 7.097 7.0@:3 7. 7 l.oo i.oo 1.0o0o 1l,.oo '-.o0o 1*:oooo 1 oo I 7.105 7,OB5 7.1os 7.102 7.100 7 105 7@085 7.107 7.106 7.11a)1 7.0 3 '-l(o"68 77,,lloo6l 7, lo4 7. A@ nao. ID64 bb 1185 bb 11982 bb 122 bb 1311 bb 14691 bd : bb 11&2o'2 bb 2 7745 bb "163235 bb 1369 bb 1 bb 168Oo2 bt 163g3o bb 15 bb 1543 bb 1570 bb 1321 bb 1367 bb IS77 bb 1301 bb 1102 2 bb 14 2 bb 1547 bb 15:78 bb 14 bb 1433 bb 1329 bb 1570 bb ii:o m 11 5 bb 1142 bb 1172 bb 1251 bb 1502 bb 131: bb 121 bb 1188 bb 11:2 bb 14,5 bb 154 3 bb 15 1 bb 15 156)1o bb 15 9 5 bb 14 9 bb 1357 bb 16879 bb 1SIAS bb l@L 'lbb it bb C@. %D- o.7o -3o 0.7B9 -22 oo.? , -21 o.:7 -19 o 99 -13 -1 1I*1o2l 12 -1 o 93 I7 1 17 7 i.os 8 o.:ai -12 o. -9 1 11 11 l:G6 1 o: 1I o 2 l.o4 A 0.88 -12 o.90 -io 1o .*, 1 0 :.973' -27 o A -6 1.02 2 1 o5 -5 o:999 -1 o. 6 5 -,s o. a 2 i.ot 4 o:771 -22 0 7 :23 0 76 242 0.7@3 2 o.:9 17 o. -1 o@:7 o .92 o9 :13 i1s - o 79 -21 01:.982 -2 2 l.o2 2 @..o2 2 1.03 3 l.o6 6 o - -1 o:.:1o9 io 1 _o2 12 1 94 -1 o .94 6 o5 5 c, On ci) Da4o- no@ Uitd. LA(, IDId-llqq Smo 02GI99: Q*Antifie! a..! by i@ = lo/19/99 Q@tLty CalLkiWatiM _., "Y RI@ 4, ...t-- I- & d.-- @. Compound1name:POAA (Chi) Response Factor:42.2698 Response type:ExternalStd,Area Curve type:RF 10/19/!Ill 63.8x x x x x xx x ResponsL- x 1 0.2 -0'3 0.4 0.5 0.6 O@7 S@v 020199: at@tlfied and PrLnted by L" m 10/19199 Conc 0.8 0.9 1.0 Q@tity C&Ii@atim TO=45-"t 2"&, "Y x*@rt . .... Compound 2 name: PFOS (Ch2) Coefficienotf Determination:0.988440 Calibrationcurve:22.5689 *x + 138.989 Response type:ExternalStd,Area I Curve type:Linear,Origin:Exclude,Weighbng: 1/x,Axis trans:None 2.22e4- x Response- 0.0 g@V 020199: ou@itied and 200.0 by j- - loiltigg 400.0 600.0 800.0 Conc g@tity Calibw&tLm TOU415-rat s@&, "Y "Mr@ I & 41 "Ut@l d...& 10/19/09 9= Compound 3 name: PFOSA (Ch3) Coefficienotf Determination:0.998624 Calibrationcurve:200.271 -x + 81.0911 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:I/x,Axistrans:None 1.96e5- Respons 0.0- Skmp 020199: Q4@tifiod am4 t,rintod by l@ m 10/19/99 Conc au"tley Tc=,s-r" C&Iibratim sera, "Y I & 4, Compound 4 name: IS(Ch4) Response Factor:1510.76 Response type:Exter:iaSltd,Area Curve type:RF 10/19/99 MZE x 1.77e37 x x x x x Response- T-- I o@o 0.11 0.2 0.3 5-@v 020199: 0%@ntLfied @A PrLnted by L@ = 10/10/99 0 .4 0.5 0.6 0.7 0.8 0.9 Conc 1.0- L.as- -f@ed :@t 2@ 99 Compc;r %A (' zt 2@ 1 ;,o:SS 1999 a C-,. 1,,., 0,,@.c Co N RT*.@ @:1 I- 5 ,.@d.: User PF Value: U. a, PeAk F&CtOr: Integr@-@e Wlr:i!, Fllt-- Ch@-- e RT R@ pelk "@'dC@..Cn: OAA (Chl) N1... I c xed 1 0000000, oi.&bld -:Ooo 00 -.0000D. 133 S..bld :000: D@..bld e.r.st R p n PPooltlyntLc@:--aClrT.y-pin: t W Axi Un,t@ -In..0re s@, j- c R.t@ R.:.e Del@@ R,,.- 3@0000 .00 @s 0 bl*d 0 50. Dis&bld 00, Di:.bid -@Go. Di &bl ad 00, Disabid C.@.PC r.-' C, Cc.-U.@U.-f :,@SSL@. C-Ae@C)ct2': ?FOS (@ %.ed Oct 2 ",P- @ t"p,roXnathDB\101999b.mdb .36..49 199 ';'0:55 1999 -OS (CIL2) 9 - ooooooo, Di-bld -:o 0000 .000 RT T. P, 3@6 R.@bld '0: Dis&bled ..clel *&rest @'clude iL. -bld :co,oo co .0 bld 30 -OC, Di:.bbll d D@ d Dis&bld Di..bled Pg. 2 Zj Cc ftC@r 0' Cc- ir. Ch RT.- PC: S, i R, R, D@ S" R, AtRI. C@- 2 PF:SA .36:49 1999 :!0:56 1999 11,OSA, (ch3) :lc C Diabld -.00001@. .@1.0 :o 1 .1315* Znabl*d D"Abled :-ld. /X n.bld 3 C-00 00 -0,.00 0 @.bld -00 53, @oo .00:. DC Di:.bld D@ bld Di..bld Di ..bld 02-,i?7 pg. 3 4.i cc@ 2' -:36,48 1999 Cc, r. 1. :s (Cil.@ ,@d cct ::10:56 1999 f CC, e C.r U , UIsrs@ :s (CbA) i..d --.0O00o0oooo. Disbld 7*000 00 -.162. --bld .030, D@..bld Non243l R'@ .3 ear*st 4 7@ ------r-@t-77 @xc lude ilx sr Wi: . D: m S; R @rabled 0.00 30.00 0.00 Di:@bld Di b d i.&bl :.Oo: DDi.&bled QuattroII,#6414E SOUP 020199:FACT Equipment Log 99092 PAGE 1/1 DATELIQU9/-99 ANALYST-mmh STUDY NUMBER7 TOX145 MATRIX: ratseraDESCRIPTION:D-aYLI-4 FACT Method: ETS-8-5.1 Injectiovnolume:_IQ-uL- Cycletime:10 min.ElectWe:-Z-5pr-a-Y- Mobfle Phase: (A)2.0mM MHACH= TN-A- orstndrdnumber (A) 99085-10-14 Prepared(datelby): (A) 10/16/99mmh Expires: (A)04/00 (B)McOH (B)TN-A-2997 (B)JDLL6M_Lah (B) 2010 Storeatroom temp? E or N Other-. Guard column: None Part number: na Lot number: na Analyticalcolumn: Keystone Betasil Size:2 x 50 mm - Type: C 18 Part number: 055-701-2 Lot number: P9E II Sphere size:5 um Serialnumber:0591804Z AiWytical parameters: Drying gas (Llhr):350 ESI nebulizinggas (iJhr)_U LC Flow rate:300 uLJmin. Back pressure:65 bar Sheathgas(Llhr)0 BPLC solventgradient:10min-10-95 Time (niin.) 1)0.00 2)1.00 3)5.50 4)7.50 5)8.00 %B 10.0 10.0 95.0 95.0 10.0 Tuning method Method: Printed: Report C: \MkSSLYNX\SOtTP-RkTS. pRO\ACQUDB\PFOS3 Tue Oct 19 15:40:03 1999 lit: Page I ms SOURCE ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. 22 - NS2 Set 3.00 40 5 0.2 150 250 Rdbk 3.01 -41 -8 150 251 Pressures Analyser Vacuum Gas Cell Rdbk 5.5e-5 4.le-3 xsi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 3 650 Set 14.0 14.0 10 2.0 0.0 40 0 650 Rdbk 8 38 1 Method: L-t nditid: Pri.t.d: Fri Oct IS ll,.35:03 T" Oct 19 15:40929 sol-t D.Iy ( Lt- ) 1 0.00 r.wti" : 1 @ of I N"s Pair C up- ISpn_ter (ChDa.nnel Dlay I 3@S 0-03 0.00 Start Ti- it(-Ki-) : 0.00 Rnd T- mi- 10.00 t. 1 channel Parent Daughter D.Oll (3-cs) C-11 R@Orgy (OV) Cc" V 1 413.00 169.00 0-30 30 is @ti- :2 3ma Of I P.L@ ( gap- I.t.r , Channel D-1*Y sp- DaltO@ start Ti- ( Mine 2@d Ti- ( Mi- S-- 0-003 0. 0 0.00 10.00 Repoot@@el p@@t Daughter 1D.Oll (S-.) C.11 Z..m (OV) C@ v 1 499.00 99.00 0.30 45 60 runatim : 3 of I m@ palr I.ter Channel D81&Y S@x 0-003 sp- ( Daltostart Ti- ( 0. .01 Z@d Ti- MI "'- 01-.0.00 R.P..C. Channel V@@t Daughter Z)well (3--) C-11 R .. W (OV) C@ V 1 498.00 78.00 0.10 45 60 @im :4 wo of I nwa pair I ter Channel Delay 3;:: ( D.It.- ) : Start Tim Znd Tim ( Mi" )ti" Rep.at. Ch --- I Parent S@s Daughter O@03 0 00 0.00 20.00 D1"ll (S*Ca) coil inargy (tv) cone v 1 427.00 80-00 0.30 40 60 Masslynx-SampleList Sample ust:C:\MASSLYNX\soup@-rats-pro\SampleDB\0l1 999b.SPL: PrintedT:ue Oct 19 15:42:351999 1;1,14 Page 1 Page Poskion:(1,1) FileName FileText MS File 1 101999012 MEOH Blank MEOH Blank IOMIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 2 101999013 3 101999014 MEOH Blank IOMIN-PFOS-POAA-PFOSA-IS 4 101999015 TOX145-RBS10199-H20 Blank-11,SEE 1OMIN-PFOS-POAA-PFOSA-IS 5 101999016 TOX1 45-RBS1 01 99-Sera Blank-11,SEE 1OMIN-PFOS-POAA-PFOSA-IS 6 101999017 TOX1 45-RTS1 01 99-Sera Blank-11,SEE 1OMIN-PFOS-POAA-PFOSA-IS 7 101999018 TOX145-RTS10199-Sera Blank-12,SEE IOMIN-PFOS-POAA-PFOSA-IS 8 101999019 TOX1 45-RBS1 01 99-5ppb-I1,SEE 1OMIN-PFOS-POAA-PFOSA-IS 9 101999020 TOX1 45-RBS1 0199-1 Oppb-1 1,SEE 1OMIN-PFOS-POAA-PFOSA-IS 10 101999021 TOX145-RBS10199-25ppb-1 1.SEE 10MIN-PFOS-POAA-PFOSA-IS 11 101999022 TOX 145-RBS 10199-50ppb-1 1,SEE 1OMIN-PFOS-POAA-PFOSA-IS 12 101999023 TOX1 45-RBS1 0199-100ppb-1 1,SEE TOX145-RBS10199-250ppb-11, SEE IOMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 13 101999024 14 101999025 TOX145-RBS10199-500ppb-11, SEE 1OMIN-PFOS-POAA-PFOSA-IS 15 101999026 TOX145-RBS10199-750ppb-11, SEE 1OMIN-PFOS-POAA-PFOSA-IS 16 101999027 TOX1 45-RBS1 0199-1000ppb-1 1,SEE 1OMIN-PFOS-POAA-PFOSA-IS 17 101999028 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 18 101999029 TOX1 45-RTS, 9RO3230M, Dyl, Control,-Olll9/99SEE IOMIN-PFOS-POAA-PFOSA-IS 19 101999030 TOX145-RTS, 9RO3231 M, Dyl, Control,-10119/9S9EE 1OMIN-PFOS-POAA-PFOSA-IS 20 101999031 TOX145-RTS, 9RO3232M, Dyl, Contml,-10/19/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 21 101999032 TOX145-RTS, 9R03233M, Dyl, Control,-10/19/9S9EE IOMIN-PFOS-POAA-PFOSA-IS 22 101999033 TOX 145-RTS, 9RO3234M, Dyl, Control,-Olll9/99 SEE 1OMIN-PFOS-POAA-PFOSA-IS 23 101999034 TOX145-RBS10199-250ppb-CCV-1 1-1,SEE 1OMIN-PFOS-POAA-PFOSA-IS 24 101999035 MEOH Blank IOMIN-PFOS-POAA-PFOSA-IS 25 101999036 TOX145-RTS, 9RO3235M, Dy4, Control,-10/19/9S9EE 1OMIN-PFOS-POAA-PFOSA-IS 26 101999037 TOX145-RTS, 9RO3236M, Dy4, Control,-10119/9S9EE 1OMIN-PFOS-POAA-PFOSA-IS 27 101999038 TOX145-RTS, 9RO3237M, Dy4, Control,1-Oll9/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 28 101999039 TOX 145-RTS, 9R03238M, Dy4, Control,-Olll9/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 29 101999040 TOX145-RTS, 9RO3239M, Dy4, Control,-10/19/9S9EE 1OMIN-PFOS-POAA-PFOSA-IS 30 101999041 TOX1 45-RBS1 0199-250ppb-CCV-1 1-2,SEE 1OMIN-PFOS-POAA-PFOSA-IS 31 101999042 MEOH Blank 1OMIN-PFOS-POAA-PFOSA-IS 32 101999043 TOX1 45-RTS1 0199-250PDb-MS-1 1, 10/19/99SEE IOMIN-PFOS-POAA-PFOSA-IS 33 101999044 TOX145-ATS10199-250ppb-MSD-11, 10/19/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 34 101999045 TOX1 45-RTS, 9RO3245M, Dyl, 5 mg/kg 10/19/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 35 101999046 TOX145-RTS, 9RO3246M, Dyl, 5 mg/kg 10/19/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 36 101999047 TOX145-RTS, 9RO3247M, Dyl, 5 mg/kg 10/19/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 37 101999048 TOXI 45-RBSI 01 99-250ppb-CCV-1 1-3,SEE 1OMIN-PFOS-POAA-PFOSA-IS 38 101999049 MEOH Blank 1OMIN-PFOS-POAA-PFOSA-IS 39 101999050 TOX145-RTS, 9RO3248M, Dyl, 5 mg(Kg 10/19/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 40 101999051 TOX145-RTS, 9RO3249M, Dyl, 5 mglkg 10/19/99SEE 10MIN-PFOS-POAA-PFOSA-IS 41 101999052 TOX145-RTS, 9RO3250M, Dy4,5 mg/kg 10/19/99SEE IOMIN-PFOS-POAA-PFOSA-IS 42 101999053 TOX145-RTS, 9R03251M, Dy4,5 mg*g 10/19/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 43 101999054 TOX145-RTS, 9803252M, Dy4,5 mg&g 10/19/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 44 101999055 TOXI 45-ABS1 0199-250ppb-CCV-1 1-4,SEE 1OMIN-PFOS-POAA-PFOSA-IS 45 101999056 MEOH Blank 1OMIN-PFOS-POAA-PFOSA-IS 46 101999057 TOX1 45-RTS, 9RO3254-1 M, Dy4, 5 m%fkg 10119/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 47 101999058 TOX145-RTS, 9RO3254-2M, Dy4,5 mgng 10/19/99SEE 1OMIN-PFOS-POAA-PFOSA-IS 48 101999059 TOX1 45-RBS1 01 99-250ppb-CCV-1 1-1,SEE 1OMIN-PFOS-POAA-PFOSA-IS 49 101999060 MEOH Blank 1OMIN-PFOS-POAA-PFOSA-IS 50 101999061 TOX145-RBS10199-H20 Blank-11,SEE 1OMIN-PFOS-POAA-PFOSA-IS 51 101999062 TOX1 45-RBS1 01 99-Sera Blank-11,SEE 1OMIN-PFOS-POAA-PFOSA-IS 52 101999063 TOX145-RTS10199-Sera Blank-11,SEE 1OMIN-PFOS-POAA-PFOSA-IS 53 101999064 TOX1 45-RTS1 01 99-Sera Blank-I2,SEE 1OMIN-PFOS-POAA-PFOSA-IS 54 101999065 TOXI 45-RBSI 0199-5ppb-11,SEE 1OMIN-PFOS-POAA-PFOSA-IS 55 101999066 TOXI 45-ABS1 0199-1Oppb-1 1,SEE 10MIN-PFOS-POAA-PFOSA-IS 56 101999067 TOXI 45-RBS1 0199-25ppb-1 1,SEE IOMIN-PFOS-POAA-PFOSA-IS 57 101999068 TOX1 45-RBS1 0199-50ppb-1 1,SEE 1OMIN-PFOS-POAA-PFOSA-IS 58 101999069 TOX1 45-RBS1 0199-1 ooppb-1 1.SEE IOMIN-PFOS-POAA-PFOSA-IS 59 101999070 TOX145-RBS10199-250ppb-11, SEE 1OMIN-PFOS-POAA-PFOSA-IS Masslynx - Sample List Sample ListC::WASSLYNX\soup-rats-pro\SampleDB\l 01999b.SPL Pdnted:Tue Oct 19 15:42:351999 InletFile Bottle InjectVolume Sample Type 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 91 4 10min-IG-95 1 5 10min-10-95 2 6 10min-IG-95 3 7 10min-lG-95 4 8 10min-10-96 5 9 1Omin-1 G-95 6 10 10min-10-95 7 11 10min-IG-95 8 12 10min-10-95 9 13 10min-IG-95 10 14 10min-lG-95 11 15 1Omin-1 G-95 12 16 10min-10-95 13 17 10min-10-95 92 18 10min-lG-95 14 19 1Omin-1 G-95 15 20 10min-10-95 16 21 10min-IG-95 17 22 10min-10-95 18 23 10min-IG-95 41 24 10min-lG-95 92 25 10min-lG-95 19 26 10min-lG-95 20 27 1Omin-1 G-95 21 28 10min-lG-95 22 29 10min-lG-95 23 30 10min-IG-95 42 31 10min-lG-95 92 32 10min-lG-95 24 33 1Omin-1 G-95 25 34 10min-10-95 26 35 10min-lG-95 27 36 10min-IG-95 28 37 10min-lG-95 43 38 10min-lG-95 93 39 10min-10-95 29 40 10min-IG-95 30 41 10min-lG-95 31 42 10min-lG-95 32 43 10min-IG-95 33 " 10min-IG-95 44 45 10min-IG-95 93 46 10min-lG-95 34 47 10min-lG-95 35 48 10min-lG-95 41 49 10min-IG-95 93 50 10min-lG-95 1 51 10min-10-95 2 52 10min-10-95 3 53 10min-IG-95 4 54 10min-10-95 5 55 10min-lG-95 6 66 10min-lG-95 7 57 10min-10-95 8 58 10min-10-95 9 59 10min-10-95 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 Conc A Page 2 Page Position(:2,1) Masslynx - Sample Ust Sample Ust:C:\MASSLYNX\soup-rats.pro\SampleDB\l01999b.SPC Printed:Tue Oct 19 15:42:351999 FlioNaffm FileTe)rt 60 101999071 TOX145-RBS10199-500ppb-11, SEE 61 101999072 TOX145-RBS10199-750ppb-11, SEE 62 101999073 TOX145-RBS10199-1000ppb-11, SEE Page 3 Page Posibon:(1,2) MS File IOMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS Masslynx - Sample List Sample ListC::\MASSLYNX\Soup-rats-pro\SampleDB\l01 gggb.SPU PrintedT:ue Oct 19 15:42:351999 InletFile Bottle InjectVolume Sample Type Conc A 60 10min-10-95 11 61 10min-10-95 12 62 10min-lD-95 13 10 10 10 - Page 4 Page Position(:2,2) FACT: DA-RA REVIEW SUMMARY FORi-vl Date: Data Analyst FACT Study N: matrixrrimepoints: eJ Sample List- Set-upAnalysis DatdAnalyst Instrument An-glio,iffr (D A,nalyft: TDA-A ee.41) Acceptable Linear Rxngc: A(A LOQ. A(A R^2: /M- Ext=tionBW& Matrix BWnic A(A CalibratioCnheck-i. #A NLS/NM: N)04 ID&t& Status: i).@ P",@kn4 Data Review Sign-Off Analyst Re-view Name/ Date: Tecbnical Review Name/ris @oks- Qu&HtyA-- Nam /Date: Review Data Entrr. P4 el Commnts /Justifkations: 4, Pe, k. .)Ll,ot [Ac yyAM4147A Analyte: A=cptabic LinearRange: LOQ: R^'2: CalibratioCnhockL MS/NM: Data S tgz t3 ExtractedBWk /e,,- Matrix BlanL- Analyte: ?rO64 eCg4)a' Acceptable Lincar Range: Y;!. LOQ: 0. R^2: - ExtractedBlank: /Itl@c zoo Matrix Blank. Calibmtion'checks: 1.;14@ MS/MSD: idataSatus: uzk @. . rfaArl)@tL lb LAC, ll)],2g)gl L4@) p,@C- .101.2 -IR @p 6^x .44( lk.,4 le@dlerxl 74-,- 4, ;B2 71yo",z '12?."/ /, 1/2,!nt4 r&,L4"e a..l @4 0, lye 17 or r@12 / -ke-y3 I j A@ia,tkL C-LV-I C44Mt4-CA LA;@k kr\UL SCfelti CIAI@l@tL ?1)). b,.Lk,4,*tCwt 40 ven Cone. @ LAC Date: Data Analyst: FACT Study M: Mathx(Timc*nu: Sample Li%LSet-upAnalysis DatdArWyst Instrument Anslyte: !r" -ro)ele A.I,, FACT: DATA REVIEW SUMNLARY FORNI DatitReview Sign-Off Ansirt Review Narne /Date: i,P;z LAC, o@z,@fr Technical Review Narne /Date: P-t@L- 1 Qu&Hty Assurance Review Nwne /Date: Data Entrr. lot@e,"A, yvri 4,@r-tA"ck)U6,@, Comnwnu IJustifications: ty", A AcceptiLbiLcinew RAnge: LOQ. _ .1@/4 - R^2: IVA CalibrationCheckL- AIA ExtractionBbmic N* Matrix BWilc 4A 7a pz@@i iko,z4 mstulmr Data St&Ms: Aniilyft: AcceptableLinearRange: LOQ: R^2: CalibratioCnhecks: MS/NM: -DatiSLtatus: Analyte: AcceptableLinearRan LOQ: R@C^22: at&Sams7 UibimbtrCia@h e.cCkhse-.cks: ExtractedBknk. Matrix13@Z- ExtractedBlank. Matrix Bl&nL- "I. f-lzl;/f coi& ('Xrte-5 :el 1,,ek-e;t../ e,<,,4S 'TLulekl reva@,tot;-e& 7Z@ A" L.I.-e ves J@ at&Satus: -:rA11 Sam \MXMTMX thd: b"w'nOct 25 Las.tt M.0.4ul:,Imd: J@b C." i '999 mmlia-mts.M\bftthDB\102299& \06:39:55 1999 IpIrLnted: mn Oct 25 06:59:42 1999 CwW@o.d 1: POAA e N@ 1022 '2 @02291:0.0.2 3 1022:90903 1 102 '90004, 2 6 102 2221999.'-016 9 102299008 9 102299009 io 102299010 112 102299011 1 102299012 13 102299013 2 14 "11 l@1o1'22::00 16 102299:0 16 22 119, 1022 2::O.@19* 2 1@o02 1'1g0.2:0,l 210 22 22 102299022 23 102299023 2 1022::024 2 56 11022 025 2 02299026 21 110229999021 28 022 028 29 11 022:9029 0 30 022 903 31 102299031 32 102299032 33 102299033 34 102299034 35 102299035 36 102299036 3 102299037 399 102 299030 3 1022: 04309 4. 022 : 41 102299041 [Cbl) =Ielist Blank .Ol, T"t Typ- Std cmc ItT :.ggo " TCX11441a!5;_LR@"0lk1o5l9g-gf_fS2.orm alk-12, SEE :lk 12: SEE Ik:12 SEE SEE Is "4,5:R BSol TOX' TOX: -_12 =12: 2 TCX TOX TOXI,., 11:99:2,5.=:12: 12 TOX TOK 1 45-"SIO199-'I$oppb-12, 'IOX1I4S-RR510199-100oppb-12, U XE SESE EE S EE s zz U SEE T1*101"41!a'InTIk-9103245M. @:5,:R.TTS,::00,322.4".: = 14 2;,:.IK: ;:I.4-S-.'IT'SS::1'.o033 5-P.BSIOI,9-250ppb D&YI, 509/kq",: I.@-o1:0:.tl@tol,*@l9,l9",99 -.,Y@'.: ='Ik,. Dl:yy1l: ,kq. D50-extio/19/99 D5,00::4 ttIO/19/99 10/19/99 CM-CCV-11-1, SEE 3't6.drd t rA&.d standard ssttandard ..r&. d stand d S3 tandard t.nda@d t=drd oc 1-00 1 .0 1:00 i.oo I 00 1i.0o0. 1..0I0o 1.00 '5 ;:0.02_0, 7.010 6.998 :.989 6 6-.9.9066 6.991 914 .::194 6.965 5 6.99 -7.01: mTea,l'l" 4 Blill"Tkl-9R03250M, DDSyY44: 9 =/k:/,k - DDSSOD::Xtlo/19/9 xtlo/19/99 TOX145-RTS-9@1103251M. Y" kq, DSO oxtIoll:/:2 TOX145-RTS ::lt03254-134, l@.y4, -Ikg: D;@o,0: 1@o0,1@19,9', 9 TOXI T 14"5--R1T,ST@1-9..3@54-2N. cy4 Sq/kg ii-2, SEE ToOxX .45-RBS10199-250ppb-CCV- M.OH glank TOX TOX, TOX145-RTS10199-SO@ ik-12. SEE .1@,-@2, S. BIX-12, SEE TOX115:=101 12 'EL TO=X114455-@5RRSIO19@o90@-,:295,p_p_5b@-=122, TOX14 TOX14 1 SIEFEE 2,SZE SEE TOX145-PlI.S.I@O.1@:9 9-_2,5O=b @=14-@'4@!-,RB_."@ b--'@22,' 00 199-750ppb-12, SS EZEE SEE TCX145-"Sl 1 99-IOOOPPb-12, SEE oc sttandard rd standard Standard s tandard stadard S5 tndard tandard standard 1.000 6.912 6.992 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.0 1.000 6.909 '67 :4 :99 3 6. 9 6.990 6.99 1.001 1.022 7 016 6:998 :.::70 AX" C@c. rla4m U)s@ 120 los 115 "@201 119 5 11 14i2l 76 ISO 24 34 3 2 2 96 7 20 25 26 22 52 11 117 119 1094 13 5 1178 10 73 130 160 19453 1.04 bd 0.94 bb 0.99 "H 0.95 bb 1 bb :0" 00.6:54 dbb bb 1.02 bb 1.22 bb 01..6367 b b bb 0.21 bb 00 .29 bb .31 bb 25 bb 00..23 bb 0.66 bb 0.11 db 0.21 bb 0.23 bb 0.19 bb 0.45 0.10 1.01 1:13 bb bb bb bbb 00.911 bb 1.19 bd 1.01 bb o.90 bd 0.63 cLb 1 19 bb 1:382 bb bb ol .824 bb 4 -6 :I 5 -11 -165 -3 2 2Z -34 31 -79 :11 69 --15 -71 -34 -93 -79 -71 -81 -55 -90 1 1 -99 19 _11 0 -37 19 39 1 24 A@lia 092490: Q@ti@tgd mid P@t-ted by 1&& 10/25/99 0Ta'x dil@"--, dy I & a- 3&-Pll List: L..t *,Ufid: ".tr-d@:difld: Job Code: C11:0\1'"OSCtLy2S=\Od@:4131:-&Srg1a9t9s9 c:\x%SELTMX\.-Iia-"".Pm @ ect 2S 06:39:55 1999 Print*d: mn Oct 25 06:59:42 1999 @Mth"\102299& C,a,poUr,d2: pvos 1 102299001 2 102299002 3 102299003 4 102299004 5 102299005 6 102299006 1 102299001 0 102299000 9 102299009 10 102299010 11 102299011 12 102299012 13 102299013 14 102299014 is 102299015 16 102299016 17 102299011 18 102299019 19 102299019 20 102299020 21 102299021 22 102299022 23 102299023 2 102299024 25 102299025 26 102299026 27 102299027 28 102299026 29 102299029 30 102299030 31 102299031 32 102299032 33 102299033 34 102299034 35 102299035 36 102299036 37 102299031 38 102299036 39 102299039 4o 102299040 41 102299041 (ch2) TYP- Std c@c SMa.mOqHpldbailtank Txt NSCH blank 12, SEE TOX145-RB510199-R2o alk- TOY,145-PBS10199--$*@ bik-12, SEE Sik-12, SEE TOX14455-_RRTBS31,00119999-SO_@ TCX !,ppb-12, SEE TOX1I45-"SlOI99-loppb-12, SEE TOX'145-RBS10199-25PPb-12' SEEEE TOX-145-pjBSlolgg-$Oppb-12, TOX 45-RRSIO199-100ppb-12, SEE TOX1I4455-_RPB.SRISO,IO9l9g-g2_5S0opoppbp-b1-21,2, SEE SEE TOX1 TOX14S-RWIOI99-75oppb -12, SEE Standard standard Standard Standard standard Standard standard standard Standard TOX145-PJLS10199-100OPPb-12. SU M.On blank TOX145-RTS-SR03245M. TOX14!,-RTS-9ltO3244M. TOX145-RTS-gRO3247M, 45-RTS-gR03242M. TOXX1145-RTs-gRO3249M. TToCX14S-RDSIO199-250ppb- ,I. 5"/kq, DA D&I D&lf D&yl, 5mg/kg, 050-..tlo/19/99 DSO-extIO/19/99 050-*Xtlo/19/99 D50-Oxtio/19/99 YI, sg/kg, 050-ext1o/19/99 D& CCV-11-1, STE N.OH Blank TOXI RTs-9RO3250M. 1 ,4, 5.9/kq, D50-OXtio/19199 Day4, 5.9/leg, D50-OxtIO/19/99 TCL(1'455-..,,-IR03251M. 5.9/kg, DSO-&Xtlo/19/99 TOX145-RTS-9RO325ZK. DI y4, D50- 10/19/99 TC)X145@RTS-9RO32S4-IN, D-lf4, 5.9/kg, 050- 10/ 19/99 TOX145-RrS-SR03254-2M, Dy4. 11-2, SEE TOX145-RBS10199-2$OPPb-CCV- M.OH Blank TCX145-RgSlo,99-H20 Blk-I 2. SEE TOX145-RBS10199-S'rM T,DX145-RTS10199-S-r@ elk-12, SEE elk-12. SEE TOX145-."510199-bppb-12, SEE TOX145-RU10199-1 Oppb-12, TOX145-RRS10199-25PPb -12. TOOXX114455_-"Slolgg@-Soppb-12. pMlolgg-100ppb-12, SEE SEE SEE STE SEE 'r I-OX145-RILS10199-SOOPPb-12, SZE 'Tf=14S-RDS10199-75oppb-12, SEE TOX145-RBS10199-100OPpb-12, SEE oc oc standard standard SSttadn&dradrd standard st@dar Stand&ri1 St=d@r stndardd 4.93 9.76 24 80 49 '30 97.-60 248.00 493.00 735.00 00 916. 248.00 248.00 4.93 9.76 2.49- .300 97.600 240.00 493-00 735.00 976.00 1.190 1.163 '7.186 7.170 7.162 7.171 7.176 7-194 1 113 1.'164 7.166 7-169 7-169 7.179 7.172 7.169 7.173 7.143 7.160 7.161 7-166 7.165 7.160 7.172 7.166 7.164 7.169 7:1?0 7 171 7.165 7.172 7.163 1.169 7.173 7 194 1*169 1.173 7-109 7-171 7.169 7.175 A119 62 112 so 263 330 520 1195 !,512 11226 22030 2a62l9 3 9123 09 4125 6459 5637 3710 4380 169 40 4350 4238 6453 !5257 4193 217 23 75 96 262 336 521 1235 2005 5514 11233 21169 29094 37681 C. riago 0.24 NK 0.00 m 0.08 NK 0.00 mm 3.44 bb 4.94 bb 9.34 bb 24.22 bb 40.12 t)d 120.40 bb 247.73 bb 490.41 bb 6245.31 bbX lia.00 bbX 0.01 w 49.49 bb 141.49 bb 123.10 bb 80.23 bb 95.16 bb 1.33 bb 0.00 mm 94.50 bb 92.01 bb 141.35 bb 114.70 bb gl.oi bb 2.42 bb 0.00 mm 0 00 mm o:oo w 3.43 bb 5.07 bb 9.20 bb 25.11 bb 420.26 bb .43 bb 12247.86 bb 469-6 bb 645.018 bbX 937.11 bbX u)-@ 0 -4 --2 19 23 :0 I -15 -16 -99 -99 3 -6 I -14 23 -0 -5 -12 -14 P.q. 2 Q@@ttatsd A@iia 062496: @.d fti,@ted by i@ 10/23/99 O...-ry c-.-TOX145-,.t ..@ "Y I t.4- $;.Vl. List: Last mocufled: .Lh@d* = at @dfld: Job Co" : p@t.t.d: N@ oc:t 25 06:43:SG 1999 cMaln Oct 25 0 1999 "On act 25 06:SR:42 1099 20/19/99 NZI \NathDB\lC2299& Cowpou@d 3: pro$^ lrh4) o NJ 102299001 2 102299002 3 102299003 4 102299004 5 102299005 6 102299006 7 102299001 8 102299000 9 102299009 10 102299010 11 102299011 12 102299012 13 102299013 14 102299014 15 102299015 16 102299016 11 102299017 le 102299010 19 102299019 20 102299020 21 102299021 22 102299022 23 102299023 24 102299024 25 102299025 26 102299026 21 102299021 29 102299028 29 102299029 30 102299030 31 102'99031 32 102299,)32 33 102299033 34 102299034 35 102299035 36 102299036 37 102299037 38 102299038 39 102299039 44 0 102299040 1 102299041 S-WIa-t T"t H.OH Blank M.OH blank Type TOX145-RsslOI99-R2o Bllt-12, SEE 145_RBS,Olgg-Sgrm Blit-12, SEE TOX TOX11445-RTS10199-5*rm Slk-12, SEE TOX S-P.RSI0199-5ppb-12, SEE TOX145-RBSIOI!19-10PPb-121 SEE TOX145-pzslol99-25ppb-12. S3EE T @145-RBS10199-SOPPb -12, ZE O'U45-p.BSIOI99-looppb-12, 39E TTOO,)@145-RBS10199-25opp-12, SEE 145-ItBSIOlgg-500ppb-12, SEE 'TYOCX"C145-MS10199-ISOPPb-12, SEE TOX145-RBS10199-100oppb-12. SEE Standard Standard StrA^rd st.n"d"arrdd Standard Stad& rd Standard standard M.OK Blank lmyi. 5.9/kg, DSO-extio/19/99 TOX145-RTS-SR03245K, TOX145-RTS-9RO3244M. DOYI, 5@g/kg, DSO- xtlo/19/99 C.Yl, -%Oq/kq, D50-:Xtlo/19/99 TOX145 -RTS-9R03247M, Toxi45-RTS-9RO324$m, DaYl, -@.q/glg, DSO-*Xtlo/lt/99 5ag/kg, DSO---tlO/li0/99 TaK145-RTS-SK03249M, D-YI, oc TOX145-"310199-250ppb-CCV-11-1, SZE K.CH Blank TOX145-RTS-9RO3250M. TOX145-RTS-9RO3251M, TOX145-RTS-9RO325ZK, TOX145-R?S-9903254-IN, I)ay4, ssq/kg, D!10-*Xtlo/19/99 Day4, 5"/kq, 050-sx tio/19/99 I)ay4. Sq/kg, DSO-Oxtlo/ 19/99 Day4 5.9/kg, DSO- io/19/99 TOX145-RTS-9RO3254-2M, Day4,' 5"/kq, DSO- 10/19/99 oc TO)CL45-"Slolgg-250ppb-CCV-11 -2. SU H.OH Blank TOX145-Raslol99-H20 Blk-12, SEE TOX145-"$'-0199-S-@= RB ik:112: SEE TOX145-RTS',0199-S.rus 2 SEE TOXl45-RaSlol99-5ppb-_Ji1.2IkSE@E TOX145-"SIO199-10PPb- EE TOX145-"SIO199-25PPb 12, SEE TGX145-pLaslolgS-50ppb-12, SEE TOX11445-p.BSIOI99-looppb-12, SU TOX S-RBSIO199-250ppb-12, SEE TOX145-RES10199-SOOPPb-12, SEE 145-RELSlolgg-75oppb-12, SEE TCOKXX145-RaSIO199-1000rppb-12, SEE standard standard Stndard standard Sta@ndd&arrd d standard Standard standard std C@ 4.93 9.77 24.80 49.30 97.70 248.00 493.00 736.00 977.00 24 g.00 246.00 4 93 9:77 24 00 49'.30 97.70 248.00 493 00 736.00 977.00 ICT 7.-946 7.840 7.043 7.850 7.843 7.126 7.834 7.640 7.020 7.821 7.020 7.826 7.826 7.435 7.653 7.825 7.029 7.825 7.925 '?.$42 7.824 7.868 7.040 7.633 7.649 7.845 7.850 7-:2 7. 52a 7.846 7.853 7.643 7 926 7:82-1 7.051 7.828 7.e30 7.B46 7.628 7.827 7.832 Ar@ 465 331 152 isi 95 $is 1344 3615 3624 IB036 39992 $6286 126147 170949 424 1404 2212 1129 1612 1370 2187 3 330 316 398 422 331 283 25 61 47 56 730 1319 3425 14:9 c- riq. 4.23 bb 3.42 bd 2.33 MM 2.33 MM 1,99 MM 6.36 bb 9.57 bb 23.35 bb 35.54 bb 110.$S bb 244.14 bb 537.25 bdX 767.03 bbX 1039.19 bbX 3.99 bb 9.94 bb 14.63 bb 8.69 bb bb 119-.1792 bb 2.73 b 1.63 bb 3.42 MM 3.33 bb 3.82 bb 3.97 NK 3.46 bb 3.13 bb 1.56 bb 1.72 Mm 1 .70 mm 1.75 M 5.94 bb 9.41 bb 22.20 bb 14,.60 bb @'.1 ' 88564 125699 16OB96 25'0..6500 bbbb $3o.93 bbX 764.31 bbX 1026.49 bbX %D- 29 -2 -6 -28 13 -2 9 A 6 -99 -99 19 -4 -10 -30 19 1 91 5 ftg. 3 092499: Q@titatod wA ftinted by in. 10/25/99 R-p-t *,*-,d 9'-'Y ILa a- -t. 20/19/99 sxz TOXI45-..t -- "Y I mplo List: C:VPJSLTM\a-li.--".FW\S.Mi.02\102299. .dfled; man Oct 25 06:43:36 1999 thDS\102299& C; \K%.ULYNX\@lia-MLG -M\No H.th.d: L..@ -dLf@@: )on 0-t 23 06:39:55 1999 i.b cd.: printed: 25 06:59:42 1999 C--P-und 4: 13 o N1 102299001 2 102299002 3 1022,9003 4 102299004 5 102299005 6 11 02299:006 7 1 022 99 007 a9 1 022 99 00: 10 1 022 99 00 0 11 1 022 99 0111 022 0 12 102299012 02299013 @4 @02299014 15 102299015 16 102299016 17 102299011 is 10229901B ICh3) SOWIOlist T"t H.OH :i@k MT-oOxHl44S-Lp@2kSlol99-K2o alk-12. SEE TOX S_RBSIOI99-$Or@ alk-12, SEE TOX 1 45-RTS10199-SO@ alk-12, SEE 145-RWID199-5ppb-12, SEE TTOOXXI145-RRS10199-JOrppb-12 SsEE TOX1145 0 1::-25ppb - 12, LE TOX 4 pasi I -50ppb -12 T.rOX145-RRS10199-100ppb:12. 2, SESE EE T.rQOXXII:SS:PPLBBS150110191-:2-550o0ppppbb-1I2 SEE OX145-PS31019 ,::7500ppb-12 : .EE TOX 4s- FLBS 01 10 Oppb -12, SEE M.O. al..k T.XI45-RTS-9ltO3245M. IMYL, . "" TOX1145-RT -9RO3246k, D&YI, Sd TC)X 45-RTSS-9RO3247M, D&YI. 50 TYP- standard Standard Standard st..drd dard Standard standard Standard Standard DS,O O::xtlO0,"1",,199 99 std c@. 1.00 1.00 i.oo 1:00 1 .00 10 1.00 1.00 1.00 RT 7.001 6. 84 7.002 6.958 7.014 67.9097 -009 6.'9603 J.::5 165.993 4 6:29882 2 19 102299019 20 102299020 21 11 022::021 22 022 022 234 11 022:99023 2 5 1 022 024 2 102299 9025 6 1 022.)9026 227 022 9021 28 102299028 TOX145 ItT -9R03240M, DaYl. SM TCX145:RTS S-IR03249M. D-YI, -@"/kg, DSO-oxtIO/19/ TC)X145- 10119-250ppb-CCV-11-1, SEE ()C 14.M Blank TOX145 RTS::,Rt*o325 Da:y4 l"a"q,l4k:4 DS,O.::Xttio/19/99 RTS TOX145- 32SIX, Da 4: 10/19/99 145 RTS-9R0325 Dy4 5.q/kg, 050D-5s0x-tl1O/19/ TTOQXX145-RTS-gRG3254-I2KM. D- 4 @.9/kg, /19/:99 11 45:RTS -IR03254 -2H, D. ;Y4 S.,/kg, DSO- 0 /1 /99 TMOOXX 45 RBS10199-25oppb-CCV-11-2, SEE oc 1.00 1.00 6.97 6.9836 6 -9,:2 7 6:1.103 7 .903 :.903 5 29 102299029 30 102299030 31 102299031 32 102299032 33 102299033 34 102299034 35 102299035 36 102299036 37 102299037 38 102299039 39 102299039 40 102299040 41 102299041 lank TeOoX'Il45O-RESIO199-H2O Bik-12, SEE 7 14 1 19:-.S:r@ :lk-12: SEE T OX 1455-"RSTS110019 Ik-12 SEE T OX s 0199-Sppb-12, SEE TCX145-Rj& 10ppb- 12, SSEEEE TOOXX 14!o-RREDSSI1O0191999--25ppb-12 : TOX145-RBS10199 SOPPB 12 ZE oppb-12, SEE TTODXX114455:RBRSB1S01109019999-91:0250ppb -12: SEE TOXI:5 VLBSIOJ199 5050ppb -12, 5 EE TOX145 RDS Iolgg_ 70oppb -12 TOX 5_P.B$l I OOPPb-12, ESElE standard Standard Standard S'ttandard t@ rd St ..daid St&nd&fd Stand& rd rd '-Do lI'.o00 1.00 1.00 1 00 1:00 i.oo I1.-9g:ll 7 09 01 1 .,:3 7.00: 7.007 012 7.004 7.0 9 7.000 6.991 A- Conc. TI&OM %D@ 30361 259 2051 2705 2840,5 2 1514 2 2:052 29 3031 3075 2977 :9 73 76 66 2290 854 go9 66 70 le$9 2112.9 23 2521 2515 23081 23 21992 2055 2958 2996 2:13 2 53 1 13 bd 0:96 bb 1.06 bb 1.00 bb 1.04 bb 0.:3 b 0. 0 bbb 11 .06 bb .04 bb dd 1-:1@14I bd mm 0.03 MM 0 03 MM 0.03 bd 0 03 bd 0 03 bb 0 65 bb 0.03 bb 0.02 bd 0.03 mm 0.02 bd 0.03 bd 0.70 bb 1.0.46 bd 0.94 bb 0. 93 bb 00:-0996 bMd 0 .91 bd 1.(@, bd 1 bb bd 1,084 bd 1 b 1:0,6 bb 13 -4 0 4 -7 -20 6 14 13 4 I -97 -97 -91 ::7 _I I 5 -91 -9.87 -981 -9 -30 _I4 -4 -6 -1 7 _114 -19 6 0 14 6 rag. 4 A@l,& 06349@: g@tit&ted nd ftinted by jas 10/23/99 Q@LLry Cal lbrat,@ Report T=45-"t "@ d"uti@s, d-Y "t. 10/19/99 S" IResponseFactor.115.946 lresponsetype:Extemal Std,Area ,Curvetype:R-F 160 x Response- __Ioto-@-0 1-@--O@2 0-3@0--4@0-1@ _,d ftint" by jas 0'6 06@, @0. 8 @101 .9@ Conc 10 Qu-tity Toxi4s-rat cLilu=@, d.Y I & 10/19/99 On ii efficienotfDetermination0:.995295 !Calibraticounrve:44.8833 * x + 108.462 Response type:ExternalStd,Area g: I/X,Axis transN:one curve type:Linear,otigin:Exclude,Weightin 4.39e4 ftg. 2 Respons x 0 Q"n__tod j,-Ii. 062496: .d ftinted by J" 10/23/99 Conc 00.0 C,@tity Calik@ati@ R6Po@@ "Y 4_ .,@ to/it/99 mz A :Coe cientofDetemination:0.9 9156 icalibratiocnurve:164-764* x + -232-515 .Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting: I/x,Axis trans:None 1.7le5- ftgr.3 Response -233 0.0 A..li. 062406: Q@tittd iob.0 @d ftiutmd by ias 10/2S/99 400.0 Conc 800.0 QtmntLfy "Libra"@ P@Po@t day TOX145-tat "@ dilo"@ 4- "t. 10/19/99 szlg e: e nseFactor:2692.44 es onse type:Extemal Std,Area ;cu e type:RF 3.07e3 ftg. 4 Respons Conc 00.1 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Amlia 062498; g@tit&t" amd ftintd by 10/23/99 ,.:thodfile: ,t modified: c:\V.ASSLYNX\@elia-r.t$.PRO\NethDB\102299&.Ndb ,on Oct 25 06:39:55 1999C; compound: 1: POAA (Chi) mo@ Oct 25 07:03:23 1999 tA. Printed: Coupo nd N"O: ouantify Tr&Ct; Conc. of Standards: user R,:Ov& luc*: User k F& tor: integrate Window rmct.r@ Chro@toqram mas window: Peak Location Retention Time T, ,@T"1t1a fr.a.nc..a.* ..t"' Time Window peak Saltction: Response R*:- ,::Typo: Re Pon C.1 Lb_rt@_ n CU--- Poiyn@to -oIf&IOrTtyp Fit W*iqhtinqg:i. Axis Transto@tLOn: Concentration poAA tchl) two. TIC Fix*d I:0D0o0oo0o00o, Di.&bld I 2.000 l'OOOODA 6.994, En.bl o.000, Di@.bi-dd 10142031 N*ar.st Lter@l AZO&S Linear Lc lude 1/X No.. Peak-to-peak awlitude: smooth $-*thinq: Wind- ,i.. (SC".): N@.b*r f @, t a: Swoth@ng method; 8&..Il... j I cvall:ythreshold: R:d' . Aq; @,.u@3,. .p...II,tn:"' peak Separation Draw vertical threshold: D* "10'ld*": ,: S Th"rreshol1d Rel3a0tivt: h:ight: Ab IU h ight! Relative r. : Absolute are&: 95 D12abl*d 30.00 200.00 5.00 9,...0"bl.d 30 0 1.50: 0.00 2.00 o.oo Disabled Di:.bld Di -blsd Di &blod Method Report Method file: Last modified: Compound: Printed: C:\PASSLYMX\@li&-rats.Plto\KthDS\lO22 Man Oct 2$ 06:39:55 1999C 2: PMS [Ch2) Man Oct 25 07:03:23 1999 Compound Qu&ntify Conc. Of M".: A.f.: Tract: Standards: user RF Value: *r Peak factor: UI. t.grate Window Chnro"togr@ mass Peak Location r&ctor: window: RT1.*RefVri c.: I @do- peak Selection: PMS (Cb2) mon-) TIC conc. A I.Oooooo, 1.000000 2-000 1.O.OOD& Disabled ad '..'007'0: rD,i&s@bbll d IN*n62l 0.2 Nearest @.*.-S@pno".s. Type: Response: Clibrti.11 Cl-*' Polynomial Type: Point of Ori Fit 3 WeTighting:qin Axi r ansfor"tim: Concentration u Its; W.@.. Peak-to-p*ak smooth Amplitude: Swathing: min=d .i.. t.c@): Swathing f m.e-th:od: B.s.lin.@ Join valley threshold: PR L:duca. p Ak t&LIIA9: I ba:eiin* mxla@: peak- Separat Dratwectvertical threshold: Do shoulder3t Sh*.,.,.I.d.*r.. tThr:.h'o0l'd.: Rol&tiv: Absolut R.lati 4 Abso lure h ight: h:iqht: &rO&; arsai LArxeta.smal Lin. r gxcludo I/x %on. 2300 abld Di 2 1 30.00 2500.00 .00 9D@0.-.'b*l.d 30.00 I so: 0.*00 2.00, 0.00, 11 o.bl*d Dit bled Di ..bled Disabled page 2 Method Report method file: "xt modified: Compound: Printed: C:\XMSLymx\@lle ,;rIat..plto%Methvs\lO2299-.-db M.. oct 25 06,.39: 9990 3: PFOSA (Ch41 mo@ Oct 25 01:03'23 1999 Cox a nd N"-: I.tp.r@nal R*f.: Quantity Trace: Conc. Of Standards@ Us:r R:,V lu : U. r P k'faector: l@tograt Window ractor: Ch r@ togr@ mass window: Peak Lzc&tlon ion Time: P'Tr ndo, taln2): Peak Sel*ction: Response R.:P.ns. TYP-: Re Pon Calibr:*tiO@ CU"02 :olynmi.1 Ty" t oint o C)ri gin rit Wei fhtfionq: Axis Trans r"tion: Concentration unit:: "ol Pea:-to-Peak "PIXE-d-: Smoth :_. thing: Ind.. i-- I-C&" 1: Numbetr of @-ths: ing method: S-0 h BAS*Iin*3 j In valley threshold: Reduce peak tailing: Ftalsobaseline "xl--: peak Separation Drta,..vtertical threshold: DS,houlderIhohlld.rh,ol:d: r ptesponse Threshold I.vt h:ight: Abso ight: Rel&ative: h&to& : Absolute area: PtRCMA (Ch4) TINCo r-onc. a Disabled I 1:*.*.,.00*.,0, 2.000 '-" 0. n0. 0.273 gn:b led Di bld Nearest zxt @l Are:2 Li" Lclud. I/X me- 161 Znabled 2 1 300 00 2 .00 5.00 ,..bi.d 30.00 1-50. Dis&bld 0@0:.00.00,.:Dt :.,b,L.,d Di'sabl*d page 3 method Report .@h.d file: ML:.t dl@@.d: Co.po..d: Pr,.t.d: pito\14*thDB%1022994.mgb \14MSLYWXN"Gli--V&ts C-:@ o@z 25 06:39:55 199'r 4: IS (Ch3) non Oct 25 07:03:23 1999 C ,po"d MMO: Ianternal Ref.: o@.,tify T@:C. f St ndards: U r RF V.I-*: user p*&k factor: Integrate Window factor: ChroMtcqr&m "23 "&Ado.: Peak Location It T .:,I,* I w now peak 5*1 ction: A.,pon.. Response Type: A. spose: Calibr&ti.On Curves p@lyno.j.1 Type: point of origin: fit3VoTi htlng: U 1 rqansfo@tim: concentration iIms.ncoch3i TIC Fixd 1.000000, 1.000000 2.000 1.0000D. Disabled 1.040. En&bl ad 0.000, Di.abld U.S@e.t Lt.mal ,,gas I.Luear I/X man* "NO,@SI.t,: Peak-ttO-PO&k "Plltude: S.00 h SWm"odtohwIngs:ize isc@s): Numb* r of s@Oths: Smothinq "th0d: B.S.11... join @&JI.y threshold: l@n RI:d C*b.P::'I@t Peak Separation Dral vertical thr..h.1d: D tact should*rs: Should*r threshold; pL.,pa@st ThreShOl Reloati h iqht: Abs lUt h:19ht: R.l.ti are.: Ab.. lute area: 89 Disabled 2 1 30.00 200.00 00 5. 9D 0 0 0*&0b0l.d 3 1.50: Disabl:d o.oo nisbl d 2.00, D :.b ad 0.00, Dit ablled Page 4 1-1--Irlft AMELIA 062498: FACT QuattroM #6448E Equipment Log 99114 PAGE DATE: 10/22/99 ANALYST: ias STUDY NLTMBER-ITOX145 MATRIX:I!,tsem DESCRIMON.@DA 1&4dilu@tiOns FACT Method: ETS -5-1 Injectiovnolumc:_IouL Cycletime:10min.Electrodc:_K:@p@. Mobile Phase: (A)2.omM NH4CH3_CO2 TN-A- or stndrdnumber Prepared(date/by): (A) 9.90.8.5.-_10-14@ (A)10/1_6s/a9h9. Expires: (A)L/00--@ (B)MEOH (B)2L-A-2_945_ (131)0/20/i9a9s_ (B)_04100 Storeatroom tmV? m or N Guard colunm: None ------- Partnumber: na Lotnumber:_La@.@@ Analyticalcolumn-. Size:2 x 50 mm Pannumber0:55-701-2. TypeC:IS@ Lot number-. 11 Spherseize5:um_. Serianlumber-.051961Z 8. Analyticaplarameters: Dryinggas(Libr):100 ESI nebulizinggas(Llhr)0 LC Flowrate30:0.uLJmirL Back pressure_:2 Sheathgas (Llhr0) RPLC solventgradient:lomin-10-95 Time Lm_in_.I-1)0.00 2)1.00_ 3)5.50@ 4)7.50@ 51-Loo O/oB 10.0 10.0 95.0 95.0 10.0 Tuning method Method: Printed: Report C. \mASSLYNX\AMELTA-RATS.pR()\ACQUDB\PFOS1 Fri Oct 22 09:58:58 1999 ------------ ms -6KV Page I ms SOURCE ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. set 1.60 40 5 0.2 150 250 Rdbk 1.60 -14 -4 149 253 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.3e-3 msi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 15.0 15.0 2.0 0.0 4 650 Rdbk 7 Set 14.0 14.0 10 2.0 0.0 40 0 650 Rdbk 41 38 40 SM-1.9 bftth@d M-PO@ imeth-d: Last Modified: p.,.t.d: C: \W4SLYKX\AMZL--PATS ot 11 09:22:17 199 N-' @s Oct 22 09:59:09 1999 sai~t rmctlm Delay I M" @ :I ): of I UMB 0.00 ftl6C l@t.rChannelWAY SoCs 00:003 Span 1 D&ltDn3 0.000 5tart Tim- M(inmei" 1 10.00 End Tie S.C,) Coll Enarqy (eV) Cone V Rep*&tSChannel Parent Daughter D-all 15 1 413.00 169-00 0.30 30 runc@0- :2 mu r I mos. P"r ( tsp- Inter Channel Del&Y t 3..s Dalto( fts ) : Ssptaanrt (Ties KL- ) : ): End TLS- i KiR.P..tL: @nol Parent Dauqhtor * :'.'0 0-.-0.. D@all ) Call (30cs Luarqy 499.00 99.00 o.30 45 1 (eV) Coca 60 VI Function : 3 W" of I Name Inter Channel D&IAY Sp:n, St r 'TD@&--to(nM3L'--1 End Ti-e Mins ) : R-P t.Channel Parent S*CS Dauqht.r 1 427.00 40-00 Fair ( asp0.03 0.00 10.00 1 D"ll 43*csl 0.30 11 Energy CO 40 I-V) CO-60 vI Function : 4 "M of I mom Fair ( asp- Inter Cha=Ol D-18Y Sp nt Dalton ) :) sta I T , :i End tT is. min3 " Rep..- .( tCh.@n.1 Parent 1 499.00 S*c3 1 D@.qht.r 18-00 0.00 10.00 C--ll I Energy (3-c-) C-1 (.V) 0.40 .45 @n. 60 VI method RePOrt method File: Last Modified: Printed: I c: \man ly-\,-Olia-rate.pro\acqudb\10min-10-95 Friday, October 22, 1999 09:56t36 Friday, October 22, 1999 09:59;25 HP1100 LC Pump Initial Conditions Solvents A!k B% ct D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Crven Temperature Right(*C) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entr ies which are Time A% B% C% 0.00 90.0 10.0 0.0 1.00 90.0 10.0 0.0 5.50 5.0 95.0 0.0 '7.50 5.0 95.0 0.0 8.00 90.0 10.0 0.0 HPIIOO LC Pump External Event Timetable The Timetable Time Initial 0.00 0.10 contains 3 entries which column Switch Off Off Off Contactl Off On Off are Contact2 Off On Off D% 0.0 0.0 0.0 0.0 0.0 Contact3 Off Off Off Flow 0.300 0.300 0.300 0.300 0.300 Contact4 Off On Off Hplloo Autogamplor Initial Conditions Draw Speed Eject Speed (gl/min) Draw Position (mm) Stop Time (mins) Injection Volume(Al) Vial Number 200.0 200 0.00 9.00 10.0 13 Page 1 Pressure 400 400 400 400 400 Masslynx - SamPIG Ust Sample ListC::\MASSLYNX\amelia-rats.PRO\SampleDB\102299a.SPL Printed:FriOct 22 09:58:461999 Page 1 Page Posibon:(1,1) FileNaffm FileToict MS File IOMIN-PFOS-POAA-IS-PFOSA 1 102299001 MEOH Blank 10MIN-PFOS-POAA-IS-PFOSA 2 102299W2 MEOH Blank 3 102299003 TOX145-RBS10199-H20 Blk-12 SEE IOMIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 4 102299004 TOX145-RBS10199-Serum Bik-12,SEE IOMIN-PFOS-POAA-IS-PFOSA 5 102299005 TOX145-RTS10199-Serum Blk-12,SEE 10MIN-PFOS-POAA-IS-PFOSA 6 102299006 TOX145-RBS10199-6ppt@-12, SEE IOMIN-PFOS-POAA-IS-PFOSA 7 102299007 TOX145-RBS10199-10ppb-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 8 102299008 TOX145-RBS10199-25ppb-12, SEE IOMIN-PFOS-POAA-IS-PFOSA 9 102299009 TOX145-RBS10199-50ppb-12. SEE 10MIN-PFOS-POAA-IS-PFOSA 10 102299010 TOX145-RBS10199-100ppb-12. SEE IOMIN-PFOS-POAA-IS-PFOSA 11 102299011 TOX145-RBS10199-250ppb-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 12 102299012 TOX145-RBS10199-500ppb-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 13 102299013 TOX145-RBS10199-750ppb-12, SEE IOMIN-PFOS-POAA-IS-PFOSA 14 102299014 TOX145-RBS10199-1000ppb-12, SEE IOMIN-PFOS-POAA-IS-PFOSA 1165 110022229999001156 MTTEOOOXXH114455-B-RlRaTTnSSk--99RROO33224465MM., DDaayyll: 55nfxfy)kggl,kgDD,55G0--eexxttliOO/l1I9g//9999 IIOOMMIINN--PPFFOOSS--PPOOAAAA--IISS--PPFFOOSSAA 10MIN-PFOS-POAA-IS-PFOSA 17 102299017 18 102299018 TOX145-RTS-gRO3247M, Dayl, 5nV/kg.D50-WIO/19199 IOMIN-PFOS-POAA-IS-PFOSA 19 102299019 TOX145-RTS-9RO3248M. Dayl, 5nigfkg,D50-extIO/19/99 10MIN-PFOS-POAA-IS-PFOSA 20 102299020 TOX145-RTS-9RO3249M, Dayl, 5nV/kg,D50-extlO/19/99 IOMIN-PFOS-POAA-IS-PFOSA 21 102299021 TOX145-RBS10199-250ppt>-CCV-11-1, SEE IOMIN-PFOS-POAA-IS-PFOSA 22 102299022 MEOH Blank TOX145-RTS-9RO3250M, Day4, &ngfkg, D50-e@10/19199 IOMIN-PFOS-POAA-IS-PFOSA 23 102299023 TOX145-RTS-gRO3251M, Day4.5mg/kg, D50-extlO/19/99 IOMIN-PFOS-POAA-IS-PFOSA 24 102299024 TOX14r>-RTS-gRO3252M, Day4, 5.nvNg, D50-extlO/19/99 IOMIN-PFOS-POAA-IS-PFOSA 25 26 102299025 102299026 TOX145-RTS-9RO3254-lM, Day4 5mg/kg, D50- 10/19/99 10MIN-PFOS-POAA-IS-PFOSA 27 102299027 TOX14-r,-RTS-gRO3254-2M, Daiy4.5mglkg, D50- 10/19/99 10MIN-PFOS-POAA-IS-PFOSA 28 102299028 TOX14-r@-RBS10199-250ppb-CCV-1 1-2.SEE IOMIN-PFOS-POAA-IS-PFOSA 29 102299029 MEOH Blank IOMIN-PFOS-POAA-IS-PFOSA IOMIN-PFOS-POAA-IS-PFOSA 30 102299030 TOX145-RBS10199LH20 Bik-12,SEE IOMIN-PFOS-POAA-IS-PFOSA 31 102299031 TOX145-RBS10199-Serum Bik-12,SEE 10MIN-PFOS-POAA-IS-PFOSA 32 102299032 TOX145-RTS10199-Serum Bik-12,SEE 33 102299033 TOX145-RBS10199-5ppb-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 34 102299034 TOX145-RBS10199-10ppb-12, SEE 10MIN-PFOS-POAA-IS-PFOSA IOMIN-PFOS-POAA-IS-PFOSA 35 102299035 TOX145-RBS10199-25ppb-12, SEE 36 102299036 TOX145-RBS10199-50ppb-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 37 102299037 TOX145-RBS10199-100ppb-12, SEE TOX145-RBS10199-250ppb-12, SEE IOMIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 38 102299038 39 102299039 TOX145-RBS10199-500ppb-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 40 102299(AO TOX145-RBS10199-750ppb-12, SEE 10MIN-PFOS-POAA-IS@PFOSA 41 102299041 TOX145-RBS10199-1000ppb-12, SEE IOMIN-PFOS-POAA-IS-PFOSA Masslynx -Sample Ust Sample List:C:VAASSLYNX\amelia-rats.PROXSampleDBI102299i.SPL Printed:FriOct 22 09:58:461999 Page 2 Page Position(:2,1) InletFile BotiJa InjecVtolume Sample Type Cone A Conc 0 Cone C Conc D Conc E Conc F 1 lOrrir@-IG-95 91 2 10ftn-10-95 91 3 10niin-10-95 1 4 10ftn-10-95 2 5 10ftr@-10-95 3 6 10min-10-95 4 7 lOrt@n-10-95 5 8 10n@n-10-95 6 9 lOtTiri--10-975 10 lOrrin-10-958 11 lOrT@n-10-95 9 12 10n@n-10-95 10 13 lOrrin-10-95I1 14 10niir,10-9512 15 10n@r@-10-95 92 16 10min-10-95 13 17 10niirIG-95 14 18 10mir,10-95 15 19 10mir,10-96 16 20 10n@n-10-95 17 21 lOff@n-10-95 33 22 10mir@-10-95 92 23 10min-10-95 18 24 10ftn-10-95 19 25 10niir,10-9520 26 10niir@-10-95 21 27 10min-10-95 22 28 10min-10-95 34 29 10min-lG-95 93 30 10n@n-10-95 1 31 lOrrdn-10-95 2 32 lOrrin-10-95 3 33 lOrrdn-10-95 4 34 10ftr@-10-95 5 35 lOff@n-10-95 6 36 10niin-10-95 7 37 10ri@n-10-95 8 38 10mir@-10-95 9 39 10min-10-95 10 40 10min-10-95 11 41 10ftn-10-95 12 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 - 10 10 10 10 10 10 - 10 - 10 - 10 10 10 10 10 10 - 10 - 10 - 10 - 10 - 10 - 10 - 10 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - FACT: DATA REVIEW SUMMARY FORNI Datc: DataAnalyst: FACT Study Matnx(rimcpoints: //27,I-e SaMle LisL Set-upAnalysis DatdAnalyst lnstrument lo-,> 5*7L- 42,/)/'5"7 Analyte: @-"?799 Data Review Sign-Off . An slystReview Name / Date: TechnicalReview Name /Date: QuaHty AssuranceReview Name /Date: DataEnftr. IA(7, Cormnenb /Justifkjktions: nI , LOQ: R^2: !E-,7f / - CalibraCthieocnks- MS/MSD, DataStatLis: ExftctioBnknic MatrixBbLnlc /)@, -Z 41 ir Analyte: 22@222/19 Ar-ccptablLeinearRange: LOQ: !2 R^2: 7-7@Z ExtractedBlaniL< MatrixBw&. CalibmfionChock3: MS/NM: Data SULtus: m@r, LASE@ sitLU (ID@ -rtEZU. LAC lcl;il9i, Analyte: AcceptableLinearRange: LOQ: R^2: Uibmtion Checks: MSIMSD: ldataSatus: ExtracteBdlank: MatrixBla@- Z(A7L4 Q.-tity C@@PW-ld WI...-Y tox 145. DLat B"A, O&Y 1&4Lasdpi@l@ucl@ gnt 10/19/92 S.Mlg Litsite:d: L-t "i tied. L@t -dL job Od-: c: %=a# Me Oct 2ue Oct Nsoup42gl9t.pro@gmupla=%Ioagttb 25 16132z&2 1999 26 09:11.31 1 99 Printed: t- Oct 26 10-31.19 less 1 102599039 2 102599040 Sam alist T=t K*OK 1':lank M.09 'SI..k Type std C@ 7.213 7.416 7.424 A@ 40 5101 nea. bb bb 2.73 3 09 3:23 3 1025990401 4 102599042 5 102599 13 6 102599044 7 102599045 8 102599046 9 102399047 10 102599048 11 102599049 12 102599050 13 102599051 11 102599052 TIOXI -RSS10199 -920 alk-1 TTIoOxXiI'&SS--RRTDsSiIo01:9 -S- 'S I 9-S@ :lk2ik-12: Set TO ,5-RISIOI:9-Sp3.pb-12 Sax Tall -RILSIOI9- ovpb-li ToXxli &4 S-RBSJ0199-25ppb-12. SszIzRR 70 S-RDSIO199-Sappb-12 SRI TTOoxliats-RDSIO199-10 4S-RaSIO199-250 oppPb-1l2. SRI Toxni 4s-Rzslol99-SOORP9 12 Sam 1= as-RasiDI9"9--I7LsOoOOpP b-12: S= T*Xlds-RBSIOL ppb-12, S= St --A-rd SSttandard St and.@d St andard & rd stand 4 stad@@d SSttaannddaarrdd 49.93 249.2706 &9.30 'g."8:.60.,oo 735..0000 976 7.4012 7:4'176 77..349402 7 3980 7:.42 0 7.12. 77.41 A 7..&32973, 73 43 bmb 13S46 bb m 2 75: NK 5113 bbbb 2693 bb 6270 bb 13890 190si 2')424 bb 202 bb 2 84 1.12 6 7 2S 10.776 10, 22 16 27 103 0.56 3 2 @.2 -17 _I4 750 3. 6 10123., 570 -4 1 .:.70 15 102599053 moH al..k 7.330 3729 bk' 3 16 102591054L -7Maxi'as-RTS-9R032450. Dayl. SM/ lzg: 7 Adi 5S0326 bb 216:3705 17 102599055 n S-RTS-:R0.3241": Dayl : =, lkg. 7:178 bb 126.9 18 10259'9gOoS6 .7 TiDX1455:RTS - 32 LTK Day 7 3:72 bb 132-99 4 1 1025 5 ?on 45_ RTS-9R0324=9. Day I 5mikg: D500:@tlo*/199//:9 3 1460.71 20 102S99058 TOXI 4,S_ RTS-9RO3249M. Day li:sm/ kg stZs)5 .tl 248a 00 7.3530 2 4!491 bb 23 -7 21 102599059 TOXI's-Rasial0 99-25OVpb-CCV-11-1, oc oc 24 0 7.3 7 :170 bb 22@:,o2, 11 22 1025:990060 'MXI SIRDSI 119-250ppb-12. Szl 7.347 47 UK 2.99 2211, 11002255 '"900'6.12 025 9906 3 236 1025 4 27 102519065 28 102599066 21 102599067 30 102599068 31 102599069 32 102599070 33 102599071 31 102599072 35 102sggo73 36 102599074 37 102599075 38 102599076 39 102599077 40 102519078 11 102599079 42 102599080 43 102599081 41 1025990:2 415 1015990 3 M*08., -lk 7on T.__11.-::00@121..:My . SM/kg, TMoX2 4s-RTS- 32 'IN Dy4,'.Smtkg, 1)50--tio/199/:9 D50-OXtIO/I 1 9 n"_IITS-::0032:2M. . 1. .Ik.. .5@ --@% xi RTS- 32 4-im. yDO.ayy1 5m/]Lg 0"1911":; 15-RTS-9R03251-2M, : SM/kg: DDS5O0- 1.,19199 TWX-.n145-RDSIO191-23OVpb-CCV-11-'2L. SZE ?TcCXIAS-RDS1010999-92509Spob-12, SIZ mnxi S5--RRaISLiSo1 II" --225 Opvppbb--CCCCVV--111-14-.3, SSK"M moor 'Slank To= 'S-"Slo0l::-220 Olk-12. SM TO Xl45 _RTSJ I _S@ ilk_-I s : "22: 92 Mxi Tt) 's-Rasloal,9-sppb-12@,ssxz ToOXXI'II--RRB'S1L.S1I1l1'-21pOpbp-p1b2 I s TOX145-RSSIO199-50ppb- 2: Sze ToxX145-ft3siol9,9-1050ppb-12, szx ..XI1S&_SR-BRSsIsOlJol,99-_2500ppppbb:12L:2 Sze SICZ TOXI4S-RB 101:9:750P0 Pb-12- SILZ TOX145-RaSsiol 9 10 Oppb-12. SZE oc oc QC oc standard st...d."-d sSttandardd Standard St rd sSttandard &ndard Standard 248.00 248.00 21::000* 24 4.93 .76a 249g-0'o 97*60 218.00 4393.000 7,:.Ol 9 7 3:2 7:2 5 19 7 23 7 2 198 72 99 77..23,21 'I 2 7.224 7.267 7.245 7.2S7 7.234 7.268 7.259 7.2,691 "' 214 7:224 -1 7 7-.222:71 7.2 2 41285 bd 46009 1 bb 6 bd 463, bd & 126',7S NbKb 76S7o17 bb slas bb 6a bb : bb 69 bb bb lei mm 233 bbX 169 1 :. bbdx bbx 1 03 21815 31733 MMX 121. -PM ISS.585 1 9226 05 13.752':174 1'1'2.13 301 250.05 2783.0005 12 30 22 3 67 4 3 .0.4 7.'910 g.:4 1,0@ I 37.5.7 51 13 13 17 5 3. 7' 50 .73 5634 1157835..2390 6 0 omp 020111: gu@tified and printed by lOi2ill' Q@-tity comvOW4 &Ammry nevo@ %,..143. at S.... Day lal diluti@. 3bct10/19199 OMWIO &dot: L@t modified: notbod: L"t modified: job C."; C:NNUSLT=NSOW020159.p"%smpl*M%10259b Um Oct 25 16:33:OL2 1929 Tu. O@ 34 01,11:31 1119 r.i.t.di T.. Get 26 10:51-11 1299 P." 2 cc.qpmmd 2: PrC" 1 102599039 2 102591040 3 102599041 A 102599042 5 102599043 6 102599044 7 102599045 a lo2s99046 9 102599047 10 102599048 11 102599049 12 102599050 13 1025990S1 14 102599052 15 102599053 16 102519054 17 102599055 10 102599056 19 102519057 20 102599058 21 102599059 22 102599060 23 102599061 24 102599062 2S 102599063 26 102599064 27 102599065 28 102599066 29 102599067 30 102599068 31 102599069 32 102599070 33 102599071 34 102399072 35 102599073 36 102599074 37 102599075 38 102599076 39 102599077 40 102599078 41 102599079 42 102599080 43 102599081 44 102599082 45 102599083 Tm ig.On DI..k N*OH al-k AS-RRSIO199-820 Slk-12, SZE TOXI 45-RASIO199-S.@ nlk-12. SEZ TOZXI145-RTS10199-Se@ Blk-12, SXZ TOX145-IRSIO199-Sppb-12, Sol Toxl&5-RBSIG199-loppb-12. sn Wn4S-RaSlOL99-25ppb-12, Sao Ton&5-RBSIO199-Soppb-12. SU TK)XI45-RDS10119-100ppb-12. szx TOXJAS-RRS10199-250ppb-12, 1 sn TOX145-RASIO199-500ppb 2, sn S= 7?0=XI44-SRSB-SR1W01109199-97-5100p0p0bp-p1b2-,12. 5= DI.OU sl&.k TOMI&S-RTS-IR03245M. T=45-RTS-IR03246K. TOXISS-RTS-9RO3247M. T03a45-RTS-110324=, D-,Yl. Sm/iLg. Day,, sm/ka, Dayl. 'SM/kg. Dnaeyy@l,. SM/kg, Dso-MmID/19/99 DSO-.=Ioiig/,g DSO-Oxtio/19/9, DSO-"tlO/19/99 TonIS-RTS-gRO3249K. 5.0/ka. DSO---tlO/21/19 -MXJAS-RBLS10199-250ppb-CCV-11-1. 523 TOX145-RESIO119-2SOppb-12. szx 9.08 blank wxl&S.M-9RO32509, Tiola&S-RTS-9RO3351N, TOX14S-RTS-9RO3252M. DOY4, 5-9/kg, DSO--20/19/99 Day4, Sm/kg, D50-"tio/19/99 Ds,yt, 5.0/kg. DSO-@10/19/19 TOXI&S-RTS-9RO3254-IN. I)OY4L.SM/ILU. DSO- 10/19/9' TondS-IrrS-IR03254-2X. Day&, 509/kg, DSO- 10/19/99 TOX145-RBSIO199-250ppb-CCV-11-2. Sn 1=45-RBSJO199-2SOVpb-12. SU TOX14S-RBSIOI99-250ppb-ccv-11-3. gn TOXI&S-RDSIO119-250ppb-CCV_11_4. Sn TYP- Standard Standard Stnd-d Standard Standard Standard Stnda@d Standard Standard QC oc oc oc oc oc IMON Bl@.k TO)U&5-RRSIO199-830 TOX145-RILSIO199-S@ TOX1445-RTSIO199-S.@ alk-12, su Sik-12. SRS Slk-12, SZZ S-RIS10199-Sppb-12. TWoxnldS-RDSIOI19-10ppb-12. TOXIAS-RILS10199-25ppb-12. WX145-"SIO199-Soppb-12. Taxl4S-RaSlOI99-loopb-12. SZX SIR SZX SRS SRI TOX145-RISIO199-2SOppb-12. SZE TOXI&5-RDS10199-500ppb-12, SZX TOX145-RaSIO199-750ppb-12. Toxl45-RBSJO199-loooppb-12. 511 SIS St--A-@d Standard Stand@d Stad-d standard Standard St--d-rd St&nA-rd Standard a" 0- 4.93 9.77 24.80 49.30 97.70 241.00 493.00 736.00 977.00 248.00 248.00 248.00 -249.00 248.00 248.00 4.93 9.77 24-60 49.30 97.70 248.00 493.00 736.00 977.00 sm 6.165 9.175 4.230 9.252 2.240 2.246 8.2&3 9.195 8.239 8.221 8.201 8.202 8.178 6.115 8.132 9.135 S.247 9.163 9.143 8.097 8.157 8.143 2.133 0.159 8.092 7.$Ot 7.922 7.803 7.759 7.782 7.786 7.788 7.806 7.809 7.320 7.795 7.808 7.776 7.328 7.799 7.783 7.797 7.789 7.808 7.801 &x@ nags 101 bb 133 bb 178 bb 194 m 245 db 1430 ma 2534 M 6361 m 11166 "M 31368 UK 83269 M 161220 m 236589 M 113964 M 1523 m 2311 m 3545 NK 190, NK 2622 M 2129 = $6047 NK $4647 NK 442 m 677 db 633 M $28 db 599 UK 607 dd 81305 m 91754 Nk 393$8 Nk 86953 M 344 bb 302 NK 233 NK 298 NK 1667 NU 2361 NU 7460 mm 11953 mm 42260 NK $9431 m 179977 m 262487 MM IS6987 m c@ %0" 3.13 3.23 3.35 3.40 3.55 6.97 di 10.17 4 22.68 -9 35.12 -29 113.77 16 243.59 -2 463.97 -5 486.19 -7 910.61 -7 7.2& 1.52 13.09 8.59 10.42 8.99 251.63 1 2&7.58 -0 4.12 4.79 4.67 5.23 4.s7 4.59 238.15 -41 269.13 a 261.29 5 254.25 3 3.83 3.71 3.51 3.70 7.66 55 11.11 14 24.dl -2 37.41 -24 125.02 28 261.41 5 523.21 6 761.77 4 1035.00 6 wL-,Lvio@ ftLLdiA @m, PFVJA, urd,-I.valuzii-ep,ritc( lDli9i9l Soup 020111: gl@tiCLo4 and primed by m 10/29/11 ou@tify Campouxkd Summary ang*M 143: Mt $or^, "y 144 dilluti@. @ &aMl a latnti: : L"t modi ad MM fled: OCt 2S 14:32@42 1999 L"t .di Job C.": Tug o@ 26 ot:ll:31 1 99 printed: T.. ot 26 10:51:19 1999 10/19/99 C.mw-- 3: 0- 2 lG25,,.,, 10o255990o40 3, IQ25999odl 1 2 9 42 5 lo2599o43 6 102599044 7 102599045 8 102599046 9 102599DA7 10 102599048 11 1025990&9 12 ID2599050 13 ID2599051 14 102599052 25 102599D53 16 ID259905& 17 102599OSS 18 102599056 19 102599GS7 20 102599058 21 102599059 22 1025::0:01 23 102 24 lo2:99o62 25 1 2511 0 63 267 lo025S99990oo6645 2 a 1o2 5 29 1 10 2 S9999o06676 20 2 10 3 1 o25S9g9g0o668g 32 l1o2599o7o 33 102399071 34 102599072 35 102599073 36 10259907& 37 102599075 38 lG2599076 39 102599077 40 lD25l9O78 41 ID2599o?9 42 102599080 43 102599081 44 102599082 AS 102599083 "HE"OoRl:lllalntk @ K.OH blank TIDy,14455_-PRaBSSlIo0l1g9:_-SK@2O Blka11k2. SZX Taxi -12, SSR TT,aoX145-RTS10o199-S@ glk-12. SIR ToX145-RBS lol5:-S1 P%Lb-12i. Sn .M XI&S-ILBS1 19 - Oppb- X145-RBSIOI:9-25ppb-12.I S5I9M2 TOX145-RBS101 9-50VPb-12i.SSXZ XZ 7oXl:5-RBS101 9-10OVpb-I TOM1 ,S:RBS101:,9-250PPb-12. szz TID ,5-RD io0i 9-sosoovpb- I2 TioXXII 5 RBSSI 1 -7 Vpb- 2 : '=" 45_::Slolgg_loooppb-12, szz IRo=n Blank 7%)Zl1,5-RTS-9:03215M: S-RTS-, .32&SK T07*1 45-RTS-IR03247M. TDXI TD3a AS-RTS-9RO32489. Tond5-RTS-9RO3249M. Day I : ./kg: Dayl . Soo/ko . Dayl Sm/kg . D-yYlI. "SMa//ikcoo, MOD:wMloO/X:/91: Dso aml 0 /1 DSo _wMl 0 /1,/99 /19, /9 VDSSO-a-wMtlIO/i /99 To=45-RASIDIII-250ppb-CCV-11-1, Z= TIDZIAS-RRSI*191-25*ppb-12. SZZ Typ- SSttaannddard Standardd st :g tt-m-@d Stmmwlard tandard standard oc QC XTo-=oInBS&I5-R&aTkS-9RO32SON. Days. T4oXl 5 -RTS-9R0a32$IX, Day&, TDn 45:RTS -:RRo32:29, Dyt, SMiko -%-Q/kg: 3M/kg, DSD--tllo0l/ll:ll:: D50- 10/1:/9 Toxi 'S_ RTS- gto32 A-IN. Day&. sm/kg. ?UZI RTS- 01,32 54 -2M. Dy4, 5M/kg. mxi 45_RSSI 's- 019: -2S Opp b-ccv-11-2. SM vs DSDo-- 110//111/99 oc TOXI RDSI -250ypb-12. Sn oc Toxl4,5-RZS10199-25OVpb-CCV 11-3. szx oc TOXI 5-ILBS1:1:9-250VPb-CCV-11-4. SZZ oc N.Ion blank ToXl 45-RBS Toyl 45-RBS TO- 45-R- To- IS-TiDxl45-Ra lol99-92G glk-12 i2S 1 1 9-S- glk lol9g-S@ 21k-12: 10199-Svpb-12, - 10199-10vpb-12. S- Standard sstt,.@.,Irrdd TOU 45-=10119-25ppb-12, Sn Tooxll55--"slOI99-50VPb-12, : K@z Standard St.,@drd s XlAS- RB 1lo11l1'1999_:2o1o5Olppppbb-1-212: SSzZxZ TTO'XOIxl45-RILBBSSIC,1 9 SoOppb-12 TaX145-RAS10199gg:?StO)rPb-12: -s '" xils-Rasiol lo Oppb-12, 1S2xz standard t"dd SSttLanndd@ard d std c- .1. 1 ItT al il..oooo 1.00 i.oo 1 1:,oOoo 1 .0(, 1 1.00 1.00 1.00 1-100* 1,00 1. 7.213 7.213 23.o, 77*.21 5 77:,2o1l1 72 7.210 7.253 7:229 7 . 205 7 .234 7 .231 7 1653 7 21 1 7 7 27 1 7..IL46 7 .123 7 . Is& 7 .ISO 7 . 11613, 7 7.0074 7 ..971 7 .054 76 7:07@l 7.0080 7.loo 7 7..I1G124 7 .088 1l..0o0o 1.00 1I.0O0o 1.00 1.00 1.000 1.0 77..100912 7 .121 77.0o9gg2 7 7.102 7.08a2 7.1 9 1 7.0 8 A- 714w 14 bb 34971 bb 22834 bb 2olO bb 239839o7 bb 325,7.0 bb 205435 kbb 3 1 UK 317 3 038 bb 3041, bKHb 6, bb 66 bb 71 42 bb 41 bb 2@8o8o5 bb 3 bb hb 475 bb bb :OG bb 55 NN 1907 "H 2692489 NbKd 2911 bb 2 a bb 3618 M 3157 bb 294@l bbdd 3177 3076 bd 2950 mm 2748 MM 3443 bb 3426 bd 3712 bb 3771 bb 3695 bNKb o-. %D- o.co -loo 1 11 11 00.7 -;9 o0.9,13 -2 :7 0.92 0.82 -1: 010-0:71 --11 0o*911 :4 0 do -10 40 0 02 -5a 0:02 -96 0.02 -9: 0.9 0.891 -ii 0.0 O..o. -109: G.01 00..0022 9: 0.02 0.60 0.90 0.93 0.92 o.oo 1.15 --l7o -lo-o is 1.0lo, -ol 0@.-01 1 0 .9: 2 D::7 -136 I1-.o.l, I1 1.10a i0s 2 11..127 17 o @ c, CLnCL) CL@ r)6@ U@ea. LA [D izi B-P 020191: Q-@-tifid @d vrizd by m ID/24/lt T@ ids. at so... D.; 1&& 20/19199 Compound1name:PFOS CoefficienotfDetermination0:.997063 Calibratiocnurve:27.1171 - x + -33.7747 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighbng: 1/x,Axistrans:None 4.3Oe4- Response- -33 .0..0.. . . .. . 200.0 6--P 0201..99; Q-tLfid .d mitd kW ILO/25199 400.0 600.0 800.0 .-Conc Q@-tify cmalbratim T@ 149% Rat Nor&, fty 144 diluti@. lftt 10/19/99 Compound 2 name: PFOSA Coefficienotf Determination:0.992571 Calibratiocnurve:345.863 - x + -981.494 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:1/x,Axistrans:None x 3.57e5- x Response- x -981- 200.0 Soup 020199: Q@tified and primed by @ m 10/26/99 400.0 600.0 800.0 Conc 9.-,,Lty cailbrati@ ROP@ 2@ 14$z ILat "r&, Day 1&4 diluti@, UKt 10/19/99 Compound 3 name:Surr Response Factor:3154.38 Response type:ExternalStd,Area Curve type:RF 3.77e3- Response- P@ 3 x nv I--- 0.0 0.1 0.2 63 Sam 020199: Q@tified and Pcintsd bY Conc 0..4 0.5 0.6 0.7 0.8 0.9 1.0 method ROPOVT 14*tl@d file: Last @dified: Compound: Printed; C:\WSLYU@&OU02oig 1.1;.pro%mothDB\102599b.odb T" Oct 26 09:11,3 99 1: PPM T- Oct 26 10,42:14 1999 ccompound M@ Internal Rot.; o@tify Waco: Co=. of Standards; u :r ILFValu*: U: r Peak Factor: Int*g,ate Mind@ Fact=: CbL@-t.g.- -.. L.2-: R.t:ntiln,.tTi@ttai") ; .1 ti,. to. ion Time ItT Re f r=c&: Ti- Wid- (.i-) Peak Selection: pros ln@l TIC C- . A 1.000000, 1.000000 2.000 1.0000D. Disabled 7.&go. -bld 0.000. 0-&bld oIs- I .312 is@.t Re p@::Typ.: A.:P.- ]Polynomial Type; Point of origin: fit wighting: Axis Tr@fO@tiOn: Unit.: P.&k-t.-Pe.k Wlitud.: mct@l A.- Zwl%,de I/X 76 S-tk@i.a: Wi.d- :i.. (.C-): number f @ths: S@thing -@h-d: join valley tbr*ahold; Reduce Peak tailing: Raise 2-bid 2 I 320..-000.00. s0 Dratwacwtarsthiocualldertsb:xoab.1d: D. Shoulder threshold: Relative height; kb.oluto hight: Relative Ak..lut. 90.00 Disabled 30.00 l.SO. Disbld Di blod *@..0*00: Di=ld 0.00, Di..bld method Report Method file; Last modified: Compound: Printed: C:%KLSSLyMX\smpO2Ol99.pro\X&thD&\102599b.odb TU* Oct 26 09:11@31 1999 2; PROSA TUO Oct 26 lo:tstlt 1999 compound xnt.-I o@tify co=. of n R.t.; Tr@..: St@A"d.: user RY value: User Peak Factor: Xnt*gret. chr@togr@ Wind@ @s Factor: wind@: PPOSA (No-] TIC c- . a 1.000000. 1.000000 2.000 1.0000D. Disabld Retention Tim (wi@): Relative Retention Time WT R.f.@.-.: Time Wi@@d- ci-) peak Selection: 7.960, 0.000, two-I 0.400 -hl*d Diabled U.@"t R.sp@. Type: R..P.-.; Bt-l A..- rolyncial Type: point Of origini pit weighting: Axis Transformation: z=lude 1/X No.. unit.: Peak-to-P.&k amplitude: s@thi-9: Wind- ai.. (SC-): Number of @ths; s@thuw method: Join valley threshold: Red... Peak tailing: Mi.. b ..line ---i-: Pr@ vertical threshold: Dot.ct houlders: Shoulder threshold: Relative JLb-oluto Relative Akwalut. kwight: height: @00: 76 2 I 30.00 200.00 5.00 90.00 Di.@bld 30.00 I.SO. 0.00. 2.00, 0.00, Di.&bld Di-bld Di.@bld Di.@bld method R*Port wtk@d file: Last modified: C@.W..nd: Printed: C!XDLLSSLyUx\smp02Cl99.pro\methDB\lC2S99b.mft Tu. O@t 26 09@11:31 1999 3; S"r Tue act 26 10165:14 1999 C@.pa,wA K@ : internal mt. z Q@tity Tr@s: c@ of Standards: Us:r " Valual Us r ftak P CtOc: lnt*grate Wind@ factor: chr@togr= mass windm sI@N*") TIC rixd I.Oooooo. 1.000000 Diabld 21-.0.0.0.. RatI:ntion Time tai@) : Re ti- Time: RT tot r..c.: Time Wind- (@inm) Peak $.I-tio.: 1--P@ Typet 7.345 0.000: I IM.*3-01 M"bl ad Dia@bld m@..t lbm 1 Ply-mi.1 Type, Point of origin; pit W.ightina: Axis Tr@fO@tiM: Units: Peak-to-peak aMlitL%6*: smooth, i.. Logi:.. Coc- Number of @tkm: S-.hi method: Join -Il.y threshold: Reduce pe k tailing: Raise b":ii.0 Dr- "rtical threshold: Detect shoulders: Sl@lder threshold: Relative Aboo lute R.lati,. Absolute height: height: r..: area: I/X 65 3-bld 120..-000.01.0 5 90 00 D3 ia'.blod 0 00 1. ".: 02-1000. 0.00, Di:.bld i &bld "Di.&bld Disbl.4 Quattro 11,#6414E SOUP 020199:FACR Equipment Log 99092 PAGE 1/1 DATE: 10-25-99 ANALYST.Mmmh STUDY NUMBER, TOX145 MATRIX:Ratsera DESCREMONLDiLut-iQ-nk FACT Method: ETS-8-5.1 Injectiovnolume:_!DgL- Cycletime:10 rnin.ElectrodeZ,-Sipray Mobile Phase: (A)2.0mM NH4CH3CO2 (B)McOH TN-A- or stndrdnumber (A) 99085-11-3 Prepared(date/by): (Al)0@/21/99mmh (B TN-A-2997 (B)Jffl@L"sah Expires: (A0)4/00- Storeatroom temp? [@ or N Other. (B)-2010 - Guard column: None -Partnumber: na Lot number: Analyticalcolumn: KeystoneBetasil Size:2 x 50 nun - TypeC:18 Partnumber:055-701-2 Lot number:P9E II Spheresize:5 um Serianlumber:0591804Z Analyticaplarameters: Dryinggas(Llhr)3:50 ESI nebulizingas(Llhr)13 LC Flow rate3:00 uIJn-@n. Back pressure:65 bar Sheathgas(LAu)_g__ HPLC solventgradient:10min-10-95 Time (n-dn.) 1)0.00 2)1.00 3)5.50 4)7.50 5)8.00 %B 10.0 10.0 95.0 95.0 10.0 Tuning Method Report Method: C:\MASSLyNX\SoUp-RATs.PRO\AcQtMB\PFOS3 Printed: Mon Oct 25 16:37:32 1999 Page ms SOURCE ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. ms set 1.60 60 5 0.2 150 250 Rdbk 1.60 -60 -6 151 250 Pressures Analyser Vacu= Gas Cell Rdbk 5.9e-5 4.le-3 msi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier US2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 14.0 14.0 0.9 0.0 4 650 Rdbk 3 Set 14.0 14.0 60 2.0 0.0 40 0 650 Rdbk 42 38 44 Method: L-t madifid: lp.im.d: CPr"i'moct 13 11:35.03 19 Mm Oct 25 16:28.24 lg:: Sol@t Dla3r pumtim : I mi@ ) 1 0.00 mm of I M". VaLr ( zap- I ter Channel Delay S@s 9= ( D.It- ) , Start Ti@ ( Ki" End Ti- I Ki- 0-00 R.P.At. Channel Parent Daughter Dw*ll (S@s) Coll Snargy (*V) Cam V 1 413.00 169.00 0.30 30 is rw-ti- :2 um of I U". pi. c a"- I ter Channel Delay S*cs ) : S= ( Delta- ) : * :0.30 Sta t Tim ( Mi tndrti@ Mi@@) I Repeats Channel Parent Daughter vwell (S@s) Coll Energy (eV) C@ V d99.00 99.00 0.30 As 60 ru=ti- ,3 IS.pt_or (ChD-e-l-ta"I Dl)y , of I Mae Sets P.L. ( Mr00:0003 Start Ti- ( Ki- End Tim Ki" 0.00 10.00 R.P..t. I Channel Parent Daughter Dmll (S@s) Call Energy JeV) C@ V 1 498.00 78.00 0.30 45 60 Functim : 4 @ of I u@ pi. ( ZBP- I ter Channel Delay S= ( Dalta@ ) : Start T@ M(i-Ki- S@s 0-.0.1a R.d Tim 0-00 R@p.at@ Channel Parent Daughter D@ll (S@s) Call Energy lov) Co@ V 1 427.00 go.00 0.30 40 60 Method Reiport Method Tilm: Lost Modified: Printed: c: \=&sslynx\scrup-rats.pro\acqudb\lOzLin-10-95 Monday, October 25, 1999 16:29:58 Monday, October 1 25, 1999 15:34itS NPIIOO LC Pu=V ZiLitial Conditions Solvents A% B% C% D% Flow Stop Min Max Oven Oven (ml/min) Time (mins) Pressure Pressure (bar) (bar) Temperature Left(OC) Temperature Right(OC) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 HPIIOO LC Pump gradient Ti@table The gradient Timetable contains 5 entries Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 which C% 0.0 0.0 0.0 0.0 0.0 are D% 0.0 0.0 0.0 0.0 0.0 HPIIGO Lc Punv axto=al Zwent Timetable The Timetable Time Initial 0.00 0.10 contains 3 entries which Column Switch Off Off Off Contactl Off On Off are Contact2 Off On Off Contact3 Off Off Off Flow 0.300 0.300 0.300 0.300 0.300 Contact4 Off On Off H?lloo Autosampler 1ZLitiai Conditions Draw Speed Eject Speed (iil/min) Draw Position (nun) Stop Time (mins) Injection volume(pl) Vial Number 200.0 200 0.00 9.00 10.0 9 Pago I Pressure 400 400 400 400 400 Masslynx - Sample Ust Sample Ust:C-\MASSLYNX\soup-rats.pm\SampleDB\102599b.SP@ Pdnted:Mon Oct 25 16:32:571999 Page 1 Page Position(:1,1) FileName FileText MS File 1 102599039 MEOH Blank MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS IOMIN-PFOS-POAA-PFOSA-IS 2 102599040 3 102599041 TOX145-RBS10199-H20 Bik-12,SEE IOMIN-PFOS-POAA-PFOSA-IS 4 102599042 TOX14-r,-RBS10199-Serum Blk-12,SEE 10MIN-PFOS-POAA-PFOSA-IS 5 102599043 TOX145-RTS10199-Serum Bik-12,SEE IOMIN-PFOS-POAA-PFOSA-IS 6 102599044 TOX145-RBS10199-5ppb-12, SEE IOMIN-PFOS-POAA-PFOSA-IS 7 102599045 TOX145-RBS10199-10ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 8 102599046 TOX145-RBS10199-25ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 9 102599047 TOXI 4-r@-RBS101 99-50ppb-1 2. SEE 10MIN-PFOS-POAA-PFOSA-IS 10 102599048 TOX145-RBS10199-100ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 11 102599049 TOX145-RBS101"99-25oppb-12, SEE IOMIN-PFOS-POAA-PFOSA-IS 12 102599050 TOX145-RBS10199-500ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 13 102599051 TOX145-RBS10199-750ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 14 102599052 TOX145-RBS10199-1000ppb-12, SEE IOMIN-PFOS-POAA-PFOSA-IS 15 102599053 MEOH Blank IOMIN-PFOS-POAA-PFOSA-IS 16 102599054 TOX145-RTS-gRO3245M, Dayl, 5mgtkg, D50-extlO/19/99 10MIN-PFOS-POAA-PFOSA-IS 17 102599055 TOX145-RTS-9RO3246M. Dayl, 5mgtkg, D50-extlO/19/99 10MIN-PFOS-POAA-PFOSA-IS 18 102599056 TOX149-;-RTS-9RO3247M, Dayl, Smgtkg, D5D-extlO/19M 10MIN-PFOS-POAA-PFOSA-IS 19 102599057 TOX145-RTS-gRO3248M, Dayl, Smg/kg,D50-extlOtl9/99 IOMIN-PFOS-POAA-PFOSA-IS 20 102599058 TOX1 45-RTS-9RO3249M, Dayl, 5mg/kg, D50-extl0/19/99 10MIN-PFOS-POAA-PFOSA-IS 21 102599059 TOX145-RBS10199-250ppb-CCV-11-1, SEE IOMIN-PFOS-POAA-PFOSA-IS 22 102599060 TOXI 45-RBS1 01 99-250ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 23 102599061 MEOH Blank IOMIN-PFOS-POAA-PFOSA-IS 24 102599062 TOX145-RTS-9RO3250M, Day4,5mg/kg, D50-extIO/19/99 10MIN-PFOS-POAA-PFOSA-IS 25 102599063 TOX145-RTS-9RO3251M, Day4,5mg/kg, D50-extlO/19/99 IOMIN-PFOS-POAA-PFOSA-IS 26 102599064 TOX145-RTS-9RO3252M, Day4,5mg/kg, DSO-extlO/19/99 IOMIN-PFOS-POAA-PFOSA-IS 27 102599M TOX145-RTS-9RO3254-lM, Day4, Smg/kg, 050- lOtl9/99 10MIN-PFOS-POAA-PFOSA-IS 28 102599066 TOX14-r--RTS-gRO3254-2M,Day4,5mg/kg, D50-10/19/99 10MIN-PFOS-POAA-PFOSA-IS 29 102599067 TOX145-RBS10199-25oppb-CCV-11-2, SEE 1OMIN-PFOS-POAA-PFOSA-IS 30 102599068 TOX145-RBS10199-25oppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 31 102599069 TOX145-RBS10199-25oppb-CCV-11-3, SEE 10MIN-PFOS-POAA-PFOSA-IS 32 102599070 TOX1 45-RBS1 0199-250ppb-CCV-1 1-4,SEE 10MIN-PFOS-POAA-PFOSA-IS 33 102599071 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 34 102599072 TOX145-RBS10199-H20 Blk-12,SEE 1OMIN-PFOS-POAA-PFOSA-IS 35 102599073 TOX1 45-RBS1 0199-Serum Bik-12, SEE IOMIN-PFOS-POAA-PFOSA-IS 36 102599074 TOX1 45-RTS1 ol99-SerLim Blk-12,SEE 1OMIN-PFOS-POAA-PFOSA-IS 37 102599075 TOX145-RBS10199-5ppb-12, SEE IOMIN-PFOS-POAA-PFOSA-IS 38 102599076 TOX1 45-RBS1 0199-1 Oppb-12, SEE IOMIN-PFOS-POAA-PFOSA-IS 39 102599077 TOX145-RBS10199-25ppb-12, SEE 1OMIN-PFOS-POAA-PFOSA-IS 40 102599078 TOX145-RBS10199-5oppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 41 102599079 TOX145-RBS10199-100ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 42 102599080 TOX145-RBS10199-250ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 43 102599081 TOX145-RBS10199-500ppb-12, SEE 1OMIN-PFOS-POAA-PFOSA-IS 44 102599082 TOX145-RBS10199-750ppb-12, SEE IOMIN-PFOS-POAA-PFOSA-IS 45 102599083 TOX145-RBS10199-1000ppb-12, SEE IOMIN-PFOS-POAA-PFOSA-IS Masslynx - Sample List Sample List:C:\MASSLYNX\soup-rats.pro@Samp[eDB\102599b.SP@ Printed:Mon Oct 25 16:32:57 1999 InletFile Bottle InjectVolume Sample Type Conc A Conc 8 Conc C 1 10min-IG-95 91 2 10min-lG-95 91 3 10min-lD-95 21 4 10min-10-95 22 5 10min-10-95 23 6 10min-10-95 24 7 10min-10-95 25 a 10mir,10-95 26 9 10min-lD-95 27 10 10min-10-95 28 11 10min-10-95 29 12 10mir,10-95 30 13 10min-10-95 31 14 10min-10-95 32 15 10min-10-95 92 16 10min-10-95 33 17 10min-10-95 34 18 10min-lG-95 35 19 10min-lG-95 36 20 10min-10-95 37 21 10min-10-95 43 22 10min-10-95 29 23 10min-10-95 92 24 10mir,10-95 38 25 10min-10-95 39 26 10min-lG-95 40 27 10min-lD-95 41 28 10min-10-95 42 29 10min-10-95 44 30 10min-10-95 29 31 10min-10-95 45 32 10min-10-95 46 33 10min-10-95 93 34 10min-lD-95 21 35 10min-IG-95 22 36 10min-10-95 23 37 1Omin-1 D-95 24 38 10min-lG-95 25 39 10min-10-95 26 40 10min-10-95 27 41 10min-10-95 28 42 10min-10-95 29 43 10min-10-95 30 44 10mir,10-95 31 45 10min-lG-95 32 10 10 10 10 10 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 10 10 10 10 - 10 10 ac 10 ()C 10 10 10 10 10 10 10 (:)c 10 ac 10 QC 10 ac 10 10 10 10 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 4.93 4.93 - 9.76 9.77 - 24.8 24.8 - 49.3 49.3 - 97.6 97.7 - 248 248 - 493 493 - 735 736 - 976 977 - - - - - - - - - - - - - - - 248 248 - 248 248 - - - - - - - - - - - - - 248 248 - 248 248 - 248 248 - 248 248 - 4.93 4.93 - 9.76 9.77 - 24.8 24.8 - 49.3 49.3 - 97.6 97.7 - 248 248 - 493 493 - 735 736 - 976 97'7 - Page 2 Page Position(:2,1) FACT: DA*RA UVIEW SUrvItNIARYFOPiNt Datc: DaL2 AiWyst; FACT Study 0: Matnx/Timepoints: SarnpleL,6L- 0v@ Set-upAnalysis DatrJAnalyst: Instrument /O-g --TA Ana": ApubW L LOQ7 RA2: R.Lng. -5-'-F30 o ExMbcdm Blank Ma= BWk C&Hbmtion Checks: ik@Awii Data Stabw Data Review Sip-Off . An airt Re-,icw Name /Date: TechnicalReview Name /Date: QuaUty Assurance Review Name IDate: Data Inny. Ein" LA Commenb /Jusdftations: 61 ID ),21 9 Analyte: AcccptRble Linear Range: LOQ: R^2: CalibrationChecks- ExtractedBWk Matrix BWxk /;7 ar/' Data Sww. Auslyte:, e' iiJ AcceptgLbleLincir Range: 9 LOQ: Exuwted Bluir R^2: Matrix Bbmk. CalibrationChecks: MSIMSD: idati Satus: ou@@fy C@wamw Tox 145: PAt S@a Summ@Y and "@, Day I & 4 SmWle LL$t: "at modLLod; method: @.d: J,;t -.L@f C.": C: \XUSLY="Da@A707 mo\samplem\102799k) Thu Oct 20 09:14:03 1::; C: \NNSSLtrAr%Da A70799. =Q\Mtbl3a\102799b Th. O@ 24 09:37:22 1999 Pr=tad: Thu oat 28 09:27:L5 1999 cmip 1 1: PWA I 1.@1,99013 2 11 027:90114 5 27 990 16 I1 10127 90 5 11 027990171 6 1 027990 1 8 7 1 027 9 a9 02799990020 1027:90921 1027 022 10 1027990203 12 102799 24 13 1l0a27::0025 14 27 26 15 11002799027 1 6 10 2799:0022: 7 27 18 102799030 19 11 0279:031 20 0279 032 21 11 0279:0343 22 1 027999 03 5 23 027 03 245 11 0279:036 2 0279 037 26 102799038 27 102799039 20 102799040 29 1027:90414 30 027 90 2 31 102'199043 32 11 0279904445 33 1 027990 34 102799904647 35 027 0 36 102799048 37 102799049 38 102799050 39 1002799051 2799052 :1 @02799053 42I 102'199OS( 43 11 02799055 4 02799056 454 102799057 :6 1027990589 47 102799060 4: 102799061 50 102799062 51 11 027990:3 52 027990 4 102799065 5s3t 102799066 5 102799067 556 10279go6a 57 11 02799069 02799070 55: 102799071 (f@ 1) 3&WI*Ust 51-k M.OR T=t N-OK 81-k TOX14154-R5RS10229-R2o TOX -RBS10229-Se@ Blk-1, RWW glk-1, RWW TOX14l5a-RBS102I29-lppb-1 I RWW TOX 1, S-RBS I0229-Sppb-- : RW T S-RB 1 0229-10p5pb-I 1 RWW TaOXXI4 5-RBS5 0229-2 ppbT Xl1:5 -RBS1022:-5.Oppb-I : RWW mm TOOX 5-RRSlO22 -1 Dppb-i. RWW TOX I&S-RBS10229-2$Oppb-1, PW TOXIIS-RBS10229-500ppb-1, FMW To lt5-RB$10229-7$Dppb-1, I&V TOXII&S-RRS10229-IGOOPpb-1, AW M.OH Bl-k TCX14154-RTS-:Ro TOX S-RTS- 3230N: R03231H oyi Dayl : 1,-.Xtlo/19/99 C.m-trto1l0, -"tl 0/ 19/ 99 TOX14S-RTS-9RO323ZK, TOX 11445-RTS-:Ro 3233M, TOX 5-RTS- R03234M, Dayl, Dayl, Dyl, TOX145-RI&SIO229-2$Oppb-1. contral,@xtIO/19/9: cmtrol, -"t 10/ 19/ 9 cmtr.l,-..tlO/19/99 RWW M.CH Bl-,k X@45_R-TS-9R03235H TOoX145 RTS-9RO3Z36M : S-RTS::RO3237M: TOXXII:4 S-RTS _g R 3238H . TOX R0a3239H TOX141 5-SA-RRST1S0229-2$Oppb-1, Day 1 ll:/:: D4y :: @c-mttrtool :-:x,ttll.o/l9 "g Day tI Da :4,: C-Mttrrooll Dy y Miw "tlo/l -:XtIOO/199//99 xtl /1 /99 M.OH 4i5l@k TOX s- 0 Dayl, 5&q/kq, TOX1115 -RATTS 9gRR032324I SGMN: Dayl, Sg/kg, TOX14I5t-RT - 32 TH Dayl, Sag/kg, TOX 5-ATSS-:11"032:BX: Dyl, Sag/kg, TOX1:15-RTS-9RO3249M, Dayl, 5=g/kg, TOX 5-RRS 10229-250ppb-1, RWW M.OH 91-k extlo/19/99 ..tlO/19/99 extIO/19/99 eXtIO/19/99 *xtlO/19/99 TO 1I:5-RT -9RO32SOM: Day:: 5.q/kg t 0/19/99 TOX S-RTS-9RO3251M Day TOXX 145-RTS-9RO3252M, Dy4, TO :5-RTS-99R 3254-IM: 0. S5.g9// lIcgg,:g-,:X,ttlloi0//1199//9999 4, 5.g/ *xt 10/19/99 TOXII S-RTS- R003254-ZK Dayy4, 5.g/kg, xt 10/19/99 TOXx145-RBS10229-250ppb-1, P.WV H.OH 4581-k TOX 145--RTL-9RO3247-M, Dayl, Sag/kg, ext 10/13/99 TOX RTL- 9R2O3253-M. Day4, Saglkg, *at 10/13/99 TM OX145-RBSIO 29-25oppb-1, Rww To.x0m 'sBI-k 229-620 Bik-I I RWW TTOOXX1114155---RRRBSSlIGO229- , alk-' , RWW RBS10229-1 S=J, RWW T X114,5-RBS110229-$ppb-I RNW Toox 14 5-RB 0229-10ppb.-i, Fuv TOX 5-RAS1012029-25ppb-I I MN T.OTXo145I-19S S la 229-50ppb- RkV Xi I-RIISI.22:-100ppb-" RWW 45-RBS 22 -2 'Oppb- 1, lww TOX1 TOoXI&1S4:RBSIOZ21 9,-75,00ppb-,. RWW s 22 - Oppb-- RWW Toyx'lt5s-RRBBS010229-1000ppb-1, RWW Std C@ 0.99 4.93 9.76 24.380 :9.,, 24 '7'0 0 4930' 0 0 735 '0 0 976:000 248.00 .0 21.. 248.00 248.00 248.00 0.:9 4:,l 24.80 6 49.30 97.60 248.00 493.00 735.00 976.00 ItT 6.822 6.793 6r.821 .825 6.8 ...131 6.02 6.925 6 :-:019 6 ' el '1 6 00 1 6 6076 6:809 6.844 3 11 6'922 6 820 6'8 6:8'2'1' :.:20 6 'l 6 01: 6:80B 6.:Il 6 7:1100 oil :.$ 6 6.800 6.8122 6.8 6.81810 6.839 6.:Ill ::.19 6.82 0 6.8a1l15 6. 0 7.173 6.00 6.71: :.:2038 6:806 6.814 :.791 -:0'1 6 0111 6*795 6 815 6 806 6 :26 6 12 6'812 A@ 557 315 5022 1:09 611151 703 1292: 21111 390 17542745 129136 4 23025499 362 38l9@: :255 514346 7'9:11 27 0 3172 4390 .16@14 '37:2 75 5 1 37519 0 468 541 42376 360393 0 :1 03180 a 2:217 2.0:,l 3 35,:14 3 360 62686 79 ::'1 07005 225 5847 5385 2075 72285 1503 4 2 810 3 29 5697 5 117936 0 2003 :3 3 67 2 374&917 c@.(ppt) 0.0000 a 0:..0.0 0. 0 . 00 0 . 00 00 0@.95 @o3g9.,0l7 riago bd H'H' mm m?mmx MMX MbMbX V7.72 "mmM 401.04 bb 753.30 9370..8060 bb bb 0.00 bb 0.00 bb 0.00 bb 0.000 bb @170:005 ' bb 00 .00 bb b 0 -00. bbb 0"00 bb 0:00 bb .00 bk, 2780 17 bb 0: bb 107.9500 bb 147.35 bb 129.31 bb 102.84 bb :03 bb 219129O..o0 bb bb 03 bb :-a, 104:': 10a0l..9:0l bb 299.90 bkbb 0.00 bb 0.00 kb 0.00 bb 318.29 0.00 dmbm bb 0.00 bb 0.00 bdX 0.00 bbX 00 bbX 05 :.35 bbX 1971 .811 bbX 3 bbX 4490.96 bbX 12015.441 bbX 52. 29 bbX lS43.4 bbX %D- -1@0.00 -1-10,0 -211 13 12 -2 2 -4 16 12 is 21 28 -10 -1001 -100 -3 S al 5 6-51: gTL PXCLP LAC@ I D)ai Da@y 070799: q@@tated and p@tod by mehlo/2o/gg Q@tify C@.p@u.4 3U.-@y R.P-@ Tox 145: PAt S"a and Li@, Day I c:\mmsLYNX\D.@.y07O799.M\S@Wl.M\102799b Sample List: Last modif&od: Thu Oct 28 09:14:03 1999 bfttk.d: C:\m&ssLyXX\Dvy07O799. PRO\bftthM\102799b L.., .dif..d:Th. Oct 28 00:57:32 1999 i.b Cd.: Pr=t.d: Thu Oct 28 09.27;L5 1999 C@.p@und 2: 980 (f- 2) 1 NJ 102799013 2 102799014 3 102799015 4 102799016 5 102799017 6 102799018 7 1027999019 a 1027 9020 9 102199021 10 102799022 11 102799023 12 102799024 13 102199025 1& 102799026 15 102799027 16 102799028 17 1027990Z9 02799030 11 102799031 20 110279:032 21 27:9033 22 102799 034 23 1027 035 24 10279:0376 25 10279 9 03 26 10279 90389 27 1027:90,30 28 102'799 041 29 1027 99 0 , 30 1027 0 2 31 10279904,3 3@' 1027990 4 33 102799045 34 102799046 35 1027990 7 36 10279,104:. 37 10 27 9 90 So 38 27 90 3490 1002799051 279:052 41 10279 9 053 42 10279 9 054 43 10279 9 055 44 1l0a279 056 4456 10 27:9057 47 la279 905: 27 905 48 1027:90:01 49 1027 90 50 1027990:2 51 1027990 3 52 1027990964 53 10 2799065 54 10279 066 55 102799067 56 102799068 57 11 027:9007609 1 0279:0_,l 027 S..pl.Ust T"t M*CH Blank HOOR Blank TOXIIS-RES10229-IL20 Blk-1, RWW TOX145-RBS10229-S.@ Blk-1, RWW TOX145-RB$10229-lppk>-I, RW Toxl45-RBS10229-5ppb-1, MM T XI&S-RBS10229-10ppb-1, RW ToOXJAS4 -RB$110229-2$ppb 1: WW Toxi14 S-Ras 10229-50ppb-I F&V Tox 5-RBS 0229-10 Oppb-1. MiW ToXl:S-RB 1,00229:2SOppb-1: FW TOX1 5-RBSS 229 500ppb--l PWW TOX145-RDS1021209-750ppb--LI,RWW TOXJ S-RRS M.OH 4 Blank 229-1000ppb- TOXI15-RTS-9RO3230M. Dyi, JWW cmtrol,---tlO/19/99 TOX145-RTS-9RO323LM. TOX145-RTS-9RO3232m, TOX145-RTS-9RO3233M, D&YI, Dayl, Dayl, cmtc0l, --tlO/19/99 cmtrcl,-*Xtl /19/99 control,-OxtIO0/19/99 TOX1454-RTS-09ZRO232345M, D&yl, cmtrol, TOXI 5-RBSI 9-2 Oppb.-I, RWW -*xtlo/19/99 H.OH Blank TOX I45_RTS-9RO3235M. TOX14$4 -RTS 3230( Toxi14 S-RTS--:9P,L.o003237M:. 0 3236H TOoXl14,5-SR-TRST-S9-R1022 3239M Day&, DOY4, Day4, Day4, Day4, cOntt0l,-GxtIO/19/99 cmt.ol,-Oxtlo/,:/:9 control.-*xtlD/l / 9 cmtr0l,-*XtIO/1:/:9 cmtrol, -*xtIO/I / 9 Tox S-R]3s 9_250ppb-1, Rw MT*OOXH145Blank -RTS-9RO3245M, Toxl,4S-RT -9RO3246., Dayl, Sag/kg, XtIO/19/9 D.,l, Ig/kg, *Xt.0/19/9: TOX1 S-RT'SS-9R*3247M, Dayl, 5-9/kg, -xtlO/19/99 TOX145-RTS-9RO324 ", Dyl, 5-9/kg, -xtlO/,19/999 TO 1I:5-RTS-92R2032429Mo@pda yi, 5.4/kg, ..tlo/ 9/9 TOXX S-RBSIO 9- 5 b-1, PJ-V M*OH.Bl-l TTOoXI -RTS-9R03250M. Dy4, 5ig/kg, -xtlO/1:/:9 X145-RTS-9RO3251M, TOX145-RTS-9RO3252,M, D.y4, 5.q/kg, extlO/l / 9 D.Yi. 5=9/kg, *Xtlo/19/99 TOX145-RTS-9RO3254-IN, Day4, 5-9/kg, -xt 100 /19199 TOX145-RTS-9R 32545 -2M, Dy4, 5-9/kg, 0-t 1 /19/99 TOX145-ILBS102029-2 Oppb-1, RWW H.OHJI!B,lank TOX -RTL -9R03Z4-Y-K, Dyl, 5ag/kg, TOX11,45-RTL-9RO32S3-M, Dy4. Sg/kg, TOX RD 10229-250ppb-1, RWW H.OH 5Bl-ank, TOX 1445-RBS 10229-RZO Blk-1, RWW TOX1 S-RBS10229-S.rm Blk-1, RW ext 10/113/99 xt 10/ 3/99 TOX144S-RBS10229-lppb-i RWW Toxi S-RBS10229-5ppb-1: TOX1:5-RBS10ZZ9-IOPPb-1, TOXI S-RBS10229-2$ppb-1. TOXI S-RBS10229-50ppb-1, TOX145-RBS10229-100ppb-1, TOXI&5-RBS10229-250ppb-1, Ww RW IWW R%V RW Rww TOX14154-RB5102291-0500ppb-1. RWW TOX,,I,-RBSI.229-750(pp)b-I AW Tox -RBS 229-10 Dppb-i, AW std C- 0.99 4.93 .76 249 4997,-38600 246'000 493:00 735.00 976.00 248.00 218.00 248.00 248.00 00 248. 0.99 3 ,9 .1I6 24:8 49.3 0 97.6.0 21.. 693.00 735.00 976.00 7.542 7.585 7.594 '7*5 7.5 9: 7.590 7.589 7.594 7.595 7.593 7.588 7.5:4 7.5 5 7.599 7.590 7.583 7.590 7.5980 7.592 7.5 4 7 593 7:589 7.598 7.594 7,5:7 7.5 1 7.525 7.5790 7.5 7.5.: 7 597 7:@.1 7 592 7.599 7.586 7.596 A@ c@ .(Ppt) rlq. %D- 24 84 173 3946 a9 1636 3918 6110 9343 10952 0.99 pm 1 4.60 bb -7 9.95 bb 2 23 340 MM 50 S bb -6I 97.73 bb 0 234.77 bb -5 366.38 MKX -26 560.46 bbX -24 657.07 bbX _33 4004 239.94 bb -3 4224 2501 2969 3580 27442 33 3 4039 1770 104 91'. 11 337 603 4020 3 912'16 @7 9 23 11 00 S2 427 0 6743 9918 11346 253.16 bb 2 1479.:7 b 1 7. 0 bb 214.47 bb 1064.1: bb 2 0.2 bb 242.02 b b -2 105.63 bb 3 bb :5'12 79:5:- 7.15 bbb 9 bb 240.87 bb -3 581.536 bb 3 222..814 bb -10 0.93 NU -5 5.53 bb 12 .61 8 bb -11 25a 5 bb -1 43.'64 klb 108.08 bb 1 21@..l 2 404.41 bbx -1 595.01 -1 660.77 bbbbXX -30 a,-L Page 2 D&vwy 070799: q@n"t&ted and p@ted by =LhIO/20/99 0-tify Compound Sum@-y Pmp=t I Tom 145: R&t S@& AM L&@ , D&Y 1 6 A --Nple LLst: Last mocufxod: Method: Last madif@od: Job Cd-: C:\WXSSLyMrDa@wy07O799.no\sanple=\102799k, Thu Oct 29 09:14:03 1999 C:\WmsLyMX\Davwy07O799.PRD\)ftthoB\IC2799b Thu Oct 20 OS:57:32 1999 Pr-L.d: Thu act 29 09:27:15 1999 Compound 3: 0 N1 102799013 2 102799014 3 102799015 & 102799016 5 102799017 6 102799018 7 1102799019 02799020 1102799021 11 1002799022 12 10279:023 10279 go024 13 279go 25 14 10 279 26 15 102799027 102799028 I@76 @.2799029 2799030 1@98 1002799031 210 100279:032 279 033 22 102799034 23 102799035 24 1 02799 a 367 2 5 12 9:.3. 26 @.2779 3 27 102799039 28 102 40 29 102799:0041 30 102799 042 31 1l0o2.7,99101.1 799 4 33 102799045 34 102799046 35 102799047 36 102799048 37 102799049 38 1027990SO 39 102799051 40 102799052 41 102799053 42 102799054 43 102799055 14 102799056 45 102799057 46 102799058 47 102799059 48 102799060 49 102799061 50 102799062 51 102799063 52 102799064 53 102799065 54 102799066 55 102799067 56 102799068 57 11 02799900679 5: 10279 0 5 02799071 (f@ 3) I-SPI&llst T=t M.OH Bl-k M.OH Bl@k TOX145-RDS10229-IL20 Blk -1, RWW TOXI&S-ILSSIO229-Ser- Bik-1, PUV TOX145-RBS10229-lppb-1, AW TOX145-RBS10229-$PPb-1, TOXJ&S-RBS10229-10ppb-1, RWW R-W ToXI45-RBS10229-25ppb-1, RWW Toxl#S-RBS10229-50ppb-1, P" TOXJ#$-RaSlOZ29-100ppb-1, OW TOXI&5-RBS10229-250ppb-1. RWW TOXI1:5 -ROS10229-500ppkl-l, RWW TOX 1,S-RBS10229-750ppb-1, Wd TOX S-RaS10229-1000ppb-I., RWW K.OH 4531-k TOXI -RTS-9RO3230M, T01145-RTS-9RO3231M, TOX11445-RTS-:RO3232M: TOX 5-RTs- R03233H Dayl, Dayl, Dayll D&yl, cmtr0l,-*KtlO/19/ @-t@-1,-*xtIO/I /:: cmtrol, -"t 10/ 1:9 control,-OxtIO/I Tox 1415-RTS-90R22O3234M. .yi, cmtrol,-OxtlG/19/99 TO 5-RBS1 M.'OXH Blank TOX145-RTS- 9-250ppb-1, RWW 3235M Da cc mtr.l,-Oxtlo/19/99 TOX 1:5 -RTs -:'1R1.o00 3236H , Do yY4&4:, c mtr.l,-"tlO/19/99 TTOoXx -RTS-9.3231, TOX145 -RTS- 3238M Day Day" tlol:-.Xtlo/199/:9 mtrol -extl0/1 / 9 -RTS-9RO3239M, Day&, control,-OxtlO/19/99 TOX145-RBS10229-250ppb-1, RWW M.OH Blank TOXI S-RTS-9RO3245M, Dayl, TO 1:1-. -:RI'324&.:11 Yi, TOX 5-RTS- R032 7M D: : TOXX145-RT S -9R03244:K Dayl, 5mg/kg, 55..q"/kkgg: 5mg/kg, extIO/1 /99 :Xtlo/l:/:99 9/ tlo/l oxtlO/19/99 TOX1@45"-_R.TSS-lS9RO.322 : Tx 29-210-,,pDb.-Y1@,' RW5'.';i/"@' ..tl./19'99 M.OH 951-k TOXI -RTS-9R03250M, Day#, Sq/kg, XtIO/l /99 Tax 5-RTS-9RO3251m, Day4, 5sglkg, extlO/1:/99 rox,1: S-RTS-9RO3252M. Day4, Sag/kg, *xtIO/190 /99 TOXI1&,S-RTS-9RO3254-IN, Day&, 5mg/kg, *xt 1 /19/99 TO S-RTS-9RO3254-2M, Day4, 5ng/lcg, ext 10/19/99 TOXX145-RSSIOZ29-250ppb-1, ItW M.OH B5 lmlc TOXI145 -RTL-:RR032547-M: Dayl, Sag/kg, xt 10113/: TOX -RTL- 032 3-H Day4, 5mg/kg, ext 10/13/ TOKI&S-RBS10229-250ppb-1, RWW M.0 H,$Blank TOXI145 -RBS1100229-HZO Blk-1, RWW TOX 1 RBS 1 229-Ser= IBlk-1, AWW TOX 4,5 - RBS 1 0229-lppk>- , AW TOX s -RBS 0229-Sppb-1, Rifw TOX, 45--RBS10229-10ppb-1, RWW 11 45-Rg 1022:-25ppb-l RW TToOyX' 45-RBS1022 -$Oppb-1: RWW TOX145-RBSIOZ29-100ppb- 1 Rhv TOX145-RBS10229-250ppb- RW TOX11445-RDS 229-500ppb-I Pjiw TOX S-RBS@100229-7SOppb-1: RWW TOX145-RBS10229-1000ppb-1, RW Std C- 1.00 1.00 1@.-.0o0 1.00 1.00 1.00 1.00 1.00 1.00 1.0. 1.00 1.00 1.00 1.00 1.00 1.00 11.:0101 1 .00 I1.00000 10 1.00 1 00 PT 33 :.:05 6*815 6.902 6.795 6.808 .004 :.Bio 6.804 6.811 6.805 6.800 6.901 6.604 6.806 6.808 ::7199. 7 :.8713 .1949 6:805 6.812 6.810 '6.802 6-:.0: :-827 :::.O1 l 6.804 :::104" 6.812 6.800 5 :-:o 6 *9144 6*790B9 (.:So5 6.8 6.8200 6.802 6.791 6.766 :.:Go a01 6 78050 6 802 6 6 .::.0O5l 19 6.8.01 6. 6.eO4 :.:007 .7 nc@ usej, LA A@ C- 20 31 178594 179068 34&59 le2303 207191 207507 199555 192001 179742 158632 159083 155316 Ill 249174 230809 225733 233026 224963 1796178 33 2045 Z105290 2016766 191867 1J.7,7017 $5134 9 121:01 2056263 197 8 174315 175461 185134 231 6 Oil 11 645230 199874 19783:28 2 1:1776 131 259082 299726 208571 152 203 27 205 0 4030789 2011546 222:580 231,1 230 2299:3 204 0911 lose 1785314, 1 461 .(Fpt)Yi-9o 00 bb 0:00 bb 1.00 bb 1.00 bb 0.19 mm 1.02 bb 1.16 bb 1.16 bb 1.11 bb 1.07 bb 1.00 bb 0.89 bb 0.89 bb 0.87 bb 0.00 bb 1.39 bb 1.33 bb 1.26 bb 1.30 bb 1.26 bb 1.00 bb 00 bb 01.14 bb 1.18 bb 1.13 bb 1.07 bb 0.99 bb 0-9010 bb bb 1 23 bb 1:.115 bb 1 0 bb 0.97 bb 0.98 bb 1.03 bb 0.00 bb 0.92 bb 0.92 bb 1.12 bb 1.10 bb 1.02 bb 1 02 bb : bb 00 01.15 bb 1.61 7 bb 1. 006 bb 0. bd 1.13 bb 1.15 bb 0.23 bb 1.12 bb 1.24 bb 1.29 bb 1.29 bb 1.284 bb 1 1 bb 1:04 bb 2.03 bb 0.98 bb *D-100 -100 -0 -0 -91 2 16 16 11 7 0 -11 -11 -13 -100 39 33 26 30 26 0 -100 14 18 13 7 -1 2 lo-o 23 15 10 -3 -2 _103 -0 12 10 2 2 -100 45 617 _10 6 0 13 is -77 12 24 299 z 28& I 3 -2 P." 3 Davey 070799: q@t4t&tod wW pr=tad by mehIO/29/99 Q@Lify Colibr&tX@ AMPOrt Tax 145: Pat S=a and U@, Day I t-4 Compound I name:POAA (func1) CoefficienotfDetermination0:.995226 Calibratiocnurve:234.909* x + 12236.1 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:J/x,Axis uuw: None 3.75e5- T. /e4@5 Response-- x 0.0 O@ 200.0 Davey 070799: q@Utated wA p@ted by mehLO/28/99 400.0 600.0 800.0 Conc ak@tify C"ibc&@= RIV=T T@ 145: Mt S@& and LL@, Day I & 4 Compound 2 name: 980 (func2) CoefficienotfDetermination0:.996332 Calibratiocnurve:16.6556* x + 7.74822 Responsetype:ExternalStd,Area Curvetype:Linear,OriginE:xclude,Weighting:I/x,A-xis=w: None 1.63e4- IP.g. 2 Response- 0.0 200.0 Davwy 070799: q@"t&tAd @d pr=t" by wohlO/28/99 400.0 600.0 Conc 800.@. .. .. . . Ou@t.ify Calxbra"m st"@t T@ 145: A&t 3@& and L@-, Dy I A 4 Compound 3 name:surr(func3) Response Factor:179082 Response type:ExternalStd,Area Curve type:RF 2.32e5x x x x x x x x x Response7- x x n- 0 1 Conc 1 0.0 0.1 0.2 --0.3 0.4 0.5 .6 0.7 0.8 0.9 .0 Davey 070799: q@Litated and printed by mhlO/26/99 Method Report Method file: L@t modified: Compound: Printed: C:\MASSLyXX\Dav*yC70799.pRO\MethDS\102799b.odb Th@ Oct 28 oe:57:139299 1: PO)LA(t=c 1) Thu Oct 28 12:41:03 1999 Compound N Internal Ref.: Q.-tify T@ac.: C@c. of Standards: U :@ RF Value: U: r peak Factor: Int,grat* Wind@ Factor: Chr-tog@- mass -ind-: POAA (f=. 1) [None] TIC cmc. A 1.000000, Dis@bld 1.000000 2.000 1.0000D. R.t:.t Tim* (niR.1 tiivo.nRetention Time RT Ref r.nc.: Time Wind@ l@i@) Peak Selection: 6.042, Inabld 0.000,Disbld lxm.) 0.414 p ....t Reap-s. Type: Response: xArte"rn.1 Polynomial Type: Point f Origin: Fit Weighting: AXi3 Tr@sfo@tim: Linear Rxclude 1/X U-0 Unit.: P..k-t@p"k amplitude: 492 S@ thing: Wi.d- 1..(scNumber3of --ths: S@thing method: Di.@bld SavitzkY GolaY Join valley threshold: Reduce peak t&ilinqt Raise baseline @im=: 5.00 $O.GC 10.00 Draw vertical threshold: Do tact shoulders: Shoulder threshold: 25.00 Disabled 5.00 Relative height: Absolut* height; R. ti@* ...&: Abs1olute area: 1.50, Disbid 0.00, Disbld 2.00, Enabled 0.00, Disabled M*thod Report thod file*. HLe..t odifid: Cmpound: Printed: C:NKASSLYNX\D&VGY070799.PRO\MethDB\102799b.adb Thu oct 28 08:57:32 1999 2: 980 @f-c 2@ Thu Oct 28 12:41:03 1999 Compound Name: Internal Ref.: Ou"tify Trace: Conc. of Standards: U..r FLFValue: User Peak Factor: Integrate Window Factor: Chrmatogr@ mass wind@: 990 (fmc 2) ["me) TIC Cmc. A 1.000000, L.000000 2.000 1.00000. Disabled Retention TiA* (mi@ J: Relative Retention Ti" RT Reference: Time Wind- tain3): Peak Selection: 7.620, 0.000, INM.L 0.359 L.@bid Di@.bld R.@po.. Type: Response: Polynomial Type; Point of Origin; Fit Weighting: Axis Tr@sfo@tion: u.it.: P..k-to-p.ak mplitd.: Sm@thing: Window size Ise@ ): Number of s@ths: So@thing @thod: Join valley threshold-. Reduce peak tailing: Raise b...li..-i@: Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative Absolute Relative Ab30lUtG height: height: area: area: Lin..r Kxclude I/X 444 Di.&bld I 1 S@itzicy Golay 5.00 50.00 10.00 25.00 Di@@bld 5.00 1.50, Disabled 0.00, Di.&bld 2.00, Lnbld 0.00, Di@.bld Page 2 Method R*port I method file: L@t modified: C:\MASSLYNX\DavoyO7O799.pRO\MathDB\102799b.odb Thu Oct 28 09*57:32 1999 Cmpound: 3: surr (f@c 3) Printed: Thu oct 28 12:41:03 1999 Compound Name: Internal R.f.: Quantify Trace: Conc. of Standards: U..r P.FV-lue: Us*r Peak Factor: Integrate WirLd@ Factor: Chr@togr- -3 window: 2ur@ (f=c 3) (No..) TIC Fixed 1.000000, 1.000000 2.000 1.0000DA Dis@bld Retention Time (mi"A): Relative Retention TiAT Reference: Time Wid- Iiw): Peak Selection: 6.820, 0.000, (Nm.l 0.265 En@bld Di.@bld P.@r..t Response Type: R.3pmse: llxternal Are- Polynomial TYP*: Point of Origin: Fit weighting: Axis Transformation: Lin..r txcld. 1/K N-. units: P..k-t@p-k aplitd.: Sm@thing; Wind- iZ- (--- ): Number of smooths: smoothing method: Join valley threshold: Reduce peak tailing: Raise -imm: Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative area: ALb..Iuta.... 629 Di.@bld 1 I S@itzky Golay 5.00 50.00 10.00 25.00 Di3.bld 5.00 1.50, Dis@bld 0.00, Disabled 2.00, LA@bl-d 0.00,Di@.bld page 3 DAVEY 070799: FACT Equipment Log 99077 QuattroUltima:#9261QB PAGE DATE: 10127/99 ANALYST-.mmh STUDY NUNMERLIox 145:Matrix:Rat Sera& LiverDESCRHMON.- _PQAA& 980 FACT Method:E7S 8-5.1& 8-7.0 Injectiovnolume:5 uL Cycletime:10min. Electrodc:_Z-$Rray_ MobiJe Phase: (A)2_0mM NH4CH3 02 TN-A- orstadrdnumber (A) 99085-11-3 Prepared(date/by): (A)10/23/9s9ah -- (B)MEOH (B)tn-a-2945 (B)10/23/9s9ah Expires: (A0)4/00_ (B0)4/00_ Storeatroom temp? E or N Other Guard column: None Partnumber:na Lot number:na AnalyticaclollimnK:eystoneBetasil Size:2 x 50 mm - Partnumber:055-701-2 Type:C18 Lot number:P9El I Spheresize:5 um Serianlumber:0591825Z Analyticaplarameters: Dryinggas(LJhr)4:97 ESI nebulizinggas(LJhr)-10 LC Flowrate3:00ulJmirL Back press=: 82 bar Sheathgaspk) HPLC solventgradient:10min-10-95 Time(mirl) O/oB 1)0.00 10.0 2)1.00 10.0 3)5.50 95.0 47.50 95.0 5)8.00 10.0 Tuning Method Report Method: C.\M&sSLyNx\DAvEy BAMWP AUG99\DAVEY-RATS.PRO\ACQUDB\Pros-4 Printed: Wed Oct 27 14:31:21 1999 Page 1 SOURCE ESP- Capillary(kV) Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set 3.15 10 o.0 0.0 0.0 150 250 Pdbk -3.07 -11 148 249 Pressures Analyser Vacuum Gas Cell Rdbk OFF 4.3e-3 Analyzer LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas rlows Cone Gas Desolvation Set Rdbk 14.5 14.5 1.0 -2 2 1 12.0 12.0 1.0 650 -3 2 0 -646 Px%k 57.8 484.8 s..nr,.V Mthod Rp-t Method: C:\WAssLyVr\D&VLY070799.VAO\AMUDB\lCKM-POM-990-IS L-t b6.Lif@.d: Wed Got 27 14:18:01 1999 P.=t.d: W" Oct 27 14:32:05 1999 X.1-t D.Iy - ) . 0.00 r-ti- : 1 bm ,EI bh-.rir ( zn- Inter Ch@nol Delay SW ( D.It-. ) : start Tim* ( )Lins End Ti.. ( Kin. Sacs 0.03 0.00 0.00 10.00 R.P.AtL: 1 @el parent Daughter Dwell (Sacs) Coll Energy (.V) C@- V 1 413.00 169.00 0.30 30 is r-ti- : 2 bw Of I buss p@ ( En- Inter Channel Delay t Sacs 0.03 sp" ( Dalt@ ) : 0.00 Start Time ( Kin3 0.00 Ed Ties Ki- 10.00 Repeats 1 Ch@el Parent Daughter Dwell (S@s) Coll Energy (-V) r@& V 1 980.00 79.00 0.30 60 so F@t.L- : 3 bm f I N-. Pat. rjp- Inter Ch@n*l Delay Sec3 0.03 sp@ ( oait@ ) ; Start Ti@ ( Hi@ End Ti" Kin. 0.00 0.00 10.00 Repeats I Ch@el Parent Daughter Dwell (sacs) Coll Energy I*V) CM* V 1 427.00 00.00 0.30 40 60 Method Report Method File: Last modified: Printed: -7 Page I C:\MASSLYNX\DAVEY070799.PRO\ACQUDB\10min Wednesday, October 27, 1999 14:25:05 Wednesday, October 27, 1999 14:25:31 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Oven Temperature Right(OC) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are Time A% B% C% D% 0.00 90.0 10.0 0.0 0.0 1.00 90.0 10.0 0.0 0.0 5.50 5.0 95.0 0.0 0.0 7.50 5.0 95.0 0.0 0.0 8.00 90.0 10.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are Time Initial 0.00 0.10 Column Switch Off Off Off Contacti Off On Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (ul/min) Draw Position (mm) Stop Time (mins) Injection Volume(ul) Vial Number 200.0 200 0.00 9.00 10.0 12 Masslynx - Sample List Sample ListC::\MASSLYNX\DaveyO7O799.PRO\SampleDB\102799b.SPL Printed:Wed Oct 27 14:34:051999 FileName FileText 1 102799013 MEOH Blank 2 102799014 MEOH Blank 3 102799015 TOX145-RBS10229-H20 Bik-1,RWW 4 102799016 TOX145-RBS10229-Serum Sik-1,RWW 5 102799017 TOX145-RBS10229-lppt@-1, RWW 6 102799018 TOX145-RBS10229-5ppb-1, RVVW 7 102799019 TOX145-RBS10229-10ppb-1, RWW 8 102799020 TOX145-RBS10229-25ppb-1, RWW 9 102799021 TOX145-RBS10229-50ppb-1, RWW 10 1OZ799022 TOX145-RBS10229-100ppb-1, RWW 11 102799023 TOX145-RBS10229-250ppb-1. RWW 12 102799024 TOX145-RBS10229-500ppb-1, RWW 13 102799025 TOX145-RBS10229-750ppb-1, R. WW 14 102799026 TOX145-RBS10229-1000ppb-I RWW 15 102799027 MEOH Blank 16 10279902B TOX141--RTS-gRO3230M, Dayl, control,-extlC/19/99 17 102799029 TOX145-RTS-9RO3231M, Dayl, control,-extlO/19/99 18 102799030 TOX145-RTS-gRO3232M, Dayl, control,-extIO/19/99 19 102799031 TOX145-RTS-9RO3233M, Dayl, control.-extlO/1-9/99 20 102799032 TOX145-RTS-gRO3234M, Dayl, control,-e)dlO/19/99 21 102799033 TOX145-RBS10229-250ppb-1, RWW 22 102799034 MEOH Blank 23 102799035 TOX145-RTS-9RO3235M, Day4, control.-extlO/19/99 24 102799036 TOX145-RTS-9RO3236M, Day4, control-,extl0/19/99 25 102799037 TOX145-RTS_9RO3237M, Day4, control,-extlD/19/99 26 102799038 TOX145-RTS-9RO3238M, Day4, control,-extlO/19/99 27 102799039 TOX145-RTS-9RO3239M, Day4. control,-extlO/19/99 28 102799040 TOX145-RBS10229-250ppb-1, RVWV 29 102799(Al MEOH Blank 30 102799042 TOX145-RTS-9RO3245M, Dayl, 5mgtkg. D50-extlQ/19/99 31 102799043 TOX145-RTS-gRO3246M, Dayl, 5mgtkg, D50-extlO/19/99 32 102799044 TOX145-RTS-9RO3247M, Dayl, 5mgtkg, D50-extIO/19/99 33 102799045 TOX145-RTS-9RO3248M, Dayl, 5mgtkg, DSO-extIO/19/99 34 102799046 TOX145-RTS-gRO3249M, Dayl, 5mgfkg, D50-extlo/lgt99 35 102799047 TOX145-RBS10229-250ppb-1, RWW 36 102799048 MEOH Blank 37 102799049 TOX145-RTS-gRO3250M, Day4,5mgfkg. extIO/19/99 38 102799050 TOX145-RTS-9RO3251M, Day4,5mgfkg, extlO/19/99 39 102799051 TOX145-RTS-9RO3252M, Day4.5mg/kg, extiOlig/99 40 102799052 TOX145-RTS-gRO3254-IM, Day4,5mgtkg, ext 10/19/99 41 102799053 TOX1 45-RTS-9RO3254-2M, Day4, 5mglkg, ext 10/19/99 42 102799054 TOX145-RBS10229-250ppb-1, RWW 43 102799055 MEOH Blank 44 102799056 TOX145-RTL-gRO3247-M, Dayl, 5mo/kg, ext 10/13/99 45 102799057 TOX145-RTL-gRO3253-M, Day4, 5mgtkg, ext 10/13/99 46 102799058 TOX145-RBS10229-250ppb-1, RWW 47 102799059 MEOH Blank 48 102799WO TOX145-RBS10229-FI20 Blk-1,RWW 49 102799061 TOX145-RBS10229-Serum Sik-1,RWW 50 102799062 TOX145-RBS10229-lppb-1, RWW 51 102799063 TOX145-RBS10229-5ppb-1, RWW 52 102799064 TOX145-RBS10220,10ppb-1, RWW 53 102799065 TOX145-RBS10229-25ppb-1, RWW 54 102799066 TOX145-RBS10229-50ppb-1, RWW 55 102799067 TOX145-RBS10229-100ppb-1, RWW 56 102799068 TOX145-RBS10229-250ppb-1, RWW 57 102799069 TOX145-RBS10220-500ppb-1, RWW 58 102799070 TOX145-RBS10229-750ppb-1, RWW Page 1 Page Position(:1,1) Masslynx -Sample List Sample Ust:C:\MASSLYNXDaveyO7O7gg.PRO@SampleDB\102799b.SPL PrintedW:ed Oct 27 14:34:051999 Page 2 Page Position(:2,1) MS File InletFile Bottio InjectVolume Sample Type Cone A 1 IOMIN-POAA-ND-IS 10mir@-ID-95f 91 2 IOMIN-POAA-98D-IS 10min-10-95f 91 3 10MIN-POAA-980-IS 10min-ID-95t 1 4 10MIN-POAA-980-IS 10min-10-95f 2 5 10MIN-POAA-98D-IS 10min-lD-95f 3 6 IOMIN-POAA-98D-IS 10min-10-95f 3 7 IOMIN-POAA-98D-IS 10min-ID-95f 4 8 IOMIN-POAAgBD4S 10min-10-95f 5 9 IOMIN-POAA-98D-IS 10min-10-95f 6 10 10MIN-POAA-980-IS 10min-10-95t 7 11 10MIN-POAA-98D4S 10min-lD-95f 8 12 10MIN-POAA-WO-IS 10min-lD-95f 9 13 IOMIN-POAA-9804S 10min-lD-95f 10 14 IOMIN-POAA-9180Dmi4n-S10-95f 11 15 10MIN-POAA-980-IS 10min-10-95f 92 16 10MIN-POAA-9804S 10min-lD-95f 12 17 10MIN-POAA-98D4S 10min-10-95f 13 18 IOMIN-POAA-98D4S 10min-lD-95f 14 19 10MIN-POAA-9804S 10min-10-95f 15 20 10MIN-POAA-9804S 10min-lD-95f 16 21 IOMIN-POAA-980-IS 10mir@-10-95f 8 22 10MIN-POAA-980-IS 10min-10-95f 92 23 10MIN-POAA-980-IS 10min-10-95f 17 24 IOMIN-POAA-980-IS 10min-ID-95f 18 25 10MIN-POAA-9804S 10min-lD-95f 19 26 10MIN-POAA-98D-IS 10min-10-95f 20 27 10MIN-POAA-980-IS 10min-lD-95f 21 28 IOMIN-POAA-98D-IS 10min-ID-95f 8 29 10MIN-POAA-98D-IS 10min-10-95f 93 30 IOMIN-POAA-98D-IS 10min-lD-95f 22 31 10MIN-POAA-98G4S 10min-10-95f 23 32 10MIN-POAA-98D-IS 10mir@-lD-95f 24 33 10MIN-POAA-980-IS 10min-lD-95f 25 34 IOMIN-POAA-980-IS 10mir@-10-95f 26 35 10MIN-POAA-980-IS 10min-10-95f 8 36 10MIN-POAA-980-IS 10min-ID-95f 93 37 10MIN-POAA-980-IS 10mir@-lD-95f 27 38 IOMIN-POAA-980-IS 10min-10-95f 28 39 IOMIN-POAA,98D4S 10min-lD-95f 29 40 10MIN-POAA-980-IS 10min-10-95f 30 41 IOMIN-POAA-9804S 10min-ID-95f 31 42 10MIN-POAA,98D-IS 10min-lD-95f 8 43 IOMIN-POAA-980-IS 10mir,10-95f 94 44 IOMIN-POAA-9804S 10min-10-95f 41 45 10MIN-POAA-980-IS 10min-lD-95f 42 48 10MIN-POAA-9810Dm-inI-lSD-95f 8 47 IOMIN-POAA-980-IS 10min-10-95f 94 48 10MIN-POAA-980-IS 10min-lD-95f 1 49 10MIN-POAA-980-IS 10min-lD-95f 2 50 10MIN-POAA-980-IS 10min-10-95f 3 51 10MIN-POAA,9804S 10min-lD-95f 3 52 10MIN-POAA-980-IS 10min-ID-95f 4 53 IOMIN-POAA-980-IS 10min-10-95f 5 64 10MIN-POAA-980-IS 10min-10-95f 6 55 IOMIN-POAA-980-IS 10min-10-95f 7 56 10MIN-POAA,980-IS 10min-10-95f 8 57 10MIN-POAA-980-IS 10min-lD-95f 9 58 IOMIN-POAA-980-IS 10min-10-95f 10 10 - - 10 - - 10 - - 10 - - 2 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 ac 10 - - 10 - - 10 - - 10 - - 10 - - 10 - - 10 QC - 10 - - 10 - 10 - 10 QC 10 - - 10 - - 10 - - 2 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - 10 Standard - Masslynx -Sample List Sample Ust*C:\tAASSLYNXNDaveyO7O7g9.PROZampleDB\102799b.SPL Pdnted:Wed Oct 27 14:34:051999 FileName FileText 59 102799071 TOX145-RBS10229-1000ppb-1. RVM Page 4 Page Positon:(1,2) .......... Masslynx - Sample List Sample Ust: C:\MAssLYNXOaveYO7079g.PRO\SampleDB\1027@9b.SPL Printed:Wed Oct 27 14:34:05 1999 Page 5 Page Positon:(2,2) MS File InletFile Bottle lnjadvolume SampleType ConcA 59 10MIN-POAA-980-IS lomin-10-95f 11 10 Standard Daic Data Analyst: AS FACT: DA'I'AREV'IEW SULNINIARY FOPNI Data Review Sign-Off An slystReview Name/ Date: :7-Al IL@L 1-2 LAC- FACT Study tv.5- tvfatnx/Timepoints:?", -k"zf Wo-@, SampleLisL- Set-upAMysis Date/Analyst Instrument --rA 6 -'w, ozo/ff e.-I Technical Review *ell Name I Date: v- QualityAmmrance Review Name IDate: Date Zntrr. oc, o-s Comimats IJustLikatioiLs: Analyft: ?OAA ecw I L4&,KW_ AlaS AA@ A=tpubio Lmm Rangc AIA LOQ. IIA EzMm:tim Bknlc. 4/A R^2: CalibrationChecks: AIA t,r*r @6 NL%INM- AJA ,DataSwo: mA NistriBxWk LAC illogli@ 0 lb, le,-l AAS AC41 Analyte: AcceptaWe Lineu Rmgc- LOQ: ExtractedBknic /&,I lkgc zo, R^2: Mabix BW& /t,15-A4,q/0,2 CalibratioCnheckL MSIMSD.-- L/ t@K - cr@L VCILL a@ 49'/ i@.1W1' iDetaSw= dol_@ea tcrnc,14@hj&A 1*10 a;@", ? (Ac. Li.aA;,l leztlsIli L/ P'AOwe a4P iiii-@ -&e Analyte: ocA "L .3) AcceptableLinearRange. @F3,4pi LOQ: R^2: 17.9? Extracted Blani-- lez IL, Iv Mti, Bink-- /e:rs 7@L, Zd,,? r.Oibmtion Checks- MSIMSD: [Data Satus: L.,tie L/ Dk E,," Lkc, itioslag 0035 FACT: DA'I'ARE'VIEW SUININIARY FOPNI IAC, Data ReviewSign-Off Data Analyst: Analyst Review Name / Date; .7)RS 5-11@ FACT Study 0: '7,,- MatrixITimepoints: Sample List- Set-upArW* DatdArWyst L, Enstrumcnt Technical Review N,,. /Daw. @e, QuaHtyAnumace Review Name /Dec: Data Intrr. LAc- ii1aliq Conunents Justifications: Analyft: (,--AVf) Ac--pb" T@n-, IL&W AIA LOQ. VA RA2: IVA Cahbration ChwJ= IVA MS%CM)... DatiLSt-hiv NA A)A Exbwdon Blank Matrix Bluk oV* Anslyte: Ac=pUble LinearPmgc LOQ: R^2: CalibratioCnhecks: M&IMSD, DittaSw= E-d=tcd BWiJc @Z Matrix Blan AC Acolyte: AcceptableLinearR..L@/ LOQ: R^2: qaMa&lli,bbm / hecks: M& m D*D--.. h ta Satur Exuutcd B4& Matrix Bta@ 0%@tify T=45-rat C=.Pound *@m@y TAP@ &or&, day 21 d@@ End @t=l- @- 11/3/tl N= Sam,* List: ..-@ Obditid@ aX-mtthad:."flodi Job C044: c: %MASLT=%00uvo2oltg:o.PI.0%840plam%llo4sla Fri @ 05 09.30: C; %M"XLT=%Noupo2ol".Dro%"lfttbm%1104"a Fri u- 05 09.29,44 191, Printed: Fri ift, 03 04:32:31 1911 C=.Va-4 1: POAA (Chi) u- ,Go, 2 1104 3 1104"99002 , 111100,9 9003 5 0":004 11 005 6 110499006 7 110499007 a 110499008 9 llod99009 10 1104,9010 11 110499011 12 110499012 13 110499013 1& 11049901, is 1104,9015 16 110419016 17 110499017 la 110499018 19 110499019 20 110499020 21 110499021 22 110419022 23 110419023 24 110499024 25 110499025 26 110499026 27 110499027 28 110499028 29 110499029 30 110499030 31 110499031 32 110499032 33 110499033 34 110499034 35 110499035 36 110499036 37 210499037 38 110499038 39 110499039 10 110499040 41 110499041 42 110499042 43 110499043 44 11049904, 45 110499045 46 110499046 S-01 :list T@ M.OH 1&.k X.09 Blank X.On Asal&.k TO 5 -RZSII03:-H2o Zlk-9 11/3//19,nm TCZXI1 -RRS1103 -Se.a Blk- 9. -t, . 21/3 :, MM ?OX145-,RTS11039-S@,a Blk- 7,,0OXI 4 5 -RBS11030 9- S1ppb-9, ext 11/3 um 11/3/19 MM ?CX14 -R&Sll 3 - Oppb-9: ext. 11/3/:9 )Wx MX145-,RBS1103:-25ppb-9 -t. 11/3/ 9, MCK MXI 4 5-RSS1103 ,-S*ppb- 11/3/9:gNCH Xl S-RRS1103 -100ppb9i. , 11/3 MCH TOX145-RDS1103111-023590_pSpobo-ppbTC)Xl4S-RILS 9. . 11/3 9. wm . 11/3/'19,9 mWcHm 7OXIIS-RSSIIO)9-750ppb- -c 11/3 BM 7UX145-RJLS11031-1000ppb-9. 11/3/99 UM X.OH Blank AS 'MX1 45 -RTS1103:-2,50ppb-KSI. &Wt. 11/3/99 WR TOn ?TDOXI 45 -RTS110 't3 ;24 0OMp_pob-KSD10, -RTS-9 03 45-RTS-IR0324IM-0 -1).y 21, "t. ext. 11/3/99 MCH 11/3/9,9 MCH 11/3/ mm Xl 45-RTS-IR03242M-O -D. 2 :. : axt. 1 11/3/ :9 9 WH TOX1 -Day TOX245-RBSII039-350ppb-ccvg y wm. 1/3/9 9 mm Blank N*og 45-RTs-9RO1243N-O-My0_ 2 11/3/ 99 =3 T"Xl 45-RTS-9RO3243M7"y,l45-XTS-IU32SIn- y sSaMg,0/ ko-D. 299: WM. 11//3/:99 UM 7VY*145-RTS-IR032$GM- kg-Dy2 11 3/ wo Ton 45-RTS-gRO1257K-Sg/kg-Day2 y 9, - - /3/99 MM T'DXI 45-RILS11039-25*ppb-CCVIO. "t. "t11'/3/I9'9l um TN.aOlHl &lank TO 45-RTS-tRO325$M-Sm/kSgm-lDkagy_2D:a:y2 RTS-gRo 59"- TOndS- 32 11/3/99 ICH 11/3/1 NCH 7UnXl 15-RXSI1039-250ppb-CCVI. H.Ou Blank @. 11/3/tl UM 9 71OX145-RSS1103:-320 Blk-9. -t. 11/3/1:,Jir-H TOXI:S-RBSIIO 3 -Sera glk-9. ext. 11/3/ 9, WR TOXI ,S-RTS110313-,S-a Blk-9. art. 11/3/ NCR TCXL .M S-RDS110 - Svpb-I 11/3/9 n4S-RILSIIOII-Ioppb - 9. . 11/3/tgg MCH TMCX145-RRS11039-2,ppb- -t 11/3 MCH Ton454:5RB511,0,3:-50ppb-9,,@..11/3/99,NM Mxl Rasil 3 -10 Oppb-:. ext@ 11/3/9@) MR MX245-5RSS1103:0-250ppb0-9, -t. 11/3/9g) MCH :RBS11039-50 Oppppb- TTIOOXxXI1 445 RILSII 3 - 75 ppb-9 145-RILS11039-1000 b- 11/3/ mm 11/3/9 /:,WH 11/3 MCH t"- :ttan"rd S,.A.d-.d.d Standard Stndrd st S5 tandard t..d&rd Standard oc oc oc Sstandard 5@t_.@..@dd-d Stand d Stnd&@d Standard r Stands Standard d stad@rd Std C@ itT 1.0000 1.0(, 1.00 1.00 1. 00 I. 1.000 I.0 0 1. 0 1.00 7.0:7 7.010 3 7. 2 7.128 a 7 128 7:121 7.112 7 . 11 1 7 is 7.127 7.113 7.090 7.111 7.01633 7. 7 12 1 7 :. 1&: 7 132 @..Oo 7.1530 7.1 5 4 7.1 1 7.135 7:102'1 7 1.00 1.000 1. a 0 1. 000 1.00 1.00 1, 00 1* 00 1.00 7.08: 7.106 7.127 7.13' 7.117 7.131 7.1057 7.1 a 0 7.0(,s 7.115 7. 7.11311 1 7..11306 A@ no. 1012 bb 1 5 bb 4 bb 1 & mm as bb 3 MM 73 bb 7,3 bb s bb 82 a UK I bb @(13 bb 5441 MN 71 bb 57 bb 55 bb 43 MNNK 54 bk. 5 1: bk) 113 bb :3 NK 1 bb 13 2 NK 2 bb 49 bb bb :@0 46 MNMK 36 bb 39 mm AS bb 47 UK 50 bb 5S2 NK 709 bxmb 2M 0-. %D- I 1 :.3467' 17 1 .3 7 37 64 36 11..2 2@ 2.' I1.07 7 1.096 -56 a5 1 19 19 1-18. 23 .5 5 00 -:2 1 0,4 -.1.1 -3 A 00::2 0.630 -18 -207 -3 00.785 -22 .:2 -"S 1:65 1.36 636 1-:: -11 1-,1629 0. 1.31 0.7: 0.652 a. 17 0.'65 0.5793 0. 75 o0. 86 I:03 1.34 :3 _3 2 1 31 24 32 40 -35 -31 -27 -2S -l' 34 gmp 020111: gu=tit&tod and pltd by i_ 11/03/,, CP@tity Compound 8%00m&" mov@ T=43-rat sera, "y 29 do- -4 Oat=l- -t. 11/3129 N= samole List; L@t modifiadt lmtb.d: L-t ."fld: Job cc": Fri lWw C: rri a- 05 06:30tlg OS 06,29.64 1999 1999 P'L.t.d: Fi m@ 03 of..s2.31toog Cmpow@d 2: RPOS al@99001 1101,1'..@ 3 499003 1100499004 5 0499005 6 11 0499006 7 110499007 9a 11 0499008 499009 10 I10 499010 11 110 499011 12 110 499012 13 110 499013 It I100499014 is 1'0499015 16 11 0499016 17 11 o@L99017 Is 121,0499018 19 11049"9a019 4 20 201 111100499021 22 11049:022 23 11049 023 110 , 24 0:9900245 25 11 9 2 26 110199026 27 11004&99:002278 289 11 20 110:9 9g 029 1 11 030 31 1100199031 32 1104A9 9033 2 33 11 0&999003,3 34 11 35 110499035 36 110:9990036 37 110 9 37 389 110449903:3 40 111100499990040 41 110499041 42 1049,9042 3 43 1 4445 110419:0044 1104,9045 46 110499046 (CIL2) sami:il..t Test )toox P-0 H .I1-Okk .. .1-k TOX145 -9 TIOX1455 -RRIaLSSI1l10033:-gS2ooraSISkIk-;, 'MX14 5 -ItTS1103$-S*ra Blk-9. 71OX14 tio3 sppb-s -t. =XlAS-R-mRl" 103 :-I0ppb- @t TOXI&S-MS11039.-2,5-pp.b-I , wm. ..11/319:9NCH 1 3/9, orH 111 3/ mm 11/3/'9999 MM 1113 mm 11/3/ T.o.=4dS -RILS3,0139-S 0vol@, :9,@t. 111113/;: MUM= -VZSII0 3 -1 Oppb- /3/99 ICE T7OOXX1I1'5S-KILSII 39-250ppb-9. 39-500ppb-9. 1213/99 UM 11/3/:9 MC7A -KILSI10 TOX145 -MUI103::75OPPb-9;. "t.. 1/3/,9,,MM TKOOXO1H45a-la-mkila 39_2l5ooovpb- = .U/3 om TIOXI,S_ Cvpb-mSg, 5 wm 11/3/99 WR TOX245-KRTTSV1I1l0o393-2 Oypb-KSUIO. OM. 1113/99 NCZ 7=15-,rrS:;10R3a240*-O-Dy 2:: 21/3,/:99 UM Taxi S-RTS- 32&IX- O-Day 2 =: 11/1 um T01115-ItTS 9RO32 42X-O-Day 29, M. 11/3/:9 am TOX115-RZS11039-250ppb--CCV9. @t. 21/3/9 MM MOOK 45DI&AX 5 -RTS-:RO3243*-D:aD.Y 7UXI TTOO==45-RT-SM--gRO3R20S35M2_4S3mX/-kg "ay TOXIAS-RTS-9RO3256M-5.g/kg TOX145-R?5-9RO3257N-Sm/kg 2:: 11/3/:99 MM 2 .t. 11/3/ mm 1113111 1 -Dy29 _ZDaMyY2 . -t. 11/3,919KM 2 .om. ii/lu/mItum TOX1 5 -RILS11039-25OVpb-CCVIQ. M.OH4 al@.k TOX1445-RTS-:,RtO3o2559N-Smikg-Dy2_9.y2 TOXI S-RTS- 32 9X-Sm/k TOX145 RILS11039-250ppb-CCV9. @. 1113 /19 11/l/99 WE 11/3199 MCH 11/3119 WH PTOIX.1O4H531-"k -RBsllCa 3:-920 alk-9. TOX145-RM11039-S allkk-9: TOX1 S-RTS11 a39 Sppb_g -9 11/3/99 WH 1 /1 3/9,9 WR 11/3/I'l,3l/ 9 To ToxXiII44S5--R"ISSl1l10319-10ppb-:: -_tt.. 11/3199999WWRR TOXI S-RBS11039-92 Sppk@ 9, wm. 11/3 f WR TIOX145-RBSI103 -Soppb- 199 WR TOX145-RILS1103:-1050vpb-9. -t. 1113/19 14CH TOX145:RILSIIOOI,-200ppb- 12/3/99 HU TOXI&S RAS11 1 -5 Oppb- 11/3/99 WH TOX145-RaSI1039-750ppk@9;.wm..11/3/19 MC3$ TOX145-RIS11039-1000ppk, *= 11/3199 INCH Type Standard t&nd@d stodrd Standard Stt..d.@d Standard Standard stva"d OC Qc oc Standard SSt,andard S.ttandard and"@rd Stan d standard t&.d..d Standard Std C@ 4.973 .1. 21 49*30 97 6.10 24.:Do 193.00 735 976.00 &.00 24 248.00 - 2418.00 1.93 9.76 24.80 49.30 97 .00 243 4"9,3..O0o0 976.00 2 $tT 7. 200 7.23 1 7.2' 7.206 7.180 7.242 7.2:7 77 7:'245 7.2550 7.2 1 7,29&1, 7:2542 7.2 7 228 7.253 7.2520 7.2 2 7.2670a 7.2 7* $a 7.22dae 9 7.-22,9@1.. 7.2 'a 7.2 7 2757 7:.21 7 .22.,l 7 7.246 7:1251 7 204 7 3 6: 7.296 7.21, 7 .3 7 .2 47 7 .2ag " .2 7 221 7.214 7.271 1 .11,9 7 .2770 A@ 3 51 261 10 78&.& 20138 5275 nas bb MbMb bIblb m bbX bb 2@. MbNb 4501 bd 1388&3 OK &2 M 172 0 bbX 193 bb 39264 bd 3637 bb 314 bmh 51 bb 4344 a39l bmb do bb 52663 bb 5'8167263 bb 11.1 bb 13 3 NK 51 :70.1a. bb 480'4L.3@ bdb 8617 bbbb 107 kh 133 bb 326 "NX 656 bb 1268 bb 24319 bb 11',17017'3bd 229-353 bdbX Ck@. %D" 0.00 00-.00 0 * 00 0:00 0.00 4.092 209:&7 48&3.5213 ---$1 -12 214.64 163730.3612 836.53 1.12 196.40 172@.14 -i93 2 9 -14 0 2060.81 -17 o: 0.00 2566.17 21859.14 320.a.&3: 12 1: 9 2 7 A 3 .3L 17.2. '9 231.197 3.59 0o: 0.00 0.00 1 3.65 -269 2 0.675 1: -6' 116 2 273 7 7 19 .1 I'l 'o sis 641 .9 1114.59 11 LA L 7. &mo 020199: 0%@titated amd winted by i@ m 1110511, Q-tLgy commpo%Lnd SUMMWLry M-P-T=45-rat or&, day 29 d... end -t-l- -t. 11/3/99 Icz sawle LLt: : c:%MUNLT=%.Guvo2olst.pro%smlplemxllo4gta L@t @odifled rri u- os 64:3o:ls lovy lfttb": c:,XL82LY=N-po2ol, v"%mthm%ilo&sl. .Ddifi.d: F@L 31@, 05 06:21.4 1 Cd.; v.int.d: pri N@ 05 09:52:31 1999 3; vro" ccw) ."9ool 2 llo499GOo2 3 4 1111,.1119:@ool 5 llo4,9oo5 67 110o419006 a 11 499007 9 llo:g:oo: 9 oo 10 llo499010 11 "0 499all 1121 1l1l0o4999loOll32 11 id o499014 IS 0499015 16 11 0499016 1I7S 1l1lo499:017 19 110 ois IIG&99029o 20 1104,902 31 llo,99o2l 22 1104:9G22 23 1104 9023 24 110499024 25 1104::0025 26 1100 6 27 11 11,90227 2: 110499:02: 2 a 110o 4 g 02 3 1 11 o 4 99 030 3 2 11 o 4 'go031 3 11 4 32 33 110499033 34 110499034 35 11049 035 36 11049 036 37 110499037 3'98o llo4:9;oo3,381o 41 19 41 42 llo499 o 42 l&@4 '11-0'6o499'19.o'1434 456 llioo499o45 110499o&6 s.m list rest M.OH 1 al@.k MX.OH :1@.k ToX H *o ,,-kll0o3:-iC Blak-9 .t. .11/3/1:gNCH wxltis-R-anssll 3 -S*o Ik-9;,, . . 111,3,9, ICII mMXx1l44$5_-RRaTSSl1l1o033g9_-SSer. alk- -t 11 3 mcm ppb-9. 11/3/99 NM TTooxl45-R]ISIIO0339-10ypb-9 ppb- TooxXi1l4s5--R"sSslllIO3:--s2o5 ppk- 9.9. ll//3/99 WH 1113319991 DICsR= Toxl45-RRS11030 :-100,pb-" I /9, ICE X14A5-RIS11 o 39 -2S Ovpb- 9. ToXl S-RILSII03 ,-50Sooppb- TGX1 S-RILS11 039:7(",ppb ToXi 5 RILSII 3 1 Oppb- &x.tt. I11//3/1 M= M /3/ ... 4= 1/3 ws M.OH Bl-..k TaOxi45-jtTSlIG31-250vpb-KS9. wm. 11/3/99 I= X145-RWI1039-2350ppb-MMIO: @=. 240m- O0-Day 29 wm. TToo- A45S -iRtTSr-s-:RR00324131 -Dy 2 70xnllS-RTS-IRD3242M--O-Day 29. WM. 21/3/:: NCR 1 /3/ NM .11/3/:9 WE 11/3/ mm WXIISS-R" 11039-250ppb-CCV9. NM.XOIAHS_ 1-k wm. 11/3/19 3KM RTS-9RO3243N-O-Dy 29, *Wt. 11/3/:: DICH TCXIAS-RTS-9RO3343.-O-Day 29, wm. 11/3/ MCH TOXI&,S-RTS-:RO3I2t,o55M- Smg,/kg-DaY 11/3/99: 3cm 7oXl S-XTS- 32 LU-MA kg-Day22,: @. 11/3/ MM 11/3/99 NM TOX1 -RBSII "39- Soppb-ccvlo, awt.@t1.1/3/9, NCR mooh Bl&Ak TTOOXxIl4,S5--RRTTSS--99:00 332255::--SSmu//kk: --DDayy2299, m. 11/3/99 mcm m. ,11/3/99 MR .Mxl,5-RBsllo3 9-250vpb-ccvtl wm: 11/3 91 wm H.CH 45BI..k To'Dxl -RDSI1039-H3O alk-9. 44 5-RBS11039-SS:r Blk-9. TOXXIl 5- tTSIIO 31- @: Slk-9, TOnA5-RRS110303: -Svpb-1. @ lmxl4s-RlLsll -10ppb-19: 1 TioXI45-RBS11039-25vpbTOX145-RBS11039o-50 vpb-9. 'Mxll,l-.1@ o 3:-1500oppb-:: T'Oxl4 5-RSSII o 39 -2 vpkl-9. 'MX1 ,S-RB'S 11 a 3 9 -Sooppk' 9. TOXI 5-RBr'11 3 -7Soppb=XIAS-RRsllO39-100oppb-9. 11/3/99 WH 11/3/99 ICH wm. 11/3/99 MCH . 11/3/99 M= 11,1319:1 11 3/9 um 11 3 9 bwx 11/31/9999 NCH 11/3/99 ICE 11/3/99 WH NcH 11/3/99 NCH 121 SStt..n.dd.-.dd Stands rd Stands d St&ad@d st&n"rd SStts.u.dd@"d d St&nd d OC OC oc St..d"d sSttta-ndd-a-rdd :taannd&ard St..dr'dd St&nd&@d Standard Stand@d otd C@ -,I sm 7. 11 7.so9 7.769 7.:7os 7. 1 7 - :.,10 29*87 44 -30D0 9 97:7 Il,l..Ol 493, ,00 7 ,00 977. 00 248. 24LB.00 7:8758 77 ..&81567 7 7::13 7 .675 7 .837 7. 305 7 .3$62 7 ..3 . 7. 0 7 oss 7.:53 7, '1 7 Sll 7 -97 7.-8B7S24 7 7:879 7 12: 7 $74 7.831 7..887301 243.00 4.93 .17 21.80 479.30 9 .70 lll..G0l 4 36,'0000 7977. 7 .836 7 ..$932 7 . 39 7 .984738 7.&76 7 7.:10a 7. 0 7. 7.:726 7. 7 7-:11 7, 3709 7* 66 9 7. 1 A- Fl". 2360 m :32,32 mom( 4.11 m 544 bb 12849 db 3 05SG db 17 252 dd 233 6322 dmb 1211 ';"31 1" 1853 64 M 2477 11 229 3o 16 611S27 6088, m 67& M '.10.07 M 585651 m 3347031 M 1277 NdXb 3m 113 dk. 553 226 M 9219 M 1875 MM 53678 'U' 360 M 221 NK 24803 xNK" db 1:229 NH 2 627I2 NK 117537 NK 249ol m 121,02 21' 1727838 N" 23Q763 mm c@ o-co ...oo o -oo o:oo 4.9o 10.6 -o 26.091 9 51.12 5 113.91 147 369.12 9 S07.43 761.56 3 9713.165 0 S 246 16 245'19 a 13 0 -000. 236:10 -5 o.oo 0.00o *..@o 1:240 1.09 222.54 -10 oo 0I.@6 21S5:'*.' 0.0 5 0.0 0 O.o o o.co 19,.@1931 22 45:213 95.8 1 242.4 5 -2 117.@ 2 -1 700.4 6 936.561 -45 P.O. 3 IAC, SOUP D2011t: Q@titated "d printed by i@ ll/OSIII Q@tigy convound am=.&" PAM@ T=45-r&t set&, "y 2% does ad oct"l- MM. 11/3/99 BM SoMis Z.Lat: L@t mo"fiod: thod: = tat@difiod: Job Co": C: rrL M" OS 06:30:10 1999 C:%N"SLTKK%o*UP020192.pm%matb=%Ilo4gsa rri M@ OS 04:29:44 1999 Printed: iri a- 05 04.52:31 1999 convowid 4: w@ lcbt) 4I X@ 9,001 SaMl:lLat T=t III Std C- RT A- c@ %D- 7.075 14 FmmI&O, 0.01 -99 2 l11i0o1,9'..@ NmNIo*OooUll 2l1a"n*k 3 110499003 4 110499004 TOXOIU&S_ &.k RASIL039-120 Blk-9. a= 11/3/99 NCR 11/3/99 UM 7.0 :5 7..91, 27657 bb 2 72 bb 1 23 23 l@29 29 1104&9:005 110 9 006 TOXI&S-RILS11039-S.m Slk-9, TOX1 4,5-M 1100 39-5 ca Blk- 11/3/99 WH 7. 2201 bb 1.02 2 7 110499007 TCXI 5-RILS11 31-5;;:-1. 11/3/ Standard 1.00 7.122 22191 bb 1.03 1 3 a 110499008 7DX145 -RILSIIa*399-10vpb-9: 11/3/9"91I9 NO"M SStta.n@dAa@rdd 1.00 7.L23 25,45 bd 9 110499009 TOX145-RRSll 3 -25ppb-9 axt . 1113 /9 WR Standard 1 00 7.123 2 1 0 bb 1..112' @2 10 1100::990010 11 T'mO Xi45-RILSIIa O3:-50ppb -9 , 6= n&S -R&Sll 3 -10 OPPB- ;. 11/3 9 a= . 11 3/1, .1 3 t..d&rd 1:00 1 .00 7.1025 7.1 6: 203 2 bb 2317 a bb 0 l@.@900 11 11 12 1104,99,012 TCn45 -RUIZ03:-250ppk@l. "t. 11/1133//,1g, mUmM t-,d 1.000 7.1 1 72 bb 1.01 1 13 110 9 013 TIOXI@15-RILSIX03 -SoOppb-9 , "t . 11 um Vtao"@d 1 .00 7.12 2 3 , bb 7 14 1100199014 5 TOX145 -RSS1103:-750ppb-9"WM 1113/1, t&ndard 1.00 7.130 23 05 bb I.07' 9 1..0020 _10 2 is 11 &9901 WX.145-RZSllo3 -IOOOVpb- @t, 11/3/11WEwu st,-rd 1 7.106 2 10 bb 1 131 0 1167 1106:9016 K.OR 01&.k 7. 7 1907 bb 0.99 -10 a 11004 9:017 TID@4 5-RTSI 1003 :- 2550VPb-M 1. -t. 11/3/11 0= .106 z 1 11 4 Oil TO= 4 -RTSII 3 -2 Gppb-KSDIO' 11/3/91 M= 15-ItTS-gRG32&C42MM-_0o- 29 11/3/:9 0= 7.077, 1730 bb 1490 0.90 -2 1 0.69 -310 1290 11049990012901 TTOOXXI145-ffS-9RO32&IX-C-Dy D-Y 29: "t. 11/3/ 1 WH 7.'146 2231 k@' 1.04 1 z: 21 1104 9 2 loxl4,5-RTS-9RO32 _Day 21, WM. 11/3/:9 mm 7 143 2377 bk' 1.10 0 22 110499022 7oxi S-RAS11039-250ypb-CCV9. =t. 11/3/9 UM oc 1.00 7:.126 2260 bbbb 1.05 5 23 1104::023 M.OH Zink 7 167 11 0.01 -99 21 110&'990245 TOX145-RTS-:2032,43x-@0-Dy 3:: -t. 11/3 7.167 2212 Mbb 1.013 1 3 25 11004&99 02 nlS-RTS- 'RRo032 5 3M- -D. 2 @. 11/311:: "W=l 7.1 9 2451 bd 1. 4 1 26 11 026 TMoXI&S,-RTS- 32 SK-S.9/kyg-Dy2g. wm. 11/3/19 MM 7..122 2005 bb 0.93 - 27 11049:027 TOXI ,5-RTS-:RO3256M-Sg/ kg-Day29, wm. 11/3/19 NCR 7 129 23:0 bb .11 11 28 110 49 028 TOXI S-RTS- R03257X-SM/kg-DAY29, wt. 11/3/99 M= 7.L22 2598 7 bb 2: 1104::029 TOXIA:-RBS11031-2500pb-CCVIC. a.t. 11/3/19 MM QC 1.00 7.090 1 6 bb 0.92 1-: 3 1 11 0A99030 3 32 11110:19031 33 11.1910@3 34 110:9:0134 35 11 .4:,0l, 1 36 11 6 337 11004:900337 a 11 4 9 a 3% 11004,990039 0 40 110499:04'1 &1 11 42 110499012, 4A3 1ll1o0d44g9:99o0t "35 45 110 '99 0 46 110 0 M.09 I..k TOXIIS-RTS-:RROO32SSaN-SM//kg-Dy2:: 322 9 -Sm kg-Dy2 -t. 11/3/:9 NCR 1113/ 9 UM TCO)Xn144S5--RRR"S-11039- S=CCV9. "t. 11/3/19 MM M.OH,S5l@.k " -.UO 39-120 llk-9. wm. 11/3/19,NCH TOX1 TOX1 45_-RTBSS1I1I003399_-SS&.rr.a :'k -:: -t. 11/3,1:,WE IIOXI Ik- axt. 11/3 mcii TCX144S-RBS11039-5ppb-9,,*@..11/3/999WH" TOXI S-RILS11039-10ppb- 9, 1113 '99 MM TCO)XIAS-LELSI1039-25pob- 11/3 MCH XI&S-RDS11039-50ppb-9. ."t. . 11/31 9 MR TOXi &S-RaSI100 39-100ppb-:. TMtXX1l45-5R_JRLBSSIJI03,39-_2SS00oppppbb- 9, A 9. Tl3xl4S-RW11019-7 Soppb-- -t. . @M . ll//931,999WR 'll/3 ,9 9 WH 11/3/9 9 WR 11 9 PICH =XIAS-RELS11039-1000ppb-9. -t. 1113/99 WR oc Standard SS t d Stt....".V.d d Standard Standard SSttr_d""@d d Standard 1.00 1.00 1.00 1.00 1:00 1 .1.0 1 .00 1 .00 11.000 7 1002 7:.1 5 la 7 ,0 7 13 7.122 7 .1J1,1 7.12 1 7.1024 7.18440 7..O,g 7. l@, 7" 7,112065 77,.130 2213 bk. 20022 bb 20 5 bb 9 bb 18077 NK 2 8. bb 670 11912052 bbbb 22063 bd 17l4@1. b1b 2 076 bb 2203092 bbbd 2 &94 MM 1 bb 3 100 .093, 9 0 00 0 87 0 93 00 ,7ag3 0 99 0 96 0 al 0 90 0 96 1 ol 0a *9838 _3 _7 -10 6 -130 -7 -_2l2 1 2 -1-94 2 A 4 _127 S@V 020111: Q@titatod =4 Printed by L" an 11105111 gt@tily calibwati@ R.P=t ?=&$-,at .*K&, "Y 29 dO" 11/3/99 N= Compound1name:POAA (Chl) Response Factor:68.6538 Response type:ExternalStd,Area Curve type:RF x 103- x x x Response- x x x x x nV-T0.0 moup 0201991 Quanti@ted 0 .1 0.2 0.3 and VWUMed bY l@ M 11/05/99 0.4 0.5 -T 0.6 0.7 0.8 0.9 iconc Ok@tity C&Iibrati@ RW@ ?=&S-@at ..r., 6.y 29 d@ MA @tw*l- WM- 11/3/99 N= Compound 2 name:PFOS (Ch2) Coefficienotf Determination:0.980777 Calibratiocnurve:20.4798 - x + 108.210 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude, Weighting:1/x,Axis trans:None 2.29e4- Response@x 0..0 . . . . . . .200.0 MOUV 020199: gl@tl@tod and mciated by L@ m &IioS/99 400.0 600.0 800.0 Conc au=tify C&LLIW&TLM R"@ lio=45-tot "K&, day 29 d@ " @@l- @. 1113/99 M= Compound 3 name: PFOSA (Ch3) CoefficienotfDetermination0:.997747 Calibratiocnurve:245.706 * x + 643.062 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighfing:1/x,Axistrans:None 2.41e5- P.g. 3 x Response- x 0 o-o SOUP 020199; g@titated a" pri=od by L@ m 11105/99 Conc T=45-Y ... ..... 4-r 29 &--- 11/3/99 mcm Compoun4dnameS:ur(rCh4) Response Factor:2153.97 Response type:ExternalStd,Area Curve type:RF 2.54e3- Response- v@. 4 x x x x x 0-. 0 Conc L 0.0 .1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Soup 020199: 9,@titatd and primed by L@ m 11/05/99 Method Report Method file: ,.at Modified Compound: Printed: C: UWSLyn"oup02Ol99.pro%N*thDB%llo499a.mdb Fri mo@ 05 06@29,44 1999 1, POAA (Chl) Fri u- OS 06@S6@56 1999 cxat.,.'lif,y NR-ef.: 01,-,. . T@ ..: c@ f standards: U :r ILFVal *: 0: r Peak F&Ctcrt Y@tor: CIhnrt@otgorg.rt=. WinMda@ss wind@ R.t:ntion Time (ai@) Rol tile Rota,tion Tim 'IT Mfere-.: Time Mid- (-i-) peak selection: Type: ".S"p*a-" :: Polynomial Type: Point Of origin: pit w.ightigz Axis Transformation: PQU fc2a) [now TXC ti..d I Diabld 1:'..O*O.*.**o- 2 1:.*.*oo. 7.1067 0t.000: no', 0 .34S M-bld Di.abid s@t at@l Ar@ LiI/X u.its: P.ak-to-p.ak awlitudez s@ thig: mind@ size (.C@)i Number t @th.; Smothing @thod; Join valley throokwid: ledu * pe:kit.:iling: Itai.:be. 1 Drw @rtical threshold: Dat@t shoulders: Shoulder threshold: Relative height: Aboo&llto height: tiv. -..: Absolute area: al U..bid 2 I 320.-000.00.0 5 9*,-.,I*blod I.SO D sab ad 0.00: Diis"lld 2.00, Disabled 0.00, Dizabled @thod Report xthd file; L"t nodifid: Co.po.nd: Printed; c:%KLSSLYNX%soup02Ol99.pr.UMthDB\lIG499--'ab rri Hav 05 OGZ29:44 L999 2: Pros (ch2) r@i u.@ DS 06,56.56 1999 Co.po,.Id UI.Sta@l Rot.: Q@tity Trace: c@. of standards: Door RY Value: beer ftak Factor: Integrate wind@ Factor; ch.@tog@- -.. .-,. : Retention Ti@ (mi=) ; Relative Retention Tim 3tTRat ...met Ti@ Wind- lsim) Peak sol.etic.; Pm (ch2) ln@ I TXC C- . A 1.000000, 1.000000 2.000 1.0000co Di.@blod 7.429, gnahld 0.000, Disabled [n@] 0.467 u@t Rasp @ . Type: R.Spo-.; Exte P@ly.-i.1 Type: Point of Origin: Fit Weighting: Axis Tr@fo@tim: a-lud. 1/X roak-to-po&k awlitu": 2-thing: mi.d- i.. C..-) : Numdmr of @ths; S@thzng "thod: Join valley thro&klold: Reduce peak tailing: Asia. b ..line .Xi-: m@ vertical threshold: Detect shoulders: Shoulder threshold: Relative Absolute Relative Absolute height: height: @**; @ea: id 2 I 30.00 200.00 5.00 20.00 Di.@blod 30.00 1.50. 0.00, 2.00, 0.00. Disabled Dia&bld Di..bld Disabled Page 2 -f!. Method Report method file: xast @dified: Compound; Printed: C: %xjLssLy=%a4v2po2ol99-yr.%MthDs%llo&99...db r@i a- as 06:29@44 1999 3@ PFOSA (Ch3) Fri U.@ 05 o6;s6.s6 1999 Compound N@ internal Rf.; Q@tify Trace: C@ . of St..drd.; User R? Value: User Peak Factor: integrate Wind@ Factor: chr@togr= mas wind@ PTO" (Ck,3) In-] TIC C@. a 1.000000, 1.000000 2.000 I.OOOOD. Disabled I.:,t:tntin Ti- (.i-) i@: Retention Ti- totere=*: RT W Ti" ind- (.i-) Peak Selection: 8.147, S.@bld 01 .000. Di..bl.d 0 110- .356 m@.st RR..-XPpooz:: Type: Polynomial Type: Point Of Origin: Pit Weighting; Axis Tr@fo@tim: units: Peak-to-peak amlituds: S-othing: Wind@ i.. (:c@); Number :f @ thm; S@thing @thods Join valley threshold: Reduce pak tailing: .is. ba..l...@i-: Dr@ vertical threshold: Detect shuld ... : Shoulder tt@@*shold: Relati V: hoigght; Abe lut hei ht: R.I.t@ . -..: Absolute r..: z=l I/X $I Z"bled 2 1 120..-00.0.. 50 90.00 Di-bld 30.00 Di.sbld '0-"o : Di bld 2.00, Dis4Lbl*d 0.00. Di.&bld Page 3 Method Report Method file: Last Modified: compound: Printed: C: XMJLSSLT31X\@p02Ol99. pro\XethM\1104999 Fri M" 05 06,29,44 1999 4: S@ (ch4) Fri bov 05 06:36zss 1999 -Oft Compound Internal Q-tity C.-. of U@ R.f.; T..C.; St.VAt.@d.% User IL;Value: User Peak Factor; Intogvate Windw Factor: ch.-t.o@- -.. ind-: S- ccb4) (w@l TXC Fi..d 1.000000, 1.000000 2.000 1.0000C. Dia&bld ::tontion Time (mi@) : lativ* Retention Tim; RT A* Time Wid- (.iM): Peak Selection: 7.218, ---jd 0.000. Dis"ld 0[now) .379 N--t Re po a Type: atax@l Poly@al Type: Point of Origin; Fit Weighting: Axis Transformation: unit.: P.ak-to-p.ak amplitu": s@thi.g: Wind@ its N,..b.r :f - the: 2@thing Method; Join valley threshold; Reduce peak tailing: itsime k@seline maxi@: vertical threshold: DDertwect shou ld.rs: Shoulder threshold: R.1 tluir-e .'. Relative hi ht; h.iggh, &... B=lude I/X N@ $I -bid 2 I 120.-000.00. 50 90 00 Di.* .bld 30.00 1--.,.*: 0.00. Di-bld i"bl*d i"bld Di"bld (tits QuattroII,#6414E SOUP 020199:FACT Equipment Log 99092 PAGE 1/1 DATE:- -01@4-99@ ANALYST-i-as STLTDY NUM13ER: T_Q.,XI45MATRIX: ratsera DESCRIPTION: d2a@9- dose@On@l FACT Method:ETS-8-5.1 Injectivoonlume:_IQ_UL- Cycletime:10niinE.lectrode:-Z--a2LaY-- MobilePhase: - (A)L.LmM-NH4-0i= (B)McOH TN-A- orstndrdnumber (A)99085-11-15 (B)jTAN-A-2-9_97- Prepare(ddatelby): (A)Igagals-a!L- (B)IE2gL9-9-54h- Expires: (A)04/00 (B_)ZQL(L- Storeatroom temp? E or N Other: Guard column:None Parntumbenra:_ Lot number:na Analyticaclolumn:KeystoieBetasil Size2: x 50 r= Type:C 18 Partnumber:055-701-2 Lotnumber:P9E II Spheresize:5 um Serianlumber:0591804Z Analyticaplarameters: Dryinggas(lJhr)3:50 ESInebulizignags(Uhr)_U_ LC Flowrate3:00uljmin. Back pressure6:5 bar Sheathgas(Llhr)_Q- BPLC solvengtradient1:0miD-10-95 Time (a@n.) %B 1)0.00 10.0 2)1.00 10.0 3)5.50 95.0 4)7.50 95.0 5)8.00 10.0 Page Tuning method Report method: C:\MASSLYNX\SOUP020199-pRO\ACQUDB\PFOS3 Printed: Tb, Nov o4 14:02:27 1999 IL bIs SOTJRCE ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. MS2 Set 1.60 40 5 0.2 150 250 Rdbk 1.62 -41 -7 150 250 pressures Analyser Vacuum Gas Cell Rdbk 5.le-5 4.0e-3 Nsi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 3 650 Set Rdbk 14.0 14.0 10 7 2.0 0.0 40 36 0 1 650 se..Duw atkd mthad; L-t Ndifted; Printed: PC& CWL 15 10:35,03 1999 11. ak@ Ot 13.16,28 1999 solvent Delay ( EL" ) : 0.40 puwti- . I @ of I 1P.Lr( asp- later Channel Delay S@s 0.03 Span t D.It.m ) , 0.00 St@ Ti- ( Ki= 0.00 Rnd T- ILi" 10.00 R.P..tC.hannel Parent Daughter DI@ll (S@.) Coll Suargy (OV) Co" V 1 413.00 169.00 0.30 30 is runctim : 2 f I la"s P&ir ( a"- Inter Ch@.1 Delay I Sets 0.03 Sp- C D&lt.- ): St-t T- ( K- ftd T@ M@- 0.00 0.00 10.00 P.P..to C@.1 p@t Daughter 1D-11 IS@s) Call MervY (OV) Co- t V 1 499.00 99.00 0.30 AS 60 FunctL= 1 3 1" of I name Pair t ZBP- I.t.r Ch@l Delay S5 P- ( D.1t@- ) , art Ti- ( Mi@ Sec. 0.03 0.00 0.00 = li- Ki- 1 10.00 Repeats Channel Parent Daughter I D@ll (S@s) Coll Itnergy (OV) C@ V 1 499.00 78.00 0.30 45 60 yu..ti- , 4 of I nw. P.L. (ROP- later Ch@l Delay S*cs 0.03 SP- ( D.It- ) : St-t Ti- (Ki- and T@ Ki" 0.00 0.00 10.00 Repeats Cb@*1 I Parent Daughter Dmll (S@.) Coll N@rgy (eV) C... V 1 427.00 10.00 0.30 40 60 method Report method File. Last modified: Printed3 Cskn"SLYNXkSOUP020199-PRO\ACQMM\IOAin-10-95 Th=*"y, November 04, 1999 llt22z29 TILurs"y, movember 04, 1999 13:18:38 nplloo = puup initial Conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Crven Temperature Right(OC) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 EPIIOO Lc Pump Gradient Timetable The gradient Timetable contains 5 entries which are Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 EP1100 LC Pump Xxtez"l Event Ti@table The Timetable Time Initial 0.00 0.10 contains 3 entries which Column Switch Off Off Off Contactl Off On Off are Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off Epiloo Autosamlor initial Conditions Draw Speed Eject Speed (iil/min) Draw Position (mm) Stop Time (mins) Injection Volume(lil) Vial Number 200.0 200 0.00 9.00 10.0 51 Page 1 Pressure 400 400 400 400 400 Masslynx - Sample List Sample Ust:C:\MASSLYNX\soup02Ol gg.pro\SampleDB\l10499a.SPL PrintedT:hu Nov 04 13:18:221999 Page 1 Page Posibon:(1,1) FileName FileText MS File 10MIN-PFOS-POAA-PFOSA-IS 1 110499001 MEOH Blank IOMIN-PFOS-POAA-PFOSA-IS 2 110499002 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 3 110499003 MEOH Blank 4 110499004 TOX145-RBS1 1039-H20 Blk-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 5 110499005 TOX145-RBS1 1039-Sera Bik-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 6 110499006 TOX1 45-RTS1 1039-Sera Bik-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 7 110499007 TOX145-RBS11039-5ppb-9, ext.11/3199MCH IOMIN-PFOS-POAA-PFOSA-IS 8 110499008 TOX1 45-RBS1 1039-10ppb-9,ext.11/3199MCH 10MIN-PFOS-POAA-PFOSA-IS 9 110499009 TOXI 45-RBS1 1039-25ppb-9,ext.11/3/99MCH IOMIN-PFOS-POAA-PFOSA-IS 10 110499010 TOX1 45-RBS1 1039-50ppb-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 11 110499011 TOX1 41-;-RBS11039-100ppb-9, ext.1l/W99 MCH 12 llD499012 TOX14&RBSI 1039-250ppb-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 13 110499013 TOX1 45-RBS1 1039-500ppb-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 14 110499014 TOX1 45-RBS1 1039-750ppb-9, ext.1113199MCH IOMIN-PFOS-POAA-PFOSA-IS 15 110499015 TOX145-RBS1 1039-1000ppb-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 16 110499016 MEOH Blank IOMIN-PFOS-POAA-PFOSA-IS 17 110499017 TOX145-RTS1 1039-250ppb-MS9, ext.11/3/99MCH IOMIN-PFOS-POAA-PFOSA-IS 18 110499018 TOX145-RTS11039-250ppb-MSD10, exL 11/3199MCH IOMIN-PFOS-POAA-PFOSA-IS 19 110499019 TOX145-RTS-gRO324OM-0-Day 29, ext.11/3199MCH 110499020 TOX145-RTS-gRO3241 M-G-Day 29, exL 11/3199MCH IOMIN-PFOS-POAA-PFOSA-IS IOMIN-PFOS-POAA-PFOSA-IS 2210 110499021 TOX1 45-RTS-gRO3242M-0-Day 29, ext.11/3/99MCH 1OMIN-PFOS-POAA-PFOSA-IS 22 110499022 TOXI 45-RBS1 1039-250ppb-CCV9, exL 11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 23 110499023 MEOH Blank 24 110499024 TOXI 45-RTS-9RO3243M-0-Day 29, ext.11/3/99MCH TOX1 45-RTS-9R03243M-0-Da)l 29, ext.1113/99MCH IOMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 2256 111100449999002256 TOX145-RTS-9RO3255M-5mg/k!g-Day2g, ext.11/3199MCH I1OOMMIINN--PPFFOOSS--PPOOAAAA--PPFFOOSSAA--IISS 27 110499027 TOX145-RTS-gRO3256M-5mgtk!g-Day29, ext.11/3/99MCH IOMIN-PFOS-POAA-PFOSA-IS 110499028 TOX145-RTS-gRO3257M-5mgtkg-Day2g, ext.11/3199MCH 10MIN-PFOS-POAA-PFOSA-IS 28 29 110499029 TOX145-RBS1 103!3@250ppb-CCVIO, ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 30 110499030 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 31 110499031 TOX145-RTS-gRO3258M-5mgtkg-Day29, ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 32 110499032 TOX145-RTS-9RO3259M-5mgtkg-Day29, ext.11/3/99MCH 1OMIN-PFOS-POAA-PFOSA-IS 33 110499033 TOX145-RBS1 1039-250ppb-CCV9, ext.11/3/99MCH IOMIN-PFOS-POAA-PFOSA-IS 34 110499034 MEOH Blank 35 110499035 TOX1 45-RBS1 1039-H20 Blk-9,ext.11/3199MCH 10MIN-PFOS-POAA-PFOSA-IS IOMIN-PFOS-POAA-PFOSA-IS 36 110499036 TOX145-RBS1 1039-Sera Blk-9,ext.11/3/99MCH 37 110499037 TOX1 45-RTS1 1039-SeraBlk-9,ext.11/3/99MCH 1OMIN-PFOS-POAA-PFOSA-IS IOMIN-PFOS-POAA-PFOSA-IS 38 110499038 TOX145-RBSI 1039-5ppb-9,ext.1113199MCH 1OMIN-PFOS-POAA-PFOSA-IS 39 110499039 TOX145-RBS1 1039-10ppb-9,ext.11/3/99MCH IOMIN-PFOS-POAA-PFOSA-IS 40 110499040 TOX1 45-RBS1 1039-25ppb-9,ext.11/3/99MCH 1OMIN-PFOS-POAA-PFOSA-IS 41 110499041 TOX1 45-RBSI 1039-50ppb-9,ext.11/3/99MCH 42 110499042 TOX145-RBS1 1039-100ppb-9,ext.11/3t99MCH IOMIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 43 110499043 TOX1 45-RBS1 1039-250ppb-9,ext.11/3t99MCH IOMIN-PFOS-POAA-PFOSA-IS " 1104990" TOX145-RBS1 1039-500ppb-9,ext.11/3199MCH 46 110499045 TOX145-RBS1 1039-750ppb-9,ext.111"9 MCH TOX1 45-RBS1 1039-1000ppb-9, ext.11/3t99MCH 1OMIN-PFOS-POAA-PFOSA-IS IOMIN-PFOS-POAA-PFOSA-IS 46 110499046 Masslynx - Sample Ust Sample Ust:C*.\MASSLyNX\S()Upo2olgg.pro\SampleDB\l10499a.SPL Pdnted:Thu Nov 04 13:18:221999 InletFile Battle lnjoeVolume Sample Type 1 10min-10-95 91 2 1Omin-1 0-95 91 3 10min-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10mir@-10-95 3 7 10min-10-95 4 8 1Omin-1 0-95 5 9 10min-10-95 6 10 10mir,10-95 7 11 10min-lG-95 8 12 10min-10-95 9 13 1Omin-1 0-95 10 14 10min-10-95 11 15 10min-10-95 12 16 10min-10-95 92 17 10min-10-95 13 18 10min-10-95 14 19 10min-10-95 15 20 10min-10-95 16 21 10mir,10-95 17 22 10min-10-95 25 23 10min-10-95 92 24 10min-10-95 18 25 10min-10-95 19 26 10min-10-95 20 27 10min-10-95 21 28 10min-10-95 22 29 10min-10-95 26 30 10min-10-95 93 31 10min-10-95 23 32 10min-10-95 24 33 1Omin-1 0-95 25 34 1Omin-1 0-95 93 35 10min-10-95 1 36 10min-10-95 2 37 10min-10-95 3 38 10min-10-95 4 39 10min-10-95 5 40 10min-10-95 6 41 10min-10-95 7 42 10min-10-95 8 43 1Omin-I0-95 9 44 1Omin-1 0-95 10 45 10min-10-95 11 46 10min-10-95 12 10 10 10 10 10 10 10 10 10 10 10 10 10 10 - 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 - Conc A Conc a - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - Conc C - - Page 2 Page Position(:2,1) FACT: DA'I'AREVIEW SUiNliN[ARYFOP@NI Data Analyst: 4s FACT Study0: Irlx/419- tvi,2trix/Timcvoint4s/: @., Sample List- Sct-upAnslyns DatdAngyst Instrument alw Lrol" Analyte: P44A AccepWAol==Ranvm LOQ. AIA NA AIA ExuactionBlank 94 M== Blank WA CalibratiCobnec H4 NSIMSDID&taSu= AJYF@- -PATA-IVT @2 IUL Data Review Sign-Off Analyst Review Name/ Date: TechnicalReview Name/Dam. Qu&Uty Amurence Review Name /Datc: Data Intrr. cittl 111611M Cormmnts /Jusdfkations: 10 @ ililre YAA- .4,, 7o'.4A -/-Y LlreaL -4A-17;^. Rd Anslyte: t@7o5 ecbfz)lo AcceptableLinearRAnge. Zf S'o L LOQ: 2f E=wtcd BIA& -le.6 I& /Do R^2: 0.lfls Mt6x Bik /e2;W--@ bQ CalibmfiCohnecicL OA MS/MND.- m DataSw= GP.(o %LlilD 4@K@ 140197 oileIr L/ Alea. cogm-4 s Irlf f Analyte: 7rvsA ("CH3) AcceptableLinearRange: @,@L? LOQ: R-2: D- ?f?70oo CalibratioCnhecks: MSIMSDI. DataSat= r@c a, Y7,7..@ Extrwted Blanir -les, -tzoo Matrix Bink.- 11@Cs A- /,Oa 01(l FACT: DA'I'A REv'IEW SULNINIARY FOR.NL Dat2 Analyst FACT Study 0: -fox lyr tviatrixmmepoints: PIJL,@ 2@ Sample LioL Sct-up Analysis Date/ArAlyst Wtrument N$(# ff 6201!?f Data Review Sign-Off Analyst Review Name/ Date: JAC 9/,C/09,f Technical Review Name / Date: Pl@Er @2 QuaHty Anurance Nme / Datp- Raview DateEntrr. PIaF,w OKIL LAC or4@ tA(l-i/i/ii Comannts Justifications: Ac=pW)io Linca Rmsc NA LOQ. AIA R^2: A#l ciaibmtionCheci= E=ac6m BWzk Matrix BU& oVA Data Staum Auslyte: AcceptableLinearRmge.- LY LOQ: Extacted Bknlc R^2: NLvjix B CalibrationChecks: msa4zi> iDatRS am Analyte: AcceptableLinearRin LOQ- R^2: Cpr-.@ail.ibb Cheecckks,: Exuwtod Blanl,Matrix Blank. taSatu. a@tity covowbd S@ T=45-d.y29 - - - I .d "PO@ - . 1113/99 samia L'int; L"t modi f led. Pri M@ 05 13:24311 1999 L"t ."fiedi ".. aw, 08 07:09,59 1999 Job C.": Printed: um MW- 02 07:20:42 1999 C@.p@..d l@ PC" (CILL) R110599028 2 1105 9029 3 110055:990a301 45 1105990332 6 110599033 7 110599034 e 110599035 9 110599036 10 110559,9037 112 I11t1.o5.9.9:0033.: 13 1105990,Ll I' I11' .111 0' 6 11 0599004 3 117 110519044'1 is illias9lols 19 110599016 20 110599047 21 110519048 22 11005990109 23 11 99 5 50 24 11055:90051 25 110599 0 52 267 110 5,:053 28 11005,9051 2 11 55 2: 1100 55 005 6 3 11 57 31 110599OSS 32 110599059 33 110599060 34 110599061 35 110599062 B.Ml:list HoO a I&nk IWCNH lank MaCH'Slank TTOO= -RSS11039-K2O Slk-S. o@. TI,X145-RBS110039-5 S:r :lk 11/3/99 34CH 11/3,/99 MM m)Ll4s-RTS11 39- @: Ik- X145-RBsllO039:S S)b-9. oxt.wm1.1/3/1919/3 WH99 "M TIDXI,S-RA 11 39 IV5pp b- 11/3//99 ICE Toxi &S_-RBSSSJ1J1003399_-5200ppppk@::9. @WMM: ll,/3,9:WH TOX1 S_RBSIIO39_loop b- 9. 1113 3 999MM Toxi 15-P@RS11039-2SPOb-9. art TToOxXiI.,-Rssllo3g-Sooppb-1. S-RRS11039-750 9, "t TOX1,ll-.1@031-101)popvpb-b-9, 1 1/3//IlMM 111/3/99 wu 3/19, mm lN.'OoHn 31-k T740DX1,15-RTS-IR0R3o25SH-5@g/)19-DOY29. xi S-RTS-:3to32556N-5M/kg@Day29, D,10 D,10 TOXI,5-R"- 32 7K-5.0/kg-D.YZ9, D.10 Toll's-RTS-9'RO32558M -smixg-DOY21. Ton S-Wrs- "32 9N-5m/kg-Dy29, 1)@10 D'i TOX.1 5 RRS11039-250ppb-CCV9, xt. 11/3'/99 Em M.OH 'al-nk TIOXI&5-RSSII003:-820 .51 -9 -t..Il/ / 9,m= -MX145:RRS1103,-Se Sklk-;.-t 113/31 :,, ics TOXIIS RTSII 3 -Serr.SIX-9. -t. 11/3/ 3= ToXI 45-RILSII0 0399-5b-9, =t. 11/3/91 MM TOXI S-RAS11 3 -10pppb-9. wm. 11/3/99 MM ToIOXIIS-RILS110039-25opP:bb:9 9: 1.111,11: -TIZOIXXX5Il&4155:PRZBSI11I1133:9--5100ppb-9. 5 RJLS110 3,-2S0Oppb-9, TOX1 S RBSIIO 3 -50 b-9 TOX1145-RBS11039-750,pb-p9p: TC=45-RBS11039-1000vpb-9, "t. a=. "t. "t. 11/31993"mm 11/3/99 UM 11/3/99 mm 11/31 9 WR 11/3/19 WH 2w. It---,d St &ra&rd sta.Ki@.d Standard Standard S3tandard tand",d QC standard Standad taodard standard 3 tandwd and"d :ttand@d standard Standard T.4 1.00 1 1:..0".. 1.00 11.00 7.17M2e 7 1724 7:19 717 7:.11753 7.172 47 7.117 7:155 7.17 4 7.131 1.00 1.00 1.00 7.1706, 7.151 7.152 1.00 7 1705 7:19 7.173 7.175 7.192 7.116 1:.*00 1 .00 1.00 1 1.00 1.00 1.00 1.-.000 7.133 7 7:'1'33 '1:17 2 7. 117 7.1' 1 7.171 7 7.1462 7.1553 7 174 7:131 Area ri"s 23 bb 2107 Mbb bb I&S. bb 48 bb &2 bb 39 bu bm 53 NK 6531 UMM 87 UK 5m 87 bb 1m 106 bb 21 m 32 17 bb AS :7 bb 3M 1 bb 4& NK 45 NK 381 bb 5sa m 7673 bMb 83 Mbb c@ . 0.49 0a .35, .2 1.203 0.98 0.7, %D- -si :76 5 1 20 --7 -22 -21: 0'67 33 0 92 1 * 06 11 '09 9 -11.0 1.0 I0 .':l 2 0'2786 -_6743 356 _d 00 29 -74 0:75 -321 1.107 17 1. 5 5 00 .75 -25 C,.71 :29 0 .76 2 .78 22 00 .:7 -33 1.09 -11 0 I'loo 10 1*14 34 1.14 14 SOUP 020119% Q@titated and printed by i" an 11100/11 G-.LEY "=45-d.y29 0--" "W- -..-I .d d.--- @. sawl. List: L"t .ditid: awthod: L@t moditiod: C.": CFri N- 09 15,26:11 1999 0 @%"58X.YMX%wouD02019g.PM%31*tW=%IlOSggb Um U@ 04 07@09,38 1999 Print.d: mm n@ 06 07:28-42 lttt Co.pmL@d 2: Prog (CU2) # m@ 1 110599028 2 110599029 3 110599030 4 110599031 5 110599032 6 110599900333 7 11059 4 8 110599035 9 110599036 10 1105990g3o7 11 11059 38 12 1105:9039 13 IIDS ,904,0 it 1105 90 1 is 110599042 176a 110559,9004315 19 110OS,:046 2. 110519017 21 110599048 22 11005999049 23 11 S9 050 24 110599051 25 11059:052 26 11059 go053 27 11059905A 28 11059 SS 29 1105::056 301 110599 057 3 1105 oss 32 11059:059 33 11059 060 34 110599g0o61 35 11059 62 sami.ii.t Tft HOOH al..k X*CH Blank M.09 DI..k TC)UTS:RB 11003,9-B2 31 -9. wm. 11/3/99 WR TOX145 RBSSII 3 -Soo,. Bklk-: wm. 11/3/ TOX145-RTS110309-Sera glk- : @ . 11/3/:: M)CcIz 'MMXI 5-ILBS11 00 3,9-Sppb-9, To Xl 5-RBSII 3 -1Oppb X145-RBS11039-25ppb-9: a. 11/3/99 )Cn m. 11/3/ 11/3/:: WWOR 110xi 44 5-RBSll 0 39-509pb -9. mm 11/3/99 WH TC)XI S-RaSIl 39-100ppb-9 axt.. 111/3/ TOIL14S-RZSII03:-20SO=:: . a,t . 11//33//:9:9NWWHCRH TOXI&S-RRS1103 -5 0 MX14S5_-RRBDSSIL1I003399_-170500ppb-91 9. "t. 111/33.//939199NCWRH Oppb- DI." XT.OOXnI&S-RTS-9RO3"205SX5-5M/ko-DSY29 D:10 'MXIAS-RTS-:,to32S6M-5M//ko-DOY29. Dzl. TOX14,5-RT.S-,,,32.7.-W k.-Day2 0:10 TOn 4, S-RTS- 'Ro 32 S In-SMlkg-Day29, 0:10 Taxi S-RTS- 32 gm-SM/ka-D.Y29, D-10 TX0*3oUn4&5-RRS11039-250ppb-CCV9, ext. 11/3/99 UM Blank TondS-RDS11039-920 Slk-9. -t. 11/3/9, WE TCXIAS-RBS11039-Se'a :lk-1. a=. 11/3/99 WR TOX145-RTS11039-S.@ a lk-9. IMXltS-RRS11039-Sppb-9. wm. -M1.1/3/1119/3/W9E9 MM TonAS-RRS11039-1 pvb-9. wm. 11/3/9: WH TOn&S-RaSlIO39-205ppb-1. 11/3/9 , BCI.CH 'Mxl :5-RZS 11039-50ppb-9. Imn S-RDS11039-laoppb-9 11/3/ a. 11/3/1: WH TOXIAS-"S 39-25oppb110 : "t. 11/3/99 ICU TOn&5-RDS11039-5000pb-9, 11/3/,g MM Toxi&S-RBS11039-750ppb-1. 11/3/ um TC)XI45-RES11039-1000ppb-9. -t. 11/3/19 )OCR syp- standard Stad"d SStandard tandard Stta.d@d sStand"d standardd St&nd"d oc sta@drd standard standard standard Standard SS tandard t..dard standard standard Std eme 4.936 9.7 2&.0300 49 2497:.6000 8 733..000 976 2&8.00 4.93 9.7806 2A 49.30 17-600 2 19@8, . 0 .0 7.3.1.--.0... nt 7.288 7.290 7.309 7 3160 7:.27 a 7 .2:4 72 7 255 7 2:4 72 2 7 271 7 21: 7 .2 7 . 2:go0 7 .3 7 245 7.310 7:315 7 3 11 7 314 7 . 331 7 .313 7 .265 7 .273 7 337 272 7,-2:0 7*2 7.27: 7.2:66 7-2 .9 7-12:3 7.2 7.2710 A452 394 386 1519, 2 55 2 318 69 41 a7 1521 rL". bb bb bb bb bb bb mm N= bb '707'02.'1 bb 2&13707 bb 02 29230 bb 0 bb 10749 bb 1197 9 bb 1203611 bb 12 2120 3 bb 701 6 bb 171' bUKb iss bb 16&9 bb bb 2982 Ma 55 , ma @87 3 bb 33 a 9 bb 70911 bbd IIS0'171 bb 22 a 2 bb 28 4 bd c@ %Do.&$ 6.39 6.62 0.116 2 17 -13 3 5 57 25 47.@0. 70 -42 2'55 37 3 &89 79 721'17 -21 967.51 1 3.70 3597.3 1 09,.1O3'' J'bk 4&12' 735 67 232 31 -6 0 0 -.10 a 00 0.00 13 -27 2 2.-292 26 I- ,2 - 1. 6 1036,.45 -9 2 .86 5 48493.73 -1 7 .27 -1 975.12 0 4-, V". 2 MOUP 020111: Q@tL@t.4 and pvinte4 by L@ ll/ogl,g Q.Mtigy cmpmmd D@m@Y MOOO@ TC= 4s-"y29 @tml and do**- @. 11 sawle List: c -UDASLTXX%.Ouvo2olgt.pco%s-plem% L@t wadifted: rri Mv as 13:26:11 1999 C:%KRSSLTXKN@IP02019S.Ma@.tus%1105*9b Mtbod: L"t ..difid:Um Nov 08 07:09:36 1999 J.b C.4.: IP.L.e.d: Mm M@ 08 07@24:42 1999 Ila 599b C.NP.=d 3- PFC" (c2L3) 0 n@ 1 110599028 2 110599029 3 110599030 4 11OS99031 5 11OSS9032 67 1105:9033 110 S 9034 a 110599035 9 110599036 101 11055:9037 1 2 110 5199003&1 "13 '11..I1'11@ao' 1 15 110599041 11059 6 05,904,2 1., 11 3 is 1105,9094 1, 110a5990405 1 1105599 046 201 11 99 4L7 2 223 111100555999:00a44890 2 110 9 5 32&5 111100055:99:0512 26 1105599 053 27 110599054 28 11 .",aOll 230 1111059905576 31 110599053 32 110599059 33 11OS99060 34 110599061 35 110599062 B..pllLst Vast M.09 Blank KNOB Blank 36.02 Blank Dik-!P. =. 11/3/99 MM TOUAS-MI1039-9290-S.@. 11/3t99 N= 'MXIAS-R3LS1103 blk-, TOX145-RTS11039-S.@. Blk-,: W,M.311/3/99 0= TOX145-RILSII0033,9:510p,p,:;!; @. 11/ /99 NCR Mxl4s-Rwll TOX115-R"11031o@9:2 5 TOXIL 5 -RAS11 -t. 13./3/99mm 11/3/99 WE 1/3/9 mm 1113/99 mm TOX24 5 -RaSlIO0a3939-2150=9, 9 'TO0X=I4II :"R"S1'1l031-,5070,.=g 1: = TOX11S-RWll 3 - : 3/ wu l11l//3/99 WH TC)XlS-RSSI103 -1000vpb-9, "t. 11/3/19 MM SOON Blank loxits-M-9RO3255K- 21, D@10 TC=45-5RTS::R032,5&K:=,t-kg/ok:DkNgY_Y-D2.9Y,", D.10 TD=4 - R032 7M 29, D@10 TOXI -RrTSn-IR03258K-5-9/kg-o*y T(,n,S_RTS-9RO32SSU-SM/ka-Dy29, . D,10 TOXI S-RBSII039-2SOppb-CCV9. ext 11/3/19 MM M*OH42lMk lk-9, wm. 11/3/,g WR /3/9: MM .T=M1X4I5&-SR-IRLZSS11I0I3*3::BS2eoaa TOX14455-_RBTSSI111003399_-5S.r. ISilkk--99.. -"tM.. 111113/9 3= ppk,- 11/3/91 WR Toxi 45-RILS11039-1 9 TT'OmOX)1Ul!,-RDS11039-25 05=:: AS-RBS11039- "t. Oppb-9;, @m. ToUi4ns-RBsllo39-IOOVP@ TO IS-RBS11039-25 vpb-9, TOX=145-RDS11039-5000ppb-9, TOKI&S-RDS11039-7SOppb-9. 1IL1I//3//:99 3MICMH 11/3/99 WR 11/3/99 WR 21/3/99 WE 11/3/99 MM 11/3/99 WR Mx245-"Sll039-ICOOPpkl-9, @t. 11/3/99 MCH rag. 3 Type standard St---@d standard t,@ -ld :tandard standard st st..drd standard oc stedrd and"d St &.d.rd stad&rd s tandard SStt@-@'-d@d St--@d standard ftd COW 4-93 7 80 24. 697.3 0 :700 262 423.000 711::* 97, . 00 24S. 4:.93 29.8 7 49.300 0 - 97.7 249..000 493 734.00 177.00 at 7.952 7.592 7.894 7:17:1, .3 7 7.051 7::71 7 .8878 7 7 .$31 77.8897.81 7.829 7-:30. 7:.3 7 29 7 :71 7: 95 7 :74 7:..5712 7. 7 . 82 7 .2: 7 7 :.@:3231 7 7.:74 7. 48 7,:1: 7, a 2 7* a 21 10 7, a 7 77.8081 AX" 27SO 1436 744 723 so$ 368 YIW- db db db db m db 1I'1,6. 1513 51 25668 !13546 M 11934 0 17776 1:21 !,7@l a 412 m 429 M 534, 1-15121 Mdb 1: 54115 7 M S7 M 17"57 33 66309 M' 13371 M 27595 ng 62165 120712 Mm 177 61 2368709 m eme %DW S.Oi 2.63 0.00 0.00 0-.0O*o 4.55 -6 9.78 0 23.79 1050.34 2 3.03 5 239.25 -4 13 -0 479396311:.,107 -0 @.10 -1 0.00 dyl 0.00 ':'.'a 0.00 2360.607 -5 0: 000 0.00 0.00 .01 -1: 2140.15: -2 1512,0o9l 1 6 1 25 1* 21 1964:.93 31 733 0 977.81 0 4$* SouV 020111: Q@tL"ted mad prlntod by I" m illog/99 0--tify cmwm=d a@"7 1,0= & S-dAY29 Mnt@l M@ DDBO- @. 1113199 somis List: I"% odlfiod: rri U., 05 15:26:11 1999 imtb@d: C'%MSOLTM%-PO20199.pro%uothos%llo3tgb t@t xoditiod: Mm lftw04 07:09:58 1999 job cd.: P.L.t.d: mm no, 09 07:24.42 1999 compmnd as surr (ch4) a- 1 110599028 2 110599029 3 110599030 4 110599031 5 1105990323 6 1105990 3 7 110599034 a 110599035 9 110599036 la L10599037 11 110599038 12 11OS99039 L3 11059904LO 14 L10599041 15 1105990A2 16 110599043 17 110599014 is 110599015 19 110599046 20 1105999047 21 11059 048 22 11OS990&9 23 110599g0o50 24 11059 go 51 25 11059 52 26 110599053 27 110599054 28 110599055 29 11OS99056 30 110599057 31 110599058 32 110599059 33 110599060 31 110599061 35 110599062 smoielist T@ N.OH SI..k X.OH &I." N.OH Blank Toxl45-ILBS11039-H2O Blk 9 wm Tc) 45-RES11039-Scra Balk 11/3/99 MM 11/3/99 MM ToXI 45-RTS11039-Ser. .k-9, ToxXl 45-P-BSII039-Slppb-9 -t @M1.1/311919/3/U9M9 MX145-RaSI1039-10PPb-9: 11/33//,3999 TCO)XXI&S-RB 11039-25ppb To 165 -RBSSII 39-5 Oppb:99, -t. .MX14,5-RES11039a -LOOppb-91 5-RB 11 39-25OPPb-' L113/9:,Wm 11/3/ 31= 3/19 MM TOX=165-RBSSLL039-SCOPPb-:: . 11.11,13/993cm TToOX145-RBSII039-7SOPPb-9 11/3119 WH XI&S-RAS11039-IOCOPPb-,, M. 11/31,9 um K.On Blank TIOXI&5-RTS-9RO325SN-=/ /kkgg-_DD&yy2299.. 7=15-RTS-:,RO3t2oS69- WX115-RTS- 325?K-S-9/kg-IDAY29- 'TMtx)l&S-RTS-99032SIM-5.9/kg U/kg:DDa&yY22:: Tc)xltS:RTS-9R 3259SH-5 Xl,S RRSI,0039-2 OIPPb-CC", amt. 0D1:1l0o 0-10 PD:l10 11/3/99MM am MOOH 'BSlank TmTooXx)Iia455_--RRaBSSI111003399--BS2.O@-Blbkl-k9-.9.-t-.t. 111/13//39/999 am RTS 1100 39-Stra Slk-9, Oxt. 11/3199 a= T()xl4s-RBSll TC) 39-5ppb-9, "t. 11/3/99 UM WXI&S-RILS1103: -10ppb-9, "t. 11/3/19 N= XIIS-"Sllo03 -25ppb-9 .t. 1 /3/ 'MX145-RELS11 39-SOlppb-9: a=. 111/3/I19, MUIEMS TToOX145-" 11003:-10000b-9, WM. XIIS-RBSSll 3 -250ppb-9. WM. TTooxi45-RaSlIO399-S7coopb-9, axt. X145-RDS110 039 -150ppb-91 Wm. TOX145-RBSII 3 - 00001pk@9, -t. 11/3/ 11/3/:: MN== 11/3/:99 MM 11/3/ am 11/3/99 mm ?"- sta 00= RT 7.189 Standard Standard Standard Stod"d Standard Standard Standard tadard Stad&rd QC Standard Standard tad@rd Sstandard St@-d a tnd@rd t&Rd&rd St--@d Standard 1.00 1.00 1.00 7.171 7.14.3, 7: 7 .1l6o11g 7 1&9 1.00 1.00 1.00 1.000 1. 77.1169 7 126 7 I0 7.LG67 7.1,668 7.1 7.L2 1.00 7 199 7:1 0 7.112 7.187 7.191 1.00 1.000 1.0 1: *00 1 .00 1.00 1 .00 1.00 1 7 IS9O 7:1 3 7 127 7 11,7 7 :.132 7 .1 7.1,1611 7 7..147 7 . 31'&7 7 . 1685 7 1.2 A@ ylw15 bb 1703 bb 208556 bd ll.,O bd 2128616 bbd bb 1 bb 2250 bb 2303 bb 23 9 bb 2114 bb 2021 bkl 2 101 M 24619 bb 2 .1'3 bb 29394 bb 21 bb 2009 bb 2 8 bb 19Sa6s bb 202,9 bb bb 2283436 bb 12432 bb 2117 bb 2280 bbbb 2135 bd 1983 bb C@ %DW 0.01 -99 0.03 -17 0 0 95 1*05 1 01 0 as 1 04 1 07 1 11 0 0::" 0.00 -14 -5 5 -151 4 7 1-1 _,6 -200 0 0. 1 122 0.11 -89 1.02 2 0.913 -7 0 97 1 ot I ot 0 06 1:13 1.00 1.06 0.99 0.92 -3 a -14 3L 3' 0 -1 -4 Omp 020119: 0'--titated and Priut*d bY I" 11/08/99 gu=tity CalLbratim T=45-"Ylg @tmi "PoAnd aox._ 11/3/99 ompound 1 name:POAA (Chl) Response Factor:57.5599 Response type:ExternalStd,Area Curve type:RF 87.0- ra1g. x x x ResponsL- x x x boup020129: 0.0 CA---titatod 0 .1 and pri=ed 0.2 0.3 by i@ m 11/09/99 0.4 0.5 0 .6 0 .7 0.8 0.9 Conc 1.0 CA-tify Calikwati= lands-day2gt @tml P@PO@ and do*._ .. 11/3,99 Compound 2 name:PFOS (Ch2) Coefficienotf Determination:0.999549 Calibratiocnurve:29.3773 * x + 191.305 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:I/x,Axis trans:None x 2.92e4- x Response- nv-T@- 0.0 soup020199: Q@tit&tsd i- 200.0 mbd PWiDtOd by I" m 406.0 600.0 800.6' Conc Q@t icy C&IL@ati@ ?C=45-"y29 @t@l and ".0- @. 1113199 Compound 3 name: PFOSA (Ch3) Coefficienotf Determination0:.999708 Calibratiocnurve:241.363 * x + 800.807 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:I/x,Axistrans:None 2.37e5- x Response@ 0.0 .... 2~ 020199: Ch@tit&tod and Vrinte4 by i@ m 11/08/99 Conc 806 T=45-dAY29 @d d...- -. 1113/99 Compound4name:Surr(Ch4) Response Factor:2157.29 Response type:ExternalStd,Area Curve type:RF x 2.43e3- x x x xx x x Response- 0-1 0.0 g-, 020192: g@_ti.&td 0.1 0.2 " @in@.d by L&. 0.3 11/06/99 0.4 0.5 0.6 0.7 0.8- 0.9 Conc 1.0 @@h.d xL..tShtod f@'e: me. -.ad: C..Po..e, Print*d C: \M;@ 10599b.." CT 37A:CCUi;::3C320119999-9p@.\@@thoa\l 03 ;7:2):54 1999 Co@p.@.d lot .... 1 ou ntify Trace: co:c. of S@ndards: U :r ",V lue: U: @ p. k Factor: In-earate '9,-ndow !'.@t.r Chl-tO'.f- :Chl) I.CQ0C300. 1.0 C]OO Di..bld R iv RT ReferrTi.. Wi (-i-) Peak Se-ectiOn: T7Pe: "::plll:@ rolynomi&l TYPO: Proint of Crigin: it aWeTi hring: AX; g u.its; P.Ak-to-7-%k S=Oth Window mum@r s--e (sc@s): c- @m'oths: 2,. Linear Ex--'-ude ilx *Icre ad I il@.9: ,t*duc' p-@ Z' Dra,ec@ver-.zcal thr.&n.'-z! D esh@,-.Ider @hreshold: Re',atlv: kb@olut Ab.011-- ght: t " 9 Ir..;t: r--; 90.c: 'ad 30.c: Di:.bled 1,..bl:l Di bl d :)i bl A Method R, Method f@@.: Last modi@.ied: CMV .. d: C:\n:.ZsLrrc@.szu;3@'3199.p@.%M.,hIDB\IlOS99b..db M., ::z@ 03 C7;-.i:@3 1999 2: P-:5 (Ch-: 08 :7;25:54 1999 C o Ad N- : lon@p.r:@l Ref.: 0 ..tify conc. of standard.; U :r RreFalVal@ea*ctor@ CIhn@t_etg.r@&t. do. P-5s"ch2) T"@C C.- - A Disabl*d T Ti-Pea'tSelection: .:p- n@. ':',-pe: R. p... 7 ED.@@.b.lbldd ::::n@ 3.5:: ' .@trn.1 lpolynmi.1 71pe poi f Or@zi.: ,it IwteIi@ht; -.g: Axis rra.@.'- @atior: units: S.@ Window sl:e (sc&n-): U@ert inogf s7o S-- h hotd@hS: J'toinc valley tirIeshold: ;:d . @, iule p < @ - ing@ Dra,, DSehculder @Ieshold@ Relati" -@;@t: JReLlb.t1@@.e Abso,@ute @rea: @n,tied 2 I :00 2.OC Di:abl:d Di..bl d Di bl:d Di..bl d Page 2 :thod :*Port 'hod il.: ft..t.d: C: Mon 1:,@ 08 0710@:SS 1999 3: PFZSA iC'%3: Mon 1:@v 08 C7;2@:54 1999 AthDg\llOS99b.odb C..pou.d 4...t Inter" (Nancify conc. Of t -.1@;ards: U or RY V&Iud: U:or P*ak ractor: Intelr. te *@ ow Fsct.@: Rate..ti n Time (mi@-') Rel tiv. Ptt'-tntlC- -r. RT Reference. Ti@ Wi@-'Ow (mins): peak Sel.cticn: p@o:AI(Ch3) C. ... a .Gooooo0, 0^. 0 2.00 1I..0o0C'zo. Di..bld E, (::cn.3 .463 I ad bld 2:,ter..l Ar.ft4 polyn..ial rine: Point f,..Cri;@n: Pit Weig :4@.;: Axis Trarzlr-t@.n: E.@.ude 1 Smot ir.-; windowh s@ze (scans); r of smzzth' Us.m-obtet, r,, i in V.Ile,/ R:duce pe-@@ Raise be. @.c, Do Sh. z_ . .12 h. ld: R. )Lbi.l.@'i.vut: -,.!:ad 2 !:.c3 .0 10 a !3, oi:.bled mi abld Di:&bl-A Di @bld Page 3 X.@h@d X.th.d file: L..t -d,!,.d Compound: Printed: C;\M;,SSLYNX\3:.L.-:0199,pro\imtbDS\110599b..ft "on :;ov 08 07;..-@ss 1999 t: S@r@ (Ch4@ 08 07i:?:St 1999 Comp.@:d Xater QU&ntify Conc. f @:e@e - Tr:ce: S@ @d.@cl.: U or RP Value; U:er Peak FaC-or: Integratte Winto" Factor cb.- 1 tifvre@_ @tent@on IT A* T- -i,.d., peak Selection@ TLmo 3-@rr (Ch4) (::Z... .C:Iaoo, Dis&bld En..bl*d ":Pon:: R. po n 7,lpe: 1poly.-i.1 7-1p.: Point of Ori7in: Fit Weig Ai. Tr--.I-.L-".n !;@ne re.k@t.-p..k -plit-d-: S-.th:ng. Wind@ Bze lsc&ns) NSwu@mtber of s'aoths@ 1-.ing 7@tr..d: 1 in vall.=3t0 -i bp.@ t;ire@h.1d: Dra@,ct e .r.: DSh*ot,id.@ "7 - :..e hold: Rel3t'vc,e Ab a @l@ R* lllvt: Ab! I ':ight@ @gh@; -::: r -ad z.@;, Disaabl:d Di .:bl d Disab ad Di blld QuattroU, #6414E SOUP 020199:FACT Equipment Log 99092 PAGE 1/1 DATE: 11-05-99 ANALYST:Ulmh STUDY NLTMBER. T Q2LL45 MATRDC: ratsera DESCRIMON:-da 2@9- di@ FACT Method:ETS-8-5.1 Injectiovnolume: 10 uL Cycle time:10 min. ElectrodeZ:-Spray Mobile Phase: (A)LOMM NIL_4CHa@_02 (B MEOH TN-A- or stndrdnumber (A) 99085-11-15 (B)TN-A-2997 Prepared(date/by): (B)IgaL/99Lah Expires: (A)_94 (B)2010 Storeatroom temp? E or N Other: Guard colunw: None Partnumber: na Lot number: na AnalyticalcoliornnK:eystoneBetasil Size:-x2 50 ffim Type: C 18 Partnumber:055-701-2 Lot number:P9E 11 Sphere size:5 um Serialnumber:0591804Z Analyticaplarameters: Dryinggas(Llhr)3:50 ESI nebulizignags(Uhr)_L3_ Sheathgas(LJhr)-Q- LC Flow rate3:00 uljmin. Back pressure:65 bar RPLC solventgradient:10min-10-95 Time (rnin.) 1)0.00 2)1.00 3)-L.20-4)7.50 5)8.00 %B 10.0 10.0 95.0 95.0 10.0 Tuning Method RePort Method: c:\mAsSLYNX\SOUP020199.pRO\ACQUDB\PFOS3 Printed: Fri Nov 05 15:32:05 1999 Page ms SOURCE ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. NS2 set 1.60 40 5 0.2 150 250 Rdbk 1.60 -60 -6 149 249 Pressures Analyser Vacuum Gas Cell Rdbk 5.le-5 4.le-3 msi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier KS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 14.0 14.0 0.9 0.0 4 650 Rdbk 3 set 14.0 14.0 10 2.0 0.0 40 0 650 Rdbk 42 40 45 saannize @tb" method: L.st modlt,od; Printed; ft-Iact is 10,35.03 1999 Fri aw. as is@31.38 1999 soi@t Delay ( uw rination: I @ at I m@ 0.00 Fair ( zop- Lute. (Cb@ I D.)14 sv&. 0.1t:. :Y Start T@ N(iKmim Rod Ti- ( R" &tSCh;&=el Parent l 413.00 S@s Daughter 169-00 0a -0030 0 00 10.00 I D-11 0.30 (s@s) C-11 a-rgy 30 (ev) Ca15 @2 mu of I K"s P&ir iSnpt_er (ChDa.n1nte@l@ De)la;y s@s 0.0a3 0. 0 Start T@2=d Ti@ ( KiKim 0.00 ILO.00 A.Pe.tcs h@.1 Parent Daughter 11 z..rgy (evi cam Dmll (S@s) Cc V 1 499.00 99.00 0.30 60 rwti- , 3 of I IN.. P&AX f a"- Xnt.rtCh.- 1 De)lay S@@ Sp" ; Start TDi..1.t.(-Kim ) tnd Tim Kim 00 .03 00 0 00 10.00 R.Pe.t. Channel Parent Daughter D@ll (S@6) C-11 It-Orgy IOV) Com v 1 498.00 70.00 0.30 45 60 vuwti- : 4 or 1 39-. F"C (zov- I t.@ Channel Dl.Y S= ( Dalto" ) : Start Ti.W '(tMii-Rod Ti- ( S-CS o.@o.,0 0..00.0.. Rep*atCh:@*1 Parent Daughter Dmll (s@s) Coll R"ruy (.V) C..* V 1 427.00 80-00 0.10 do 60 Masslynx - Sample List Sample Ust:C:\MASSLyNX\Soupo2ol gg.pm@SampleDB\l 10599b.@PL Printed:FriNov 05 15:26:201999 Page 1 Page Position(:1,1) FileName FileText MS File 1 110599028 MEOH Blank 1OMIN-PFOS-POAA-PFOSA-IS 2 110599029 MEOH Blank MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 3 110599030 4 110599031 TOX145-RBS1 1039-H20 Bik-9,ext.1lrwS9 MCH 10MIN-PFOS-POAA-PFOSA-IS 5 110599032 TOX145-RBS1 1039-Sera Sik-9,ext.11/3/99MCH TOXI 45-RTS1 1039-Sera Blk-9,ext.11/3199MCH 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 6 110599033 7 110599034 TOX145-RBS11039-5ppb-9, ext.11/3/99MCH 1OMIN-PFOS-POAA-PFOSA-IS 8 110599035 TOX145-RBSI 1039-1Oppb-9,ext.11/3199MCH 10MIN-PFOS-POAA-PFOSA-IS 9 110599036 TOX145-RBS11039-25ppb-9, ext.11/3f99MCH 10MIN-PFOS-POAA-PFOSA-IS 10 110599037 TOX145-RBS1 1039-50ppb-9,exL 11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 11 110599038 TOX1 45-RBSI 1039-100ppb-9, ext.11/3/99MCH TOXI 45-RBS 11039-250ppb-9,ext.11lWg MCH IOMIN-PFOS-POAA-PFOSA-IS IOMIN-PFOS-POAA-PFOSA-IS 12 110599039 13 110599040 TOX145-RBS1 1039-500ppb-9,ext.11/3/99MCH IOMIN-PFOS-POAA-PFOSA-IS 14 110599041 TOXI 45-RBS1 1039-750ppb-9,exL 11/3/99MCH IOMIN-PFOS-POAA-PFOSA-IS 15 110599042 TOX145-RBS11039-1000ppb-9, ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 16 110599043 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 17 110599044 TOX145-RTS-9RO3255M-5mgtkg-Day29, D:10 10MIN-PFOS-POAA-PFOSA-IS 18 110599045 TOX1 45-RTS-9RO3256M-5mgtkg-Day2g, D:l0 10MIN-PFOS-POAA-PFOSA-IS 19 110599046 TOX1 45-RTS-9RO3257M-Smgtkg-Day29, D:l0 IOMIN-PFOS-POAA-PFOSA-IS 20 110599047 TOX145-RTS_9RO3258M-Smgtkg-Day29, D:10 10MIN-PFOS-POAA-PFOSA-IS 21 110599048 TOX145-RTS_9RO3259M-5mg(kg-Day29, D:10 10MIN-PFOS-POAA-PFOSA-IS 22 110599049 TOX1 45-RBS1 1039-250ppb-CCV9, ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 23 110599050 MEOH Blank 1OMIN-PFOS-POAA-PFOSA-IS 24 110599051 TOX145-RBS1 1039-H20 Bik-9,ext.11/3199MCH IOMIN-PFOS-POAA-PFOSA-IS 25 110599052 TOX1 45-RBS1 1039-Sera Bik-9,ext.11/3/99MCH IOMIN-PFOS-POAA-PFOSA-IS 26 110599053 TOX145-RTS1 1039-Sera Bik-9,ext.11/3t99MCH 1OMIN-PFOS-POAA-PFOSA-IS 27 110599054 TOXI 45-RBS1 1039-5ppb-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 28 110599055 TOX145-RBS1 1039-10ppb-9,ext.11/3/99MCH 1OMIN-PFOS-POAA-PFOSA-IS 29 110599056 TOX145-RBSI 1039-25ppb-9,ext.1113199MCH IOMIN-PFOS-POAA-PFOSA-IS 30 110599057 TOX145-RBS1 1039-50ppb-9,ext.11/3199MCH 1OMIN-PFOS-POAA-PFOSA-IS 31 110599058 TOX145-RBS11039-100ppb-9, ext.11/3/99MCH IOMIN-PFOS-POAA-PFOSA-IS 32 110599059 TOX145-RBS1 1039-250ppb-9,ext.11/3199MCH 1OMIN-PFOS-POAA-PFOSA-IS 33 110599060 TOX145-RBS1 1039-500ppb-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 34 110599061 TOX145-RBS1 1039-750ppb-9,ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS 35 110599062 TOX1 45-RBS1 1039-1000ppb-9, ext.11/3/99MCH 10MIN-PFOS-POAA-PFOSA-IS InletFile 10min-10-95 10min-lG-95 10min-lG-95 lomin-10-95 10min-10-95 10min-10-95 10min-10-95 lomin-lG-95 10min-10-95 10min-10-95 10min-10-95 10min-lG-95 lomin-10-95 10min-10-95 10min-10-95 10min-lG-95 10min-10-95 10min-10-95 10min-10-95 lomin-10-95 lomin-10-95 1Omin-1 0-95 10min-10-95 lomin-10-95 1Omin-1 0-95 lomin-10-95 10min-10-95 1Omin-1 D-95 lomin-10-95 10min-10-95 10min-10-95 10min-10-95 lomin-10-95 lomin-10-95 10min-10-95 FACT: DA'I'AUVIEW SUNINIARY FOPINI @@selio1v Data Rcview Sign-Off I)alaAnalyit: @rA6 FACT StudyN: -ro,4 Matrix/Timcpoints: SamplLeig; 1015'ffo- Set-upAnalysis Datr/Aradyst Instniment: C5 A..Iyte':FC,4(Ael;i AcceptLaibnleRaarnge- LOQ: NA R^2: IVA @e&P- ExtracBtWi&on Matrix BlaniL R-4 CalibratioCnhecks: MSIMSD: %IA A,, Data Status: AnalystReview NamcIDate. ;@*s Technical Review Dt,: QualitAyssurancReeview Nwnc /Date: DotsIntry-- @A (1, LLL2 I-La Comments IJustincations: 0 4@- tl -13t_ Anslyte: ?Fos ecqz AcceptablLeinearRangc: LOQ: pi, :5-,--70 ExtracteBdlank.le.,-,2@- /-.2 R@2: matrix BiniL -Lr -k. CalibrationChock3: OAC MSIMSD: Data Status: C)k @-n4ttA !@,gDLlu@bnjnf-,Apl Pot I?,:Z:V II PZl lels 'IlLt-#Ce IDQ. 6L -L- Ae 171WAt--Skac.)-ILS Analyte: prSA (-CH3) Acceptable Linear Range: LOQ: /,7 ExtractedBlank: Ck R@2: MatrixBlank. CalibratioCnhecks: MSIMSD: Data Satus: E(N@xcA LAC, ,@P,,09AA@,iU,@Itgedfn IDI:Il@gi "Of ye@A'ci 2@r /* t i KA4 e- k4L (olig III FACT: DA'I'AREVIEW SUNIINIARY FORINI I)aLaAnalyst: s- FACT Study 7.-), MatrixiTimepoints: ZJLV;-, AIL4, Ae Sample List: lg>t"@'f3@4.- Set-upAnalysis Date/Analyst r@- f --as- Instniment Z. Data Revicw Sign-Off AnalystReview Name/ Date: rks "-Ilr&2 TechnicalRe Name /Date: h@r Quahty Assurance Review Name IDate: 4-,o a Alp- u Data Entry: !D/Jilq@ Comments Justifleations: Analyft: --rs ("-Arf)o AcceptableLinearRanp: IIA LOQ. IfA R^2: Af* CalibratioCnhecks: MS/MSD,. Data Status: Exbwbon Bla& 1/4& Matrix BWnic Anslyte: AcccptibleLinearRange: LOQ: R^2: CahbralionChecks: ExtractedBlank.Matnx BLU& fl , 7ew.L- #ids- L) 1,@,,e.1 to/.211i DataSftwr Analyte: AcceptableLinearRange: LOQ: R^2: CalibrafiCon ks: NiLstaNvims Da atus7 ExtractedBlank: Matrix Blank: IPV,4AA4PrA 61-ox lrj Al;@,ns4 t")Aoo!a@,- 4.j6 O=.-tif5y4 rat "Y I a 4, @t", &.a do..- -t. 10/13/99 sample Listti:ed : Lee. Ddi No. Ot 10 06:42:08 1999 i"fattbod: t modified: mm oct IS 06z&1:21 , 99 Job Cd.: @i.@.d: M. @t to 09:20:02 1299 compound 1: PC" (Cbl) 0 02 101595900(2, 3 101 99 03 A 101599004 5 101599005 6 101599006 7 101599007 a 101599008 1 9 10159:0009 0 1 0 10159 1 1 1 1015990910, 2 2 10159 1 13 101359:013 1 101 14 15 101599015 16 101159:01.6 7 1789 10,1595901081 1 0 10 155999019 2 10 9020 21 1015990201 22 10015:99022 23 1 015 990 23 24 1 15 24 25 11 015990205 26 1 01599990 26 27 015 27 28 101599028 29 1011599029 30 10 1599030 31 10 599031 3 2 1015990932 33 34 11001155999030433 3: 101599030536 33 7 101,99037 389 10159:003: 10159 3 40 101599040 1 1015;9041 4 2 1015 9042 , 3 11 01599043 99014 4 4 015 1,65 11 015:9909&0546 4 7 1 015 9 9047 ,g1 111 9 1041g S5o 10o1i5s9909500 51 10159;051 2 10159 052 53 10159:053 54 10159 9 OSA 5: 10159 OSS 57 110011:9990905567 a lols99058 5 9 101599059 601 110011559999006601 :2 101599062 3 101599063 :4 101599064 T@ HaE-O1HpillIl&*Mkt MKOOHOH Blank 70 45Blank L1013:-920 Blank-Li s MXXlds:5. R"BLIG13 -Li"r gl@Ak-li 'M 45, REL10139-5 b-11. 319 Toy'1 I RBL10139-1 pppp TOXX.1l&5. RBL10139-25 Opp b:llll:SZEZ TOXI&S RDLIO139-soppb-11, SRS TOX145: RBL1013 100plpb-ii. SRI TTOIXOI&S, RBL10013:-92-So Oppb-ii. sn XI 5 RBLI 13 - Oppb -11 Toxi 5. RDLI0139-750ppb- 1 TIO & 5. RBLI0139-1000ppb-11. 1 SZE M.0X914 Blank MXJ1&4S5: TOXJ&5. TOX145, MX145. ItTL-9RO3230M, L-:RRO3231H RTL- 03232M: RTL-9RO3233M. RTL-9R01323&M. Dyl, Dyl: DYI DDyyll., ContMic ntml- CC=-tt="ll_- SZZ SIZ SM SS=ZZ 10/13/99 10/13/99 10/13111 I10C//1L33/ /;: TOX145 5 _kRBL10 31-250ppb-CCV-11-1. S= K.OH i TOxl&S 70 45: TIOXXl145. TOX145. TMOXX114455 R'TtL-9_Rg0R3235M TL _ 03236M: R L 9R03237K. RTL-9RO323&X. RB-L-9R03239K. DY : cmtmlDDYy4&4, cC@o.@tl=_%- DY4: DY& C.U@lC-.tr-l- szz sSzIzR SZE SEE 10/13/9: I10//113 3/ 11001,131:: 13/ Bl: ank L10139-250ppb-CCV-11-2. SXS MOOH TToaxi4s: 9R.132331 X145 . 032 lyl: Cont@01-2,11.)Vb-us-ll trol-2 pb-MSD-11 -MX145 MM 15: TOX145 S. TOX14 99R03235M. DDyytl, CCocntrol -2509k@NS-12 9RO32]SN. DY4. CO-trol-2509b-KSD-12 RTL-9R0312345M , Dyl. 5=g/ka- SSS 10/13/99 FtBL10 9-25.@pb-CCV-11-3. sxz meox isBl@k Toxi a REL10139-250ppb-CCV-11-3, SZE MeOX'Si-,k RTL-9RO32ifiN. DYI. 5.9/k/g- S T7OXX1145. TOX145, 'MXI 5 TIOX14S. WX145, @TL-9R03247K. RTL-9RO324:.K: RTL_ 9R0324 DYI sw kgI)yl: 5 /kg- Dyl 5:: 5:: SZZ SM RTL-9RO32SOX. DY4. 5-9/kg- RBLI0139-250ppb-CCV-11-4, SitZ S= 10/13/99 10 /13199 100 /13/:9 1 /13/ 9 10/13/99 MT*OCXHI4351a@.k RBLICI 3 9-2509pb -CCV-11 -4. SKS N.OH I..k TmOX145 7VXJX&1S4.5: Toxids TOX145: 1 RTL-9RO3251M. DY4. UM/kg- SEE RRTTLL:::012532,X 0 253 RTL-9RO325@LM. : DY'd sw kg- SZE py : 5.g/kg- S= Dy4. 5.g/kg-$SRZ RBLI0139-250ppb-CCV-11-4. 22 K.OH4,3 5, - =Xl 31 RBL10139-250pipb-CCV-11-4, S= M.OH -k 5 7MVxXl1t& S RBLI01039-Sppb-11, PLBLI (,13:-10ppb-11. SZE SEE MX145 S. TOX14 To ITIlOIXXI145, To 45 . RBLI 0 133, -2$pp 11 RaLl 1 -SOVpbb--ii: 1.sszz, RBLI0139-100ppb-1 I SSE SZZ RBLI0139 -25 Oppb-1 1 RBLI01(319-,30 Oppb-1 I RBL1 0 13 9 -7 S00oppb-1 S92 SIX TOXXII455. RBL1 13 -2 Oppb-11, SZZ 10/131:9 10/13/ 9 10/13/9 9: 10/13/ %we s5 t t Standard Standard tandard st :t_d&rd Standard oc oc oc oc oc oc oc oc Standard s t@ra"d Stta&nodda-rdd SSttandard ,d&ld Sttandard d-rd St' nol LAseA LA S" cme 3tr .1o:*00 0 l0l-*l 1090:00 250.00 ,5000:.00. 5 1000.00 250.00 7 72 7:..0o:: 7..S@ 7 7:.*Ill 7.ogl a 7.091 7:105 70 7 7 7:..O:l 7 092 7 7 :,.4 7 .112 .00 250 '7.079 7.00:7 7:113 7.(,Sl 7 .08 7 7 7.09 50 7 . 110 7 06 250.00 7 .106 77.091 250.00 7.084 7.105 7.104 7.00:7 .00 250 7*.00.6190 7. 250.00 7.036 7.0091 7.(,83 7- 250.00 7*.053 250.00 7.064 ,0".:0o.00 2 55.000 120500.00 500.00 1070500..0000 7.113 7.1090 72 7:.@0.'10 7 .191 7.013 7 .0:7 7 .08: 7 A@ Fle. 0- %D- 41 m 12 klb 12 bb 17 UM 34 M 25 UN 295 xx 2 32 NlKo( 14 xx 34 bb 14 NK 45 NK 33 bb 12 bb 29 NK 229 M 34 bb 24 mmm 54 13 XK 14 m 17 bXb" 25 m 22 3139 bb S6 bb 2& xbbx 24 bb :2 MM 592 mNmK 3 NK 2 2@0 Mmmm 14 m 480 bb 39 bb 3 0 mm 55 m 1 mm 19 mm 12 bb 16 m I1t UK 3 5 mm 2 1 bb 33 M 2 , bb 1 bb 29 NK 950.81 0.000 110- 1 0 709.'7 53 3063.730 5 0.1 343.34 617.9200 -100 274319@ :27 00 37 _I 24 690'12 -00 11 1:905.29 6 .68 0.00 514.8 0 2 2400' 31a -4 17@1.016 14604.0 130 4 0 a0 38 4 0 344 5 249 475 291' 134 3 1520 '3 0 298.9' 50 20 330.57 32 1734.25 1370.02 1,6328.25 11 2 .S83 1_6,3g- 2 4 . 2 -28 0.00 -100 909 32 :37:01 :7.41, @2 3.0 0 00 -100 115.94 -54 2-01. 0 1066.27 S 56.5301 38 S:" 582.57 223 . 33 4986.73 -110707 1 325 033 2113 13 -43 -9560 SOUP020199: Q@tifid and pri"o4 by I" 10/18/99 ou@t tty Compound Bmm@rv Raw*" T=45- cat li@r. day I & 4, @t@l amd does- OWt. 10/13/99 sawl 0 List: : tied Last =Da Ngtbod: tied: L-t -" Job Code: CI%NUSLT=\Soup-rats.vm%mamloca%laistoo Man Oct 14 06:43:08 1999 C. %N"gLyKX\._V-@.ts.p_%Ntb=\10159ta u- 0" is 06.41..21 lsts printed; Man Oct 18 09:20-02 1999 2: pro& (cb2) 01 99001 2 1015 1015990002 34 11 015 9000 3 56 113159900 79 1 1 0 ,01599006 01599007 9 015990 09a 10 1 0 5990 11 lols99010 132 11 001159990011021 1, 101599 13 is I01599014 10 1 17 10 1 S9901716 is 100115:90'1o8 9 19 1 15 991)1 20 1015 20 21 10155:9021 22 101 39 9022 23 1015,9023 24 101 9024 25 11 013;90,25 26 015 026 27 101155::0027 28 10 28 29 1015990g2o9 30 10159 90330 3 1 11 0159 9 903 1 3@ 1 ":11.3'3 34 1 ol 59903 35 1 '1l59903 ' 36 100 159903 5 37 1 1599037 6 38 1 0 1599038 39 1 a 1599039 40 1 0 1599040 41 101599041 42 10IS99042 4"3 11 '0115990043 599 64 45 10a1599045 46 1101159904647 A 7 10 5: 9 0 48 1 0 1 5 9 90 49 9 1 1 1 gg91.,o 5 5so 52' 101599051 11 0011559999005523 3 1 0 1599054 54 5S65 1,001,59:055 1s7a 1 0 1'5:900'5'7 59 1 011599058 9 6'0I 1,00155999900:50 62 11001159909:2 1 13 1 0159 0 3 01599064 Sam :list T@ HOOHI la@k HOOH 331"k X&O l@k ToO x 1,45 Xl ,5:. 'R:"L11'013'9:--L"i r glank- ICXI 5 RaLI013I -Sppb-11. SIX ..ZS. TOXITS, Taxits TTOoX145: RBLI0139-10ppb-11. RBLI01o3l9-925ppb-11 RBL1 3 -50ppb-11: SRI S.,X"Z, TaXx14i5t. s RBL10139-100ppb-11, RBLI013:-210ppb-11: SIR S.I.R. TIOX AS:, RBLIG1a3 , -50 ppb-11 TOX14114'. "Ll .13 9 -7 50ppb-Ili.szz Txi RELI 13 -1.0 Oppb-I six al-J, NIOX"115 TTIoDX145: RTL-:RO3230X RTL- R0333LU: Dyl Dyl: ControlControl- SIR SS IR TOxidS. TIIOOXI 5 Xi": RTL-9R03232M, RTTL-:R.012339 L 3234X: Dyl, DYI Dyl: Controlntt=l- Cc Cc ral- = S3 IR IS Ton&5 RBL10139-250ppb-CCV-11-1. SU 10/13/9: 10 /13/9 100/13/:: 10/13/ 1 /13/99 N.OB Di@.k TO 45 RTL::,R0o323SM: DY4 TOZXII&5: RTL 3236* I)yd: TOX145 TIOX1 4 5 as: TTOCX)IXld$ RTL-9RO.30237M DY 4 tTL-9 323$K: ItTL-:R1O3239mS, Z)yd: I)y4, RBL1 39-2 Oppb-CCV- C..ntral- S Cc tral- SZ"Z Control- SIM Control- SRS Control- SIR 11-2. SIR 10/13/:9 1 /13/ 9 10/13/99 10/13/99 1 /13/99 M.OR 4b5l-k TC)XI . 9RO3230K. Dyl. Cmtrol-2:00pb-KS-ll Tt)Xl&S, 11,1: Tuxid 9RO3230M, Dyl. 9RRO33235M . Dy4. 9 0 23SM, Dy&, Cmtrol-2 pb-KSD-11 Control-250pb-"S-12 Cmtrol-2509b-XSD-12 TIOX145 'MY14': RB RTLL-1091R3O93-23&5S0pKp'k@CCV'-I1'1-35.W'kg- 1 .22. '0/3.3"9 MI@OH &551- SRI Taxi B L10139-25OVpb@CCV-11-3. K.OH i-@"' TOX115, RTL-9R03246X. Dyl SW/kg- SIM TC)Xl45 TOX145: . TOX145 TOXI&S. RTL-:RRO3247M RTL- 9RO03324S9MM:, RTL- 24 ATL-9RO3250K. Dyl:. Dyl , Dyl Dyt, 5M,kg- SM kg Sm ko : SM k,- SIX SRI SIR lzx REL10139-250ppb-CCV-11-4. S NM*XC1H45'Blank 10/13/:9 10/13/99 10/13/99 1 /13/ 9 10/13/99 TOXII5. RBL10139-250ppb-CCV-11-4, SRI M. H Al-k WX145, RTL-:RRO 251M DY4 5.2/,kg- SIR kg- TTlOXXlJ.S1: RTL- '3 SM 5= TCX145, RTL-9.103 -DYy4a, 5.q//k - SIR 5= Tox 145, RTL-9RaOl]0 22SS3&XX: I)y 5m kog - ITBLI 39-250ppb-CCV-11-4. SIX M.OH &5Bl@ TOXI . ROL10139-2SOppb-CCV-11-4. SZE M.0 al-k 1 11,1: . Lll@"l-lppb-1.1i.sax TIDXxl 5 RIBILI 9-10ppb-1 SEE IIOX145. RBL.10139-25ppb@-11: SZE TC)XI45. RBLID139-$Cppb-11 SEE TOX145 5 RBLI0139-100ppb-11: SZE MX14 : RBL10139-2sOppb-11 szz TO 45 TOXXI115: TIDXI&5, "Ll 0139:500ppb-11: KIL10139 75 @Vpb-11 RAL10139-100OVpb-11, S.E.X. SIR 100113//999 1 /13 9 100//13/99 9 1 13/9 -ly Standard tand@d :tand.@d stadard stSt.." @d St -@rd St .d-d .dard Standard oc oc OC oc oc oc oc oc SSttandard d Standard Standard t&od@d Standard Standard S3 tandard t@.d@.d Std 0- 126.13 .30 361(l.70 030 123'-00 161.37:00 920.0 0 0 1227.00 307.00 .00 307 - 307.00 307.00 307.00 .00 307 307.00 307.00 6..1330 1320.70 61..3000 123 307.0000 613.00 . 00 122270. 7.31a5r 7.242 7 2535 7:2 3 7 27 7.250 3 7.24 3 7 241 7:23, 7 242 7.25 7 2405 7.2 7 . 2156 7 . 2 AS2 7. 7 272 7.27S2o 7.2 7 2 73 7 2451 7:.2 45 7.2 7 .224016 7.295 7 .2 7. 71' 7 . 2247 271 77..254.9 72 7.23207 7 . 2 AS 7 .2 29 7 7.2273 7.245 7.295 7 2,4 7.2S& 7.2 290 7 .2-13 77..231 7 .297 7 247 7 so 7..2243"1 7 7. ' 5. 7..2228 7 . 2492, 72 7.24781 7,275 7,251 7*2 So 7,2 7,227 7.229 7 251 7:.229 7 .227 7 226 2 A@ 27 14 31 59 71 bb'g bb mm UK 7,55 Mmmx is 5 mmx 5 mm 254 408 mm 934 bmmb Isis 2347 Mg 2856 bb 175 bbX 37 bb 37 so bb 38 bmb 59 mm 71: bb 14 bb 7 7.:6 MN 14630 bb 73419 bkb 773 MN 742 bb 652 bb 627 43197 bb $0g3o bb mm 732 bd 532 32 bb 6 bb 625'0'1 bb 41315 bb 512 63 bb 169.210 bb 67438 bb 60338 M 7638293781 bbbb 65796708 bb 17S mbmb 6 bb 1 .9611 Mbb"X 169 mmx 221 m 394 bb 836 12613173 bdb 2575 bdm Co.o; 0.00 00 .00 .00 %D., 0 0 0 -100 2 5 0 -71 21 - 3'1 4 66*51 128,32 340 9 690984,3'31 1113 267 -1 9 ,1I 13 -1 34 561 -9 0 00 00 a 000 a 00 0'00 264.2& -14 22.73 0(.100 0 28648,2 21 750 0 00 2S& 48 00 275:1 o MttLI -16 262.8 4 226.6: 17 216.37 345-69 297.13 -6 0.00 25:.Bo -16 .00 22 34,01.31 151 (,:.09 6 2 6572 .801 0 29'*56'3* 242 0 o: -11 2340.98 0 -23 .0 24242 92 29433*790 27716 ct 26424 *5 357 .89 16 31.4.59 244.39 -20 6A 0 00 -100 321.997 -71, 1 lbo C ID it)L) W-SCL 53 *193 122 ' 30. -I6s0 622'81 ]LsOlOOd':5&7 6 -13 --2' 2 -_1I1 a LA@, LAC @AL -i C,.u6( ka- h- LAC-1011?iii Soup 020192: Qa@titiod &ad printed by Lee 10119/99 Qu-tity Co@v@-.d Su--@y "Part TOX14s- rat liwr, day I a &ad do"- @t. 10/13199 O.Mi. List: "at @difie4: n.tl.d: "at modified: co": non O@ C: Oct 18 06:42:08 1999 14 06,41-.21 1929 Oct 14 09:20:02 lggt 2: Pro&& (CIL3) o it- 99001 ,2 3 1015599002 1l0o1lSggggOoOo3& 5 101S 67 110011SS99990000 56 a 101599007 1 599004 9 01599009 10 101599010 11 1011599011 12 10 1599012 13 10 599013 14L is 101101599014 599015 16 @ol 599016 1,7a 101599017 101599018 599019 19 101 599020 2201 l10l1)59l9021 22 101599022 21 1015$9999002243 24 25 101599025 267 10115:90026 2 8 10 IS59 9 27 3 9 10 IS9 90289 2 10 902 30 10IS:90301 31 1015 903 32 IOJS99032 134 1015999033 3 1015 9034 33 5 101599,035 10159 9 036 31 76 10159 go037 10159 38 3'9ao 101599039 41 101599040 1015:9041 ,3 1015 9042 " 1015990434 45 1015990 A ,6 1015599:0045 46 4478 1015990407 ,g 1111:9,.1: 50 1015 & 51 1015999050 1 5S32 11001155999900552 S'L 10155,9053 SS 101159990054 S6 1011559999005556 587 10 15990 57 59 10 58 1599059 60 1001599060 61 1 1599061 62 1599062 63 11001599063 64 101599064 amlii. T@ Blank M.OK KOOH blank MOOH Blank TOX145, ILBLI013 TOoX145 RBLI 399--3L2i0ver Blank-11,SZZS" To Xl:S,: ::LIO013 -Spob- 11. .SSSrEg Taxi 5 L101139-10ppb-11 To X145 Xl&S . TOXI TIOX 5 TOo 1 5 RBL10139-25ppb-11 RBL10139-SO b-11 RBLI0139-IOOPP ppb-11 RILBBLIG139-250ppb-11: 23 :Z"x "': 'I.XI&5, L1013: -55OOVpb -11 L1013 -7 OVpb-11: Me RDLIO139-1000ppb-11. S.". SIZ TMCOxXH14LSs5l:-RRTkTL ::JtR0323ON: DYl: TC) 145, ITTL 0323IN DY1 xl L ::003212:: Dyi: Tatx)i4s. ITTL - 3233 Dyl C nt=l - SZE C-.i- sm co =al- 3= CO.,.I- Szx xits RTL-:RIO1234X, DYI. CMt=l- 9 T'O,Xs1o45: 1 RBLI 39-250ppb-CCV-11-1. SM U T.XiH'S8..-RkTL-9R03235M: I)yA Mxl TIDXJ&S@ RRTTLL-_gj,tto03216M , Dyd 3237M DY4 Cc ntrol- SZE CCo.n.tt@@.011- . :12m2 TOX145,: TOXI 5 RTL-IR0121:.N: _,.0321 I)y COntrOl: Cant a _ SRZ RTL Dy, rI TOXIIS. RBL10139 -250ppb-CCV-11-2. SZZ N.OH Blank 10/13/99 1L.0,13,99; 1 /13/ 10113/:9 10/13/ 9 10/13/99 10111119 10/13/"99 10 IQ /11133/999 TOX145, TOX145, 'MX145, 9RO3230M, Dyl. C.atral-250pb-KS-ll 9RO1230 . Dyl, coutral-250ob-KSD-11 9RO 323S:, Dy4. Control-250pb-05 -12 Tax 45 R0323$K. DY4. Control-25OPb--12 Tloxll4LS: 9RTL-gR032415M. Dyl, SM/kg- Szlt 10/13/99 TOX145, RBLI0139-250ppb-CCV-11-3. SEX HEOH 45blank TOXI a . MEOH 1 7TVoX114455 x: TCO)XIAS X145: TOXIAS. TOX145, REL10139-250ppb-CCV-11-3. SZX RTL-_9gRRO323:6M t)yl Sw/tkg- L 0 2 7M: Dyl: Sag kg- S ZX 324&N Dyl SM/k/ = 1I.TTLL--::003249M: Dyl: 5M /kg- SM R'rL-9RO32SON, Dy4. 5me kg- RBLI0139-25OVpb-CCV-11-4, SZE 100/13/99 1 /13/99 100 /13/999 1a//13/ 9: I 13/ HEOH 45Blank TOX1 , RBLI0139-250ppb-CCV-11-4, SNE NeOm 'SBlank IX14,: RTL-1.@ 321., Toxi RTL-9Ro3252M. TO RR TL-9R 3253m, TOXX114"5 : TL-9R003254K. Dyt, 5w@kgz)y4.Sg/kg- DY4, 5m/kgDY4. Sm/k 'MX145, RSE.10139-250ppb-CCV-11-4@l SSZ.B2 S. szz SXZ 100/13/99 10/13/99 10/13/999 1 13/ 9 M.OH 'S31" TOXI . RBLI0139-250ppb-CCV-11-4, SZE MeO Blank TOX145, TOX1 : 7VX115,5 Toxids TOX145 Wxlts TTIcD)XxJl4&5S. WX RR BL10139-Sppb-il , 52 :Ll0139-10ppb-li1 . :IM R L10139-2 Sppb-I KE RaLlOI19-5 RDL10139-1*O1v-p"bi-.I,:,. ARDBLI013:-250ppb-ii RS L1013 9 -'aDVpb-11 . S KI L1013 710ppb -11 as 145. ABLIO139-1000ypb-11. SZE T"o St,@,rd s5tandard tandard t.@,@d :tandard St ---rd Standard tand"d :tandard OC oc QC oc oc oc oc oc Standard SS tandard St@-@@m-r@dd -@ @d SS tandard tandard stodrd Standard ftd 0=0 6.14 12.40 12 00 11-1.00 62* :00 30'7 61&.Oo 12921.00 0 29. 0 307.00 307.00 - 107.00 307.00 307.00 307.00 .00 307 307.00 16.14 . 3 2 '00o 6 21 ,* 00 12 361.7*000. 4. 129281.00 7. JtT 269 7.83 7.796 7.801 7.7:63 7.7 7:71*21 7.89a 7.804 7 7 .1 7 7 .880413), 7. 7 $to 7.:352 7. 3 7::331 71 7.$13 7.:13 7. 74 7 :24 7: 33 7.807 7.357 7.:33 7.8059 7. 5 7.213 7.813 7.:it 7.a 11 7. 07 7.2a13 7. a 537 7. a 0 7 7. 5 7.806 7 7::01,3 7.811 7.857 7.1:2 7.8 1 7.:10 7. 79 7.:16 7..016 7 7 :.769020 7 as 4 70 7 :io 7: 79 7.78361 '7 .19'0 7,789 1::13 7 7.792 7.:1120 71 177 bdwe 339 bb 178 NK 11459 mm .51 No 522 3U0Ka 14165 mm 22 73 M 43693 10 M 2056: 26902 31M 35703 Ma 166 M" 147 M lis m 2.27 M 1407 MM 8210253 MUK 10 mm 277 NK 1&7 M 77671 db 2 NK $I35.3 227.123 KH m 10526 nu 9524 NK 7892 NK 14738'9a M( 73682 db 0 156 NK 7941 NK 138 N" 176413 mdmd 153273 dd 156909 kb 160 752 db a93 NK 752809 M 2 NK 7441 M 172 NK 663106 bb 73 9 dd 6.9246.,. 7 7269121 bMb 2 mm 7&4s8o M 1" NK 351 I= @4'67 "K 2205 MmmN 1 4116 NK o.il 1 65 m 25247 OU 35385 mm c@ %D- 0.0 0.00 0-*0 . . 39.-700a -40 .1 -21 39.36 24 t-4 @,''922.:7"9 -1 308 6#1056-.1306 0 . 77 _1132 10720.065 0.0 0 0.000 *.:o*o 0.00 241 -21 o:'oO' 35 a-, 23&2.* '2,w 4:62 0.00 243.307 -21 11 0:0,2 282 .712 2321. 3 217.22 12454.76 47.241 \)ttA -19 2330.'9020 -24 0.00 5323.21-\ 4621.70 1731.S7@ 4854.396.@. 22.1 223.216 -27 0.1 21:.790 -29 .0 1997.35-\ 2214.16 2'0o17--@ 2 2140.-2': -10 lc)c) 2190'39: -28 0*00 !1:07 -17 10a.64 -14 3 33 242 60 61 - :4 10J.:@ '1 2 4756.7: -11 1063.05 -13 0,11 LA 101 L4c htlw ,,rZO LU- g-W7 Soup 020199: Qa@tified =A printed by L@ 10/18/99 T=45- Cmwowad sum"" Report rat li@r, day I & 4, OCR@L and 6000- WM- 10/13199 Samlo List: Last modified: O..*attbodm:odified: Job Cod.: Mon Oct 18 06142:08 C:%KLBSLYNX%@p-"Cs.swo% Mon Ocz IS 06:41:21 1999 1919 @i.@.d: @ 0- It 09;20:02 1119 compound 4: Xs (ch4) 1 @.@5 2 10159:90002 1 10 is 03 4 101599004 5 1015599005 6 101 5 99006 7 10115:9007 8 10 9008 9 101599009 10 IOLS99010 11 101599011 12 1015:99012 13 1015 13 14 101599014 5 101599015 16 101599016 17 101599017 18 101599018 9 101599019 I201 1l0o1I5S9999002201 223 101599022 101599023 24 101599024 25 101599025 267 101599026 2 a 110011559999002278 2 9 101599029 2 0 101599030 31 101599031 32 1015990323 33 3 34 1101155999034 3: 1001599035 37 10159,90336 7 338 11011559990038 39 1015:9039 40 10015 990040 &412 101155999042Ll 3 101599043 44 lol599044 45 1015999045 46 1015 9 9046 47 1015 9047 48 1015990,489 49 1 15990 so IDIS999050 51 1015999051 52 loll 052 53, IQ015:9053 5 5 10 15990054 5 6 11001I5S9999005565 57a 1 0 15 9990 57 5 1 is S8 59 101599059 60 101599060 61 101599061 62 101599062 63 101599063 64 101599064 ga"pl:lil T@ H&CH 1=k K.CH blank X&OH Blank Tcxl&s R L1013::H2 .Blank RBBL1013 LLOv r 31&Mk-ii' 323 IT'OCX145, RBLIO,31-5ppb-11 st ToOXI&S. RBLI0139-loppb-li,1. SSEEEE ,oX1445: R :LI0139:25PP -1 xi 5 L10139 SOPP b IICX145, ROL10139-1.@ k'bl'i 5, RBL10139-2509pb -1 TIO"XX11&45. RZL10139-SOOPPb-ll-.11: SSSZEEEEE T'OMX145 Rt:LlO1l39-750 b-11 X145: LIO 39-100107ppvb-ii, SEE H.OH Blank TO 111&55 TO-1 : 45. TOX1 'ToMX145, X145 RT L -:RD323am RTL- R03231M: RTL-9RO.1.232K : TL- 3233X RT -091R3O323&M. Dyl: C. tv.1 SZE I)yl control := Dyl: Cn=01- 92 Pyl Control- Sn Dyl, Co@t"l- SM MX145: RBLL1 9-250ppb-CCV-11-1. SXZ 10113/,99 3.00/23/ 1 /13/99 10/13/ 9 10/13/ 9 HT&cCXH145BlanRkTL-9ROs3o235H Toxi 4'S5.: RT L-9 3236M vya: Control- SIM l)y4 control- SEE zi TTOoX145 tTt,-91L03237X. VY C n@l- SXR :TL -9R03238M. DY,,: C: ntml- SU TOXX2I,I5S.: TLi9RO 3239K. DY4, Con I- En blaRnBkL 0139-2 50ppb-CCV-11-2t.@a SZZ 10/13/11 10/13/:: 11,0,/13/ 113/99 10/13/99 X.Oz TOXI"S: 9RO323ON 9RO323=: DYL Cont..1-2509b-KS-ll DYI Control-25OVb-MSD-11 TOX145. 9RO3235X, Dyt, Con@1-250pb-MS-12 TO 45 9R 323SX. Dy4, Control-2k5g0_pb-SKRSID-l12o/ TOXXII45: RTOL-9RO324SK. Dyl. SM/ 13/99 Taxids L10139-250ppb-CCV-11-3, SM X.CH i _, @', I'CX!4a5. RBLI0139-250ppb-CCV-11-1. SEE XECH Blank TOX145. RTL::,t.... 7,m 'MXl145"- RRTTL _gR,0124 RT L _gR 0324 TTCCYX@L145. L 0324,.: Dyl: 5,g,, Dyl 5.9 kg- SRS 5m/kg- Sax Dvyyll: s.9/10- sSzMz TCX:4,5: ItTI.-I,RIIII*ID.Y4.,_151W_/"kg- S. TCXI 5 ILBLIG 3 -2 @Oppb- H-CH Blank TC 45, RBL10139-2SOppb-CCV-11-4, SM @Lol@3,11 10/13/99 10/13/9: 10/13/ I'9ll ..CH Blank TC 145, RTL -gRD325LK. DY4 TIOXXII5. RTL-9RO3252M. Dy4: TOX145. RTL-9RgR32353 K: TCXI 5, RTL-9 0 254 Dy4 ICX145. RBLIO'39-250ppb-CCV- 5.gj,kg- S SM kg- SZ. S 5.l9l_ke- 32 4. SZE 10/13/99 10/13/9: 10,13/:g 1 13/ M.OH alk SEE Toxi45 ItIL10139-250ppb-CCV-11-4. K.CK TOX14S P.BL10139-Sppb-11, SEE TIOXIA4S:, RSL 0139-10ppb 11, SIR TC 5 RILlOI39-2 Slppb:ll, SEE TCX145. R.B.LL1J1011331,-_1100ppb-11, SEE '.X)lall. 1 Oplpb-11 Tioxi45 To R:L 013;-250ppb-11: XI&S : R L11 013 -500ppb-ii SSE TOXI&S. RELIO139-7$Oppb- 11 : ZZ TOX145, RBLIG139-1000VPb-ii, SZE T"e std c@ RT Standard stnd@d Standard Standard S-d t&ra&rd sstta-n,d,a-rdd S@ @@d OC QC oc oc OC oc OC oc standard tandard Standard Standard &Dd@d 5Slt d tandard SS.ttandard d 1 00 1:00 1.00 1.00 1:.0 1 .00 1 1:.*0 10 7,067 7.00:1 7. 3 7.099 7.00 9: 7- 0:, 7-.., 7*078 7,064 7 7:.79 7:.*71 7 8@ 7:.0:2 73 7-0:3 7. A 7.0:5 7. 2 7:017 1@ 1.00 77 ..:2 7.079 J... 7.083 7.082 7.086 7.082 7-00748 7. 8 1.00 1.00 7.100 7.100 7.0099 7.0:3 7.081 7,031 7. 6 1.00 1.00 7.01080 7. 6 7.086 7.0a7 7 7 7 .07 3 1.00 7 .0.S 7.081 1.000 1. 0 1.00 1. 0 1.00 1.00 1.000 1:01. I 7.00:4 7.084 7. as a 7:082 74 7.00:4 7.084 7.0.2 7. 1 Area Flaws c@ %D- 887 bb 1355 bb l@1738 bb 1:75 bd 70 bb 11 6"0.9 bb 13LS6S5J1 bbbb 1, 1 67 bbbb 9 bb 163073 bd 1757 bb 1612 bb 1698 bb 1396 bb 15213 bb 1 9 bb 1435 bb 1439 bb 1466 bb 1417 bb 11924 bb 112&25764 bbbb 11 8 bb 14379A bb 1313 bb 13900, bb 14 bb 13053 bb 141, bb 13835 bb 12 bb 12391 bb 1289 bb 1382 bbbb 14601 bb 134, bb 133 bb 1 253 bbbb 1495 bb 1498, bb 157 15725 bb 151., bb 1 527 bb 1400 bb 1392 bb 0 1 .:. -1-1 0.96 -1-24 1.09 11-.00a, L.06 6 1.07 7 1.01 0.96 -4 1.04 1 1.012 1 2 1. a 4 1.04 A 1.10 10 0.90 10 1.03 3 o.:9 3 7 10.93 7 O.:s 5 0. 2 0.97 -3 *.17 2 -1 2 0 779 23 0 96 -4 0.'89 11 0.35 -15 o.:o -10 0.a1 --9 0 9 5 15 92 _-80 0 ..-.Ia -2I0 I0 ..Ilo_ -21 0a,*5g4o 1-016 0 0.95 -1-5 0.:7 -13 0.0 7 -11 . 0 10@90 0.97 :3 01.97 3 02 2 1.:02 2 1.03 3 0.,A -4 11.11, -19 0.90 -10 C, Aar@-V &Y)016@t + LA Soup 020199: Q@tified And printed by L" 10/18/11 7' 1 au"tit C-libr ti@ Row@ "ii4s-yrat liv:@, day I & 4, cmt"l And dDs*- @t. 10/131FS9 Compound I name: POAA (Chl) Coefficientof Determination:89334.567901 Calibratiocnurve:0.0264689 - x + 15.6723 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:ltx,Axistmns: None 42.1- Response- x x x x x x x ol 0.0 Soup 020199: Q@titiod 200.0 and printed by I" LO/18/92 400.0 600.0 800.0 Conc 1000.0 QU@tity T=45- ca4ibrati@ sepom rat ii"r, day 1 & 4, @@l &ad Compoun2dname:PFOS(Ch2) Coefficienotf Determination0:.983941 Calibratiocnurve:2.48521 *x + 89.0578 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:1/x,Axistrans:None 3.14e3- P.g. 2 Response- x x x 0.0 Soup 020199: Q@tilled 200.0 400.0 and printed bY 1" 10/19/99 600.0 Bon n 1000.0 Conc 12O00L.O0.--i ou@-le caii@&tL" "P@ TOX145-yrat li@." dy I & 4, @t-J. d".- @. 10/13/99 Compound3 name:PFOSA(Ch3) Coefficienotf Determination0:.999594 Calibratiocnurve:33.0992 - x + 198.731 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:I/x,Axistrans:None 4.08e4- P.O. 3 Response- 0.0 e@v 020199; 0-@tified 206.'0' 400.0 &ad VCLZMed b3r 1" 10118/99 600.0 800.0 . . . . . .10. 0.0 Conc 1200.0 QU=tify calibrati= ROP@ TO=45- rat li@. "Y I & 4, Compound 4 name: IS (Ch4) Response Factor:1542.30 Response type:ExternalStd,Area Curve type:RF x 1.67e3- x x Response- nv-i0.0 Smp 0201999 Q@titiod ol .1 O@2 O@3 and Printed bY L" 10118/99 ol .4 0'5 O@6 0 Conc 0!7 0'8 .9 i.o x.thca Report tthod file: .t modifid compound: iprijited; C: \MASSLyNX\Soup-r&ts.prO\M*thDa\loiSS9...db Ron Oc- 18 06:&1121 1999 1: POAA (Chi) Non Oct is 07:&6:51 1999 Compound K@ lot.@ I Rf.: Q,tity Tracei C@ , of Sta""da: U or R? Volue: U:or Peak Pactor: Inteqr&ce Wind@ Factor@ cbx@togr= @.s wind@ POAA (CIII) IN.'el TIC C@-. A 11..000000000000, Disbi-d 2i..0.000.. ::t-tic. Tim (.i-) lative Retention Time RT Re for@ 0: Time Wind- ii") P"k Selection: 7.12 anbld o.oo,.: Di.@bld IN*n5e,l 0.3 N.@.st Re.go-. TYP-; R.Op@., Polynmial Type: Point of Origin: ,it Weighting; Axis Tr@fO@tion: ibt r-I Line Z=Iud. I/X N.- units: P.ak-to-peak &Mlitud*: S@ thig: viad@ six@ lac@ Nuub.r f @tho: Sm@tkiing method; Join @.1l.Y threshold: Reduce p.'k t iling: R.i.. ba..li.: @..i Dro. v*rtical threshold: D.t@t shoulders: Shoulder threshold; Relative b.ight: Absolute height; R.1-ti- "..: Absolute @OA: 66 Zn&bl*d 30.00 200.00 5.00 90.00 I3 )isabled 0.00 1.50 D :.b d 0.00: Dii &blld 2.*.0: Di:.b".d 0. Di bld pog. 1 Method Report Method file: Last odifid: compound: iprinted: C@\MASSLYUX\s@P-rst*'Pro\NothM\101599&.mdb Mon Oct 18 06;41;21 1999 2. PFOS (Cb2) No. o@@ 18 07:46!51 1999 Compound N@ i internal Rf.; Q,tify Trace; C- . of Stand"doz aU: :rr RPeFavkaFlaucet:or; Integrate Mind@ factor: Chr@togr@ mass wind@: PFW in@ TIC c@. I(Cl@2) 11-0..00.0.0D.i0p.b1lad 2:00a00 I oooa Rot RT T- ti*n Tim (-1-) Retention Time WiDd- (-i-) Peak Selection: 7 313: --hl*d O:Ooo, Dis&bld 0.400 N.-..t Response Type: Response: Ar- polynmial Type: point of origin: Fit weighting: A.im W@fc@tiOD: Lilwlude I/X A.- P..k-to-p..k Mlit." 2@ ing: Wi.d@t i.. (.C-): WA.b.r of @*th.: S@ttLing method; join Valley threshold: Reduce peak t ilidg: : Raise b...li@: @mwi@m w v rti &l threshold; oDr.tecte.hoculders: Sb@lder threshold Raj ti@ height: Akl&olut. kmight: R.l.ti- --&: Absolute @0&: 66 Z@.bled 2 I 3(0,.Oo 2 .00.00 50 n93@00-0b0ld .00 I D :ab ed 0.-0".': Dii ablld D s@kaod '0-*.'D.i:i..bld method Report method file: Last modified: Compound: printed: C:\KASSLyNX\s_p-ratg.PM@Imthva%lol$99&-Ndb ft..Oct Is 06:&1:21 1999 3: proSA (Ch3) "on Oct IS 07:46:31 1999 compound into @ I ()%@tity co=. of n- Ref.: Trace; Standards; U.:r RY value: r Peak F-C... UI.ntWrat. Wind@ Factor: Chr@toqr= mass wzndow: PPOSA (C2@3) (H I .. TIC C.-. C 1.000000. 000000 1. 2.000 1.0000D. Disabled Retention T@ (mi= ): Relative R4tentl-- Time RT Time Wind- peak selection: 7.797 o,o 0: (Mon0.) 0.679 -bld Di..bld U.-O.t Re p.- TYP-T R.:Po-:: Polyn-i@l TYP-: Point of Orivin: Fit Weighting: A.i. Transformation: Li@ z=lude I/X Unit.: p.&k-to-peak amplitude: S-tbli-9: wi.d- i.. (.CV..b.@ of @oth@: Swathing mthod: Join .Il:y tM j.h.1d: lteduc. pe ,k t i img: Rai&. be. Iin: Dratwo. vertical threshold: D. t hould*rs: Shoulder threshold: R. I.ti@ absolute Relative Absolute height: height; area: area: 9-bld 2 1 30.00 200-00 5.00 90 00 D@0.'&bld 3 00 102 .50: . a*o0. 0.... Di.@bld Di:&bld Oi lbl*d Di..bid page 3 Method R"Crt Method filei L&st -difid: C:\KASSLYUX\s@p-ratS.PrC\X@tILDB\101599a-mdb 1w. o@t le ofi:41;21 1999 Compound: A; IS (Cb&l -V no. o@t 18 07:46;51 1999 ipriated: Compound N lot.@ I R.f.: gu-tify Tv ce; C.@. of Stand&rdAt U :r RIIV lu-; U: r Peak'ractor: integrate Wind@ Factor; chr@tour= @SS mid.@: is (Cht) [None] TIC r -d 1.000000, 1.000000 2.000 1.0000D. Di.abl*d Retention Time (mi=@ R.I&tive Retention IRT R for@c*: Ti-*Mind- (-1-) P*ak selection: 7.157, Rn@bl-d 0.000, Dis@bled IN*.*, 0.41, N.-..t Type: Rl:p*w :: poly.o.i.1 Type: poimt of Origin; ritn Weighting; A@i Tx@fO@tiOn: units; Exto@l A.." Li. z@..Iud. 1/X P..k-.t.-p..akplitud.: s@ thing; Windw :ize isc@l: NuoLber f @oth-: S@thiM method: 67 @--ld 2 I join V&Ilay threshold: Reduce p.@k t.ili.9; Raise b--li- 30.00 200.00 5.00 Dr.. @*rtical threshold; Detect shoulders: Shoulder threshold: .J&tiv. hight: A :Oolut- height: R.lati@. re&: Ab.. I.t. r..: 9 .00 D3i0sabl*d 0.00 1.50 Di:abl*d 02.000 v i &bl*d -A Ili:@bl ...0. Di @bld Quattro 11,#6414E SOUP 020199:FACT Equipment Log 99092 PAGE 1/1 DATE.LJD/-IL/9-9ANALYST.ias STUDY NUMBER.LI_QX145 MATRIX: ratliverDESCRIPTION:dLYLL&-4 FACR Method: ETS-8-7. Injectivoonlume:_jD_d- Cycletime:10min.ElectrodeZ:-Sgray Mobile Phase: (A)2.gMM_NHACH= (B)_Me-QH- TN-A- orstndrdnumber (A) 99085-lrj--i Prepared(datdby): (A)IOL@@@ Expires: (A0)4/00- Storeatroom temp? E or N Other: (B)IWIQM_Lah (B)-Zglg-- Guard column: None Partnumber: na Lot number: Analyticalcohimn: KeystoaeBetasiI Size:2 x 50 mm - Partnumber: 055-701-2 TypeC:18 Lot number: P9E II Spheresize:5 um Serialnumber:0591804Z Analyticaplarameters: Dryinggas(Llhr)3:50 ESI nebulizinggas(Uhr)J.L- LC Flow rate3-00 uljmin. Back pressure:65 bar Sheathgas(LJhr)_Q-- BPLC solventgradient:10min-10-95 Time (min.) 3)-5-IQ4)7.50 5)8.00 %B 10.0 10.0 95.0 95.0 10.0 Tuning Method Method: Report C:\KA.SSLyNX\SoUp-RATS.pRO\ACQ=B\PFOS3 Printed: Fri Oct 15 11:42:32 1999 Page ns SOURCE ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. KS2 Set 3.00 40 5 0.2 150 250 Rdbk 3.00 -41 -6 153 250 Pressures Analyser Vacuum Gas Cell Rdbk 6.6e-5 4.le-3 msi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier KS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 14.0 14.0 0.9 0.0 4 650 Rdbk 3 Set 14.0 14.0 10 2.0 0.0 40 0 650 Rdbk 7 38 -0 tbod: =,. ndifid: P.L.t.4: PWi OM 15 11:3S'031999 Fri Oct IS ll:&2s4l 1999 sol-t play puwti- .I at. ) . @ of I is@ 0.00 VaLr t UP- I ter Channel Delay S@2 ) z S= ( Delta" ) : *o:*.'O starTtiT_i@ m(iK"i" Rod 0@I-00.0 . R".t. Channel parent Daughter Dwell (S@ &) Call Emrgy (*V) CO@ V 1 413.00 169.00 0.30 30 is F@ti= . 2 mm of I "-a P.Ir ( Zap- lat. channel Delay S". sp"r( Delta" ) : Start Ti" C bLi" Rod Ti- Ki- 0-00 X.P..t. channel P--t Daughter Dwell (3"8) Call Z"rgy (eV) c@ v 1 499.00 99.00 0.30 45 60 runtl- of I aftso walr (sop- x ter Channel Delay t 5,.a 00.03 S= i Delta- )., Start Tim Ind Ti" MtiK.i- .00 0.00 10.00 Repeats I v Channel P@=t Daughter Dwell (S@.) Coll AbOrgY (OV) c@ 1 498.00 78.00 0.30 As 60 F.Wti- : 6 of I =we Pair (Z"- Inter Channel Delay t Seca 0..0.3 Sp- ( Delta- ) : Start Ti@ and Tim ( KiKiw 0 '000 10'.00 Repeats Channel parent Daughter Dwell (S@s) Call 3n.rgy (.V) C..* v 1 421.00 60.00 0.30 40 60 Method ROVert method Tile: "at --Alfied: Printed: cs\jwsLTEM\Roup-]LLTB.Plto\ACQM)B\IozLin-10-95 priday, octabox 13, 2999 llt43sO4 rciday, october 15, 1999 11143:13 upllOO L4C FunV XzLitial Conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Oven Temperature Right(OC) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 NPIJOO L4C PU=p GrUdi*nt TLM@t&blG The gradient Timetable contains 5 entries which are Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 Hplloo Lc pu=V zztornal mvent Timtab3.e The Timetable Time Initial 0.00 0.10 contains 3 entries which Column Switch Off off Off Contactl Off On Off are Contact2 Off On Off Contact3 Off off Off Contact4 Off On Off Bplloo Autonamplar initial Conditions Draw Speed Eject Speed (111/min) Draw Position (mm) Stop Time (mins) Injection Vol,,-&(Iil) Vial Number 200.0 200 0.00 9.00 5.0 91 Page Pressure 400 400 400 400 400 Masslynx -Sample List Sample List:C:\MASSLYNX\soup-rats.pro\SampleDB\l 01 599a.SPL Printed:FriOct 15 11:56:251999 Page 1 Page Position:(1, 1) 1 2 3 4 5 6 7 8 9 lo 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 " 45 46 47 48 49 50 @51 52 53 54 55 56 57 58 59 FileName FileToict MS File 101599001 MEOH Blank 101599002 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS IOMIN-PFOS-POAA-PFOSA-IS IOMIN-PFOS-POAA-PFOSA-IS 101599003 MEOH Blank JOMIN-PFOS-POAA-PFOSA-IS lOl599oo4 TOX145, RBL10139-H20 Blank-11, SEE IOMIN-PFOS-POAA-PFOSA-IS 101599005 TOX145, RBL10139-Uver Blank-11,SEE 10MIN-PFOS-POAA-PFOSA-IS 101599006 TOX1 45, RBL1 01 39-5ppb-I1,SEE 10MIN-PFOS-POAA-PFOSA-IS 101599007 TOX145, RBLI0139-loppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 101599008 TOXI 45, RBLI 01 39-25ppt>-1l.SEE IOMIN-PFOS-POAA-PFOSA-IS iol5ggoo9 TOX145, RBL10139-SOPPb-11, SEE IOMIN-PFOS-POAA-PFOSA-IS iol 599010 TOX1 45, RBLI 0139-100ppb-1 1,SEE IOMIN-PFOS-POAA-PFOSA-IS 101599011 TOX1 45, RBLI 0139-250ppb-1 1.SEE IOMIN-PFOS-POAA-PFOSA-IS 101599012 TOXI 45, RBL1 0139-50OPPb-1 1,SEE IOMIN-PFOS-POAA-PFOSA-IS 101599013 TOX1 45, RBL1 01 39-750ppb-11,SEE IOMIN-PFOS-POAA-PFOSA-IS 101599014 TOX1 45, RBL1 0139-1 000ppb-1 1,SEE IOMIN-PFOS-POAA-PFOSA-IS 101599015 MEOH Blank IOMIN-PFOS-POAA-PFOSA-IS 101599016 TOXI 45, RTL-gRO3230M, Dyl, Contml- SEE 10/13199 10MIN-PFOS-POAA-PFOSA-IS 101599017 TOX1 45, RTL-gRO3231 M, Dyl, Control-SEE IOtl3/99 10MIN-PFOS-POAA-PFOSA-IS 101599018 TOX1 45, RTL-9RO3232M, D)fl,Control-SEE 10/13/99 10MIN-PFOS-POAA-PFOSA-IS 101599019 TOX145,RTL-9RO3233M,Dyl Control-SEE 10/13799 IOMIN-PFOS-POAA-PFOSA-IS 101599020 TOX1 45,RTL-9RO3234M, Dyl: Control.SEE 10/13199 IOMIN-PFOS-POAA-PFOSA-IS 101599021 TOX1 45, RBL1 0139-250ppb-CCV-1 1-1.SEE IOMIN-PFOS-POAA-PFOSA-IS 101599022 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 101599023 TOX145, RTL-gRO3235M, Dy4, Control-SEE 10/13199 10MIN-PFOS-POAA-PFOSA-IS 101599024 TOX145, RTL-9RO3236M, Dy4, Control-SEE iG/13/99 10MIN-PFOS-POAA-PFOSA-IS 101599025 TOX145, RTL-9RO3237M, Dy4.,Control-SEE 10113t9g 10MIN-PFOS-POAA-PFOSA-IS 101599026 TOX1 45, RTL-gR03238M, Dy4, Control-SEE 10113/99 10MIN-PFOS-POAA-PFOSA-IS 101599027 TOX1 45, RTL-9RO3239M, Dy4, Control-SEE 10/13/99 IOMIN-PFOS-POAA-PFOSA-IS 101599028 TOX1 45, RBL1 01 39-250ppb-CCV-1 1-2,SEE 1OMIN-PFOS-POAA-PFOSA-IS 101599029 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 101599030 TOXI 45,9RO3230M, Dyl, Control-250pb-MS-11 10MIN-PFOS-POAA-PFOSA-IS 101599031 TOX1 45,9RO3230M, Dyl, Control-250pb-MSD-11 10MIN-PFOS-POAA-PFOSA-IS 101599032 TOX145,9RO3235M, Dy4, Control-250pb-MS-12 IOMIN-PFOS-POAA-PFOSA-IS 101599033 TOXI 45, 9RO3235M, Dy4, Control-250pb-MSD-12 10MIN-PFOS-POAA-PFOSA-IS 101599034 TOX1 45, RTL-9RO3245M, Dyl, 5mg&g- SEE 10/13199 10MIN-PFOS-POAA-PFOSA-IS 101599035 TOXI 45, RBLI 01 39-250ppb-CCV-1 1-3,SEE 10MIN-PFOS-POAA-PFOSA-IS 101599036 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 101599037 TOXI 45, RBL1 0139-250ppb-CCV-1 1-3,SEE 10MIN-PFOS-POAA-PFOSA-IS 101599038 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 101599039 TOX1 45,RTL-9RO3246M, Dyl, 5mg/kg- SEE 10/13199 10MIN-PFOS-POAA-PFOSA-IS 101599040 TOX1 45, RTL-9RO3247M, Dyl, 5mg/kg- SEE 1Otl3/99 10MIN-PFOS-POAA-PFOSA-IS 101599041 TOX145, RTL-gRO3248M, Dyl, 5mg*g- SEE 10/13199 10MIN-PFOS-POAA-PFOSA-IS 101599042 TOXI 45, RTL-9RO3249M, I)yl,,Smgtkg- SEE 10113/99 IOMIN-PFOS-POAA-PFOSA-IS 101599043 TOX145, RTL-gR03250M, Dy4 5mg/kg- SEE 10/13/99 IOMIN-PFOS-POAA-PFOSA-IS 101599044 TOX1 45, RBLI 01 39-250ppb-CCV.1 1-4,SEE 10MIN-PFOS-POAA-PFOSA-IS 101599045 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 101599046 TOX145, RBLI 0139-250ppb-CCV-1 1-4,SEE 10MIN-PFOS-POAA-PFOSA-IS 101599047 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 101599048 TOXI 45, RTL-gR03251 M, Dy4, 5mglkg- SEE 10/13t99 10MIN-PFOS-POAA-PFOSA-IS 101599049 TOX1 45,RTL-gR03252M, Dy4, 5mglkg- SEE loll3/99 10MIN-PFOS-POAA-PFOSA-IS 110011559999005501 TTOOXX114545,,RRTTLL--9gRRO033225534MM,, DD)yf44.,55mmggl/kkgg-- SSEEEE 11O0t/l1331t9999 1100MMIINN--PPFFOOSS--PPOOAAAA--PPFFOOSSAA--IISS 101599052 TOXI 45, RBL1 0139-250ppb-CCV-1 1-4,SEE 10MIN-PFOS-POAA-PFOSA-IS 101599053 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 101599054 TOX1 45,RBLI 01 39-250ppb-CCV-1 1-4,SEE IOMIN-PFOS-POAA-PFOSA-IS 101599055 M90H Blank 1OMIN-PFOS-POAA-PFOSA-IS 101599056 TOX145, RBL101 39-5ppb-11,SEE 1OMIN-PFOS-POAA-PFOSA-IS 101599057 TOXI 45, RBL1 0139-1Oppb-I1,SEE 10MIN-PFOS-POAA-PFOSA-IS 101599058 TOXI 45,RBL1 01 39-25ppb-I1,SEE 10MIN-PFOS-POAA-PFOSA-IS 101599059 TOXI 45, RBL1 0139-50ppb-11, SEE Masslynx - Sample List Sample Ust: C:\MASSLYNX\soup-rats.pro\SarnpieDB\101599a.SPL Ponted: FriOct 15 11:56:25 1999 InletFile 13ottle lnjoe VolumO Sample Type 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 65 56 57 58 59 10min-lG-95 91 10min-lD-95 91 10min-lD-95 91 10min-lD-95 1 10min-10-95 2 10min-10-95 3 10min-10-95 4 10min-ID-95 5 10min-10-95 6 10min-10-95 7 10min-10-95 8 10min-lG-95 9 10min-10-95 10 10min-10-95 I 1 10min-lD-95 92 10min-10-95 12 10min-ID-95 13 10min-lG-95 14 10min-10-95 15 10min-IG-95 16 10min-10-95 36 10mir,10-95 92 10min-10-95 17 10min-lD-95 18 10min-ID-95 19 10min-10-95 20 10min-10-95 21 10min-10-95 37 10min-lG-95 93 10min-10-95 22 10min-10-95 23 10min-10-95 24 1Omin-1 G-95 25 10min-10-95 26 1Omin-I G-95 38 10min-IG-95 93 10min-10-95 38 lomin-10-95 93 lomin-lD-95 27 10min-10-95 28 1Omin-1 0-95 29 10min-IG-95 30 10min-10-95 31 10miri-10-95 39 10min-10-95 94 10min-10-95 39 10min-10-95 94 10min-10-95 32 10min-10-95 33 10min-10-95 34 10min-IG-95 35 10mir,10-95 39 10mir,10-95 95 10min-10-95 39 1Omin-1 0-95 95 10min-10-95 3 10min-10-95 4 10min-10-95 5 10min-lG-95 6 10.000 10.000 10.000 10.000 10.000 10.000 io.ooo 10.000 10.000 .10.000 io.ooo 10.000 10.000 10.000 io.ooo 10.000 10.000 10.000 10.000 io.ooo 10.000 10.000 10.000 10.000 10.000 - 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 - 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 - Conc A - - - Page 2 Page Position(:2,1) Masslynx - Sample Ust Sample Ust: C:\MASSLYNX\Soup-rats.pro\SampleDB\101599a.SPL Pdnted: FriOct 15 11:56:26 1gN FileName FileText Go 101599060 TOX1 45, RBLI 0139-1 00ppb-I 1.SEE 61 101599061 TOX1 45, RBL1 01 39-25OPPb-1 1, SEE 62 101599062 TOXI 45, RBLI 01 39-50OPPt@-1 1, SEE 63 101599063 TOX1 45, RBL1 01 39-750ppb-I 1.SEE 64 1015990r>4 TOXI 45, RBL1 0139-1 OOOPpt@-1 1, SEE Page 3 Page Posdion:(1,2) MS File IOMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS_POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS Messlynx - Sample Ust Sampie Ust:C:\MASSLYNX\soup-rats.pro\SampleDB\oll599a.SPL Pdnted:FriOct 15 11:56:261999 InletFile Battle InjecVtolume Sample Type Conc A 60 10min-10-95 7 io.ooo - - 61 10mirlG-95 8 10.000 - - - 62 10min-10-95 9 10.000 - 63 10min-lG-95 10 10.000 - - 64 10min-10-95 11 10.000 - Page 4 Page Position(:2,2) Date: Data Analyst: FACT Study #: MatrixrrimCpOint3: Sample List: Set-upAnalysis Date/Analyst Instrument: FACT: DATA REVIEW SMNLARY FOIZNI Data Review Sign-Off AnalystReview Name/Datc:.:@QL /107@@ #/c5@ TechnicalReview Nune/Date: y6pl.2 )4,f h-A IOIZO163 QualityAnumuce Review NiLme /Date: Data Entry:_ LAC, 1[) 9 Con=nts /Justiflcations: Analyft: Ftos A=ptable LineaRrange: LOQ: EV=ti,,BW& < R^2: CalibratCihoencks- Mbix Bknk.- P4)AII w MS/NMD: idataStaMs.4L 1)4rea 'A@5 Ai,-,r L@ C, toip 9@ I t^.-C-LMAZZL ii &@.4,ev,@--7-- IQZ-- 14 Analyte: AcceptableLinearRange: LOQ: /2@ R^2: 41 !2zR67 CalibratioCnhecks: msimsm@. ID&taStaum/"R) Ptclcd 1,<: MatrixBlank- Analyte: AcceptableLinearRange: LOQ: R^2: CalibratioCnhecks: MSMSD: ID.tSat.: T-37 ExtractedBlank-. MatrixBlank: 14&4EAj 7' @ le-") /Vs-r -Z7v 7r@e.,vp@e- wg7e,;-512FA&z.)Qev,-, Date: Data Analyst FACT Study matrixrrimCpOint3: Simple LisLSet-upAnalysis DatrJAnalyst Instrument Anatyte: AcceptableLincarRange-. LOQ: R^2: CalibratioCnherks: MSMSD: Data Status: FACT: DATA 'KDjLr:,VISEUWMIMARY FORNI Data Review Sign-Off AnalystReview Njunc IDate: TechnicalReview Li Name /Daft: QualityAssurance Review Name /Date: Data Entry: LAc- Comments/ Justifications: ExuactionBla& NiatrixBbuilc Analyft: AcceptableLinearRange: LOQ: R^2: CalibratioCnhecks- t MSft,LSD-. iDatiLS Extmctedog@r_ Blank. Atialyte: AcceptableLinearRange: LOQ: Extrac ank: .nk- R^2: Z trixBIl.aBnNk.- z CalibratioCnhecks: \.O MSAZD: Data Sams: LAC,lo)-alig ii QL@tify Compmnd $@rY ROPOTT T" 145: Rat P@ oilutA@-@ Day 1-4 UT" la-.I,-P,Yl(K?) I Smiple List: L. t wadified: ftd Oct 20 00:31:47 1999 I"=: C:\MAMSLYNX\@li*--t--"C\NGthDS\101*tga Last .dLfld: Wd Oct 20 09:16-18 1999 Job C@d.: ftinted: wed oat 20 09:00.41 1999 compound 2: PIO@ a 1 N@ 1I01I999001 I @I ::9012 3 1 @'g.900034 4 1 0 1999 50 005 6 11001199999900006 1019990 07 9 00 101999009 1 101999010 10 101999011 121 101999012 3 101999013 I4 @o", 9'.01,5 116 1 6 1011,9017 1, @0o,@,::Oo@,: 9 20 101999020 21 21 22 23 1l1 o1l:::022 019"1123 21 0 @9990022:1 2 1019,90 2 2 21 101919027 2: 2 lol:::.2Ol: 10 10.1:::00301 31 1 1 3 32 101:::0032 33 101 33 34 11 011 :9:034 31 @019 9,031 36 1019 9 9036 3 37 387 101199:999@013: 39 03 ampilint T"t M.OH N 'M T 11 45: Too I45: a 45: T x 145: 0 5: To To.x @.1: To 145: T x 145: To 145: Ta0x 145: b rt SEE 10-13-99 P.BL,10139-Li@*r bik-11, Lxt SEE 10-13-99 R"SL 0139-5 PPb-ii, Ext SEE 10- 13-99 L10139 -10ppb-11txtSEE 10- 13-99 RBLI00139-25 0 _111": -tt SEE 100-13-:: RB Ll 119-S@o. ,b_@@, 13- L@o .1 SEE 0 RB 10 139- L 139-250 ppb-11 Ext sEE 13 RBLI00139-5070 0 = 10-13-99g RBaLLi 139- 5 1111 U.t1 SU. 10- 13- 39-1000 ppb-11, Lt SEE 10-13-99 TTo x To0xx T? 0 I. Toag N*OH Taoxx 7Tax Tx To0. Tax 141: 145: 1455: 145: 145: 11455: 1@ 145: 1:5: 1 5: 1.01 .17M. -yy 41: C5o@.t9r/kolq, D:1I0o0o 3245M. Da :RiRtO.(3,24 @2:7M, . 32 I014_ Day 1. 5 mg/kg, D: RBL 10 36K9: 2D5a0yypp1Ib:-151-.2./-/kkgqE:xt 0DS:EllICE0oO0oIO-13-99 032 gm Day :"R,.0033225,2lMM.: Dy Dy 9RO3253N, Dy 1, 3 mg/kq, DIIOO 4, 5 0:1000 4. 5 .4/",;,D:l 4. 5 D:100 9lto3254M. Day 4. 5 mg/kg, DTIOC RDLI0131-250 PPb-11-1, txt SZE 10-13-99 "T*.O.M145: Tx 1:1: 1.. : To 1:5:: T.4. T x 145; TT.I: 1:5: x T x 1455:: TTax 145: LI0139-IL2. blll-ll, t SEZ 10-13-99 131-111.1 1 10 13-99 IML10139-5 ppb-11. Lt gut SEE SEE 10 3 -;9 RRSDLI100139- 05 ppb- 1, Ext SEE 10-13-19 Ra L 139-21 L10139-50 ppb-i1,il ppb- LLxxtt S3 LEEE 11 00-1133 ::: R13L1I013:-Ioo ppb-ll. Ext SEE I 00_ 13::: PLBL 10113 9:250 ppb-11I: Ext SEE 1 13 FRLBBL 10 3"_S5o0 0ppb-I Ext SEE 10 -13-:: L 013 7 0 p Ext SEE 10-13- RBLI0139-100 pPpb-b1-1l'l, Fxt SEE 10-13-99 Type Standard S3 tandard candar d Standard SSttaannddaarrdd Standar d stands rd Standard oc oc standard S3t nd&rd t=rd Standard St:nd& rd St ndard standard Standard Stand&rd std C- 19:9,3 6 24 497:.3,*0 @:..00 .00. 113 735.0000 976. 249.00 248.00 4.13 9.76 24.630 479.60 ;,:..:00 493.00 135.00 976.00 ItT 59 7. 16'7 7.140 7 123 7:120 7.120 7 137 7:.120 7 . 141 7 "8 7 1209 7 11 7.149 7 li: 7 13 7.1431 7.1 9 7:.113494 7 163 1 1465 7:24 7:@1:3 7. 165 77.16: 7 :t"5@ 77.1.. 7.165 7 140 7:149 7.1480 ": @ll 7. 7.@1:25 23 '77 .141 + 33 2: 1 1207 13,: 563 @2 2 610 4:96 :3535 03 41 13 23 91: 3037 3370 2132 204 3 250 263 30 0 3857 33:5 3:70 1 os 3S 270 29, 496 170S7 07 26453 4135 1I'0l9l 0.00 0.00 00 0.-000 TIM9. bb bb bb to.@ 0 :o0.0 bbX 00 25.:4 mm 3 4 @l5,:!,,6 mm 3 29 0 .6$ M 2 56:.13 MMM" 10 727 43 NK 130:73 M -5 bb 3100.00 240 - .1 bb 325:31 M '2@065-.,0:5, 'M 2 1O..o NH bb 276.01 mm 326.91 429.51 361.6 bb 3.78: bb 1 0-:90.2:. M bb 1.:11 lb 00 ..0. MbNbX o.oo mm ll:-13 bb :2.92 bb a am 17::,Il -29 -100 -100 -2193 -9 12 :97.60 MN -01 .9@1.1. mMmM -6 ',Pd,@56m, Li 5- LAC- /)c-a LAC- A@lLa 062498: Q@t&t&tod W ft,,,td y _h 3.0/20,,, a.- tity C-P-.d T.."145: MtZZ7@ 3-" D.L. A.P.-t S.wl. LA*t modifi&d: Nj*ot:ht"E:*dL @..d: C.": sod oct 20 06;21:47 1999 V"SLY)ix\a..Ll,a;rata.m\mothDa\loltgga CW;ed Oct 20 00--ld: 999 ftinted: Wd Oct 20 09:00:41 1999 Co.p@und 2: 77*L% 1 101999001 2 101@:1:002 003 45 1001199:'99004 05 6 101999006 7 101999007 9, 11 01199900: 10 , 0 99900 01 :::010 12 10199900111 2 13 l10o0lg9::013 14 0119990 014 1 1151 10199901151 is 10 1:1 01: 19 1 9:01 20 101999020 21 10 1999021 22 1:::022 23 0 023 24 1001:::024 25 10 1 go 025 26 1 026 27 10199:90 27 28 101 9026 29o 101::,9029C, 303 3 101 31 101199990031 32 11 019990 32 33 1 0 19990 33 34 0 34 35 1011999:035 376 1 0 9 036 3 6 1 01199:037 3 0 99 038 39 101999039 s am &LI.t T..t M.OH 3' H*om @45: Tx Taax Tax 145: 145: 145: Tax 145: T . 145: T:x 145: To. 145: Tax 1:5: Tax 1 5: T.Ll45: RDL10139:H2o blk-11, Ext SEE 10-13 RZLIO139 Lil*r blk-11, Ext SEE 10-139-999 RBL1013::Soppb-11, Ra I I Ext SEE 10-13-99 aL 1 RRBLIO10.3193_ g-'2@ r-xtt SEE l.o--1"3--:: L 3 o p::;Illi,ll,.,El 1*1;13 -119 IRtDBLI00,13399:10205 L 0 ppb-ll, RBLI0139 S.5000 ppb-11, RBLI0139:7 ppb-11, LExxt SEE t SEE zxt SEE 0:13 -9 1 1310-13-:: 10-13- RBL10139-1000 ppb-11, Lxt SZE 10-13-99 NT:X 145: 9RO3237H T x. 1:5: ::0.32:SM: 'D"OYY D. *.'10.00 -ro. 1 1: ..o 32 Day 1 5 D:1000 T xx 1:5! -,.,, q@,.: To 1RS.L0.3"24.., Day //kgr,xt Dt:)l:I()o Tax 14 551 Day 139-2 ppb- 5 !29 SILEOIO-13-99 N.OH To. Tax Tax Tx To Tx 145; 145: 145: 1:5: 1 5: 145: 1.. 31:4., SDoy 09A 3251M Day 9RO3252m, 9gRo03253M Day RBL3254M: Dy @0131-21. 1 5 mg/kq, 4: 5 mg/ 5 4. 5 .9/kg, ppb-11-1, Lxt D:10000 D:l D.:I@0000 D:100 SEE 10-13-99 M:@H T. xx To 1.. Tax Tx Tax Tx To0 TT*xx T.. 145: 145: @4@: 145: 145: 10139-H20 blk-ll, Lxt SZE 10-13- 9 RRBBII'.1.01139-1,i,.,,1,1.k-@l, t . l@-13'-91 Li 39-5 ppb-ll, Lot SEE 10 13-99 RDL ppb-11 lex SEE 1;-13-99 RSL 1000113399--2150 ppb-il: Xxt SEE 100-13::9 145: 145: 145: 1445: RBLI1 139-50 P::@1,1,.rxtt$ZE "LI0139-100 RBLI0103,9:25 ppb RSL 3 50.0 ppb 11, Lxt SEE 11: .x, SEE ML10139-"50 plb: Ext EE 1,;13 -13-:9 10-13 -19 10 :@13:9: 1 39 14 55:: RaLI0139-1000 Ppb-11, EXt SEE 10-13-99 TYP- Standard tt-d rd 33 .:Id t.rA&rd d 3Standard Stan r st"d&rd d Standadrad OC oc Standard Standard SStta.ndard d Stta.nd'arrdd Standard Standard Standard Std C-0 43 :917 219. 0 49.30 97: '10 2 4938-0000 736.00 971.oo 248.00 248.00 -93 11.17 2"4:$a3 .7 0 97 246.0 0 493.0 0 73767..00009 I]tT 7. 1.#4 7.62@ 1 1.003 7::00 7 .6 01 7 17 1:,$g.@ 77.7s: ').Soo ?.:Do 7. 52 7 :22 : 7')...l24'2 76 0240 77 7990 7::2 7 . 256 77 .s 2 .8 2: I .2829 7 .8242 7 .810 7.:11 7. 45 7 21 7:.:820 '.,2: 7.70go 7 .526 7 23 7.82016 t r)LA?h@r rnr,@ hay-e- @Uy\ SWi @chLA A@ 24 19 2, 1 3 146, 24 a0 13 4 24 0 6 6409 4 12860 14433 20057 196310 1:.l@* 1821 666: 2344 947 109633 11349 7149 32 60 53 147 271 136,64 245 653: 3734 1@59735 20 as C-. 00 .00 0 -@0@0 0:51 risq. bb bb bb to- 4.61 @m2m' 5.41 mm 29.60 bb 48.21 M 93.11 bb 240.28 bd 483.44 M $42.66 MM 754.50 .23 350.31 PM bb MM.+ 1,1:1.4 1 0 75 mm 63 0M 67 2500 :1, W 09 bd m *,'4:'7.bb 3::4Il m 3 1. 6 bb 4 2 bb 26. 3 .326 MbM 1.3 bb 1 11 bb 4 : 65 bb 9.32 bb 3 4g'l8:.',@135 kbbb .3 bb 245 3 bb 51 5::1:.2'646 MM 7 1 MMX 14 19 -2 -53 -2 -29 -23 a -6 -5 228 -6 -1 -1'9 -20 9,kC) D4@i, L4 Sphalk@ LA A-11& 062490: Q@tit&tsd &W ftinted by wh 10/20/26 ot@tiry C=wowtd *U@, Tax 145: MtZ,7 C PAPORT 1, sa.p 1 . LA.t: L.St *Adified: vw oat 20 ol:31:47M1t2&*.o method: \N"sLywx\@1.1a I;wa ta.vw\methdn\lol 3.oo9 La.t .dif..d: co@w oct 2o ol.16; Job Co": toga Pri.t.d: wd Oat 20 Ot:00:41 1999 c@..P..nd 3: pom I "I1 lolls9ool 3 lol999oo3 4 101999004 5 lol9s9oo5 6 101999006 7 101999oo7 89 1011999oO: 1 0 @99:00@ 0 @::,Ol 11 1 a 12 1 0 1999 0 12 a 13 101999ol3 14 101999014 15 0 167 199'.@lI 1011,9901$ 1 11 10a 1:::019a Zo I 1 02 21 11 019999:002212 22 01 23 11 01:::023 24 ,01 999024 25 0 025 26 1019::026 27 1019 027 2: 110@l::.:Ol: 23o, 1@00119999990DI2O 3 31 32 101999032 33 1,01,;::033 34 101,99 034 35 035 36 101999036 37 101999037 38 101999036 39 101999039 S..plealat Text "HO-om 7 a. T Tox To.ax. Re L 1j0o1l39 -K2O bit-11 txt CE 10-13-99 11:55:: RBL 1 39-Liv*r bik- LxSt SEE 10-13-99 145. RDL 0139@-5 ppb-11 .Ext SU 10-13-99 , r@t SEE 1@.0:@13::: 145;: RRBBLLI100113399--1205 Ppppbb-- Lt SEE 3 Taxx It RBLI10113:-l5o0oppb-11, Lxt SEE 10-13-9:9 To. .5: RBL 39- Lxt SEE 10-13- T.. @.l@ UL@ 10 13,:2,500. ppb-@1l, r-t SEE @10-13-11 T 5: RBL 0O@3 "1. ,Iaxtt S..E.E. @00:13 145: RBLIO139@750 13- TTo x 145: RAL10139-1000 ppb-ii, Lxt SEE 10-13-99 .:L T:: @ll@l:::003@3?M: T 5: 3@.. 0Di,:,y4,: C,o::,ro.l:D ;1@0.0 0 T x 1:5: 9RO324& Toax 1 5: IR03247K: 0.4,y,@': .5 -oq/,kg,:Dl:lloo. TTox, 21:55:: 9PARL0I3O241M3,92-D&ySO pp1b.-*131!29./kaqx,t D:S1Z0E0 lo-13-99 K*OH Toxx "4': IR,0t3o24 5 ag/kg, D*.100 To 5: 3259IMM: DDaayy 1, 4. 5 og/lcq, D:100 T x 1,45: :.RO03252M Day 4. mg/.. D:100 To 45: 32 3K: Day 4. 15 magq/ ,g: D:LGO T x 145: 9R03254N. Day 4. /kq, D:100 TzM145: RBLI0139-2$o ppb- 11, Lx3 SEE 0 1:-13 99 "T:. T, T*o. Tax Tax Tax Tx To Tax Tx Tax @4@: LI0139-IL20 blk- Lxt LE I - 3-5-9 III: R3110.139-Li"r b1 ik-11 45: Ml 139-5 ppb- 1, Zi Ext SEE 10-13-99 SEE 10-13-99 145: 145: 145: 1:5: 145: 145: 145: RDLI0139-10 ppb-11, txt SEX 10-13::: RBLI 0139-25 ppb-11, Zt SEE 1 13 _99 RBLI0139-50 p;@ll_,,,Xx.@tSU.. 1.0@;-13 RaLlOI39-100 -13-9. RBBLI0013:-25000 R 5 RBLII'0l11339:750 ppb-11 Lxt SEE ppb - : Ext SEE ppb-111, Ext SZE 1o0-13::: @o:@13 3-99 REkLI0139-1000 ppb-11, Ext SEE 10-13-99 Type std c@. RT Standard ta.ds @d St nd.@d S5 t:n @d t ndd-ard Standard 1S 1.,I.@d t..dard Standard oc o*0 iI.ooo 1,*0c0 0 1:00 1 1:o"O 1.0o 6 66 :::477, fi.:71 :6:-9.66-121 6.94: :::,4,6 6.17o ::::3, ::::7 1 6.197 :::,1,4 6.972 OC Standard S3 tandard 3 tandar'i tmdard Standard Standard Standard Standard Standard 1.00 1@-000. 1:00 1 00 i1.:0o0o 1.00 1.00 1.00 6.914 6 :O9@94 6 6.992 ..169 6.976 :.9 5 6..9.71418 6.9 0 6.9 74 6.96' 0 A- C@ Tlag. *Dev 637 2.61 b 92 0. bbb 29 0.86 b b 29 0.08 b S4 1.63 mmb 34 1I.02 KN 3: 07 bb 3, 10:.15 bb 3 92 bb 19 0.56 bb 41 1.23 bb 1619 - -11@ 63 2 7 is 23 17 0.51 bb -41 1: 00.4503 bb :52 1 bb 47 is 0:!iG _:4 1 0.54 bb 6 65 1.94 bb 94 24 00 .72 b :238 29 .81 bbb 1 27 0 1,,9 0:.@,:bb 14 2 45 1.34 MbMb 34 109 3.27 bb 227 35 1.067 b _4 6 19 0.5 bb 21 G.023 bb 1 41 1.2 bb 23 29 0.8184 bb -112 b 14 33:5 1:13 bbl, 3 3 1 .07 bb 7 22o 1 .65 bb -32 5 4 a1.20 bb o sLd P." 3 A-IL& 062498: Q"ntitated and Printed kry mh 10/20/90 Q@-tiry Cqp-.d 2@ly Tax 145: ftti!;@*1 "Mlt D-Y I 4 1A.t: L@ t modified: L@a modified: Job tCo": ' w" Oct 20 06:31:47 1099 C:\Wj&LyXX\@JIM-Mtg.pW\NothDB\Ioltgoa Wed Oct 20 06:26:18 1999 Printed: wd Oct 20 09:00:41 1999 C..p..@d 4: 13 tCh2) 0 m- 1 99001 2 11 01:99002 ol 3 1 1999003 4 1 1999004 5 100 1:::015 0 006 10 11011:9:00; 9 1 0 ,9 00 l@ 0 @9 9:001 0 19:901I0 12 1001@999,11021 1 03 1,45 1@0011:::014 015 16 110001999016 1,7a 10 199,011 @9 lo@1:::Oll 01, 20 101119020 21 1019,9021 22 101119022 2 3 1011:9:023 24 10 9 024 25 101999025 26 101999026 27 11 01199:021 221, ,0 1:9.02 30 10199902:0 31 21001l9g9::00331 3332 1 0 1999003332 1 0 1999034 34 1 0 19990 35 1 0 19990 35 36 1 0 19990 36 31 10 19990 37 38 10199903 39 0 3: .-Epleliat 2ext MH.*OH" Tx Tax T 1. T0. Ta0x, T TI., T Tax TToo,. 145: 145: 1:55:: 145; 145: III: 1 45: 45: 1@4451:: RBLIC139@H20 blk-11, Lxt SEE 10-13-99 RBLI0139-Liver blk-11, Lxt SEE 3-'9 IBLL1013::S.Ppb-l@li,Lxtt-- @@0-1_11_-:0g;1 3 1 ppb- Ex SEE 0 13 RRBDL 10131-25 ppb-11, Ext SEE 1@o0__@13:,9: LIOI.19-50 ppb-11 PLBL'@.o,139-10500 ppb-l!1,.Ex"tttSSESEEE 1l0o-_3133_-9999 RRBBL 101 39-2 050 0ppb 1 EE L 39-5 PPb--11, rE'x4t SEE 10-113-19 .RBLI1O01133::7100 PPb 11, Fxt SEE 1 13-9:" ppb-11, Lxt SEE 10-13- MTax @41: IR03237M, Day 41 : Cc trcl, 0:100 Tax 145: :RC32:-IM: Day " 5 Z./"kgg,, DD::1I0o0o 14!,: , 3244M. 04 T ox 145: :,0t0o32 7N Day I, 5 mg/kg, D:l Tax 14 5 324,1M. Day 1, 511mg/,kg,tD. -100 Tax 14 Mia 31-250 ppb- -2 Lx SU 10-13-99 now Tax 145: IR03249M. Dayy TTo 1:55 : 9R032 Do 'I: 5I k9k.: 0'.l@ 0-00 I : 9lt032,'2'K: Day 4, 5 q/kkq: D:110000 T@ IR03253M. Day 4. 5 .9/ 9 D: Tax 145: 9R0L3254M y 4, qlkg, D:IFO.O T4aoxx 145: RB 10131-23D0s ppb-11-1. Lxt ST 10 -13-19 TO.ON145: T x 145: Tax 145: 'Ta1x.. @14415:: Tax Tax Tax Tax T.. T.. 145: 145: 145: 145: @ll: 145: RBLlOl3l-K2O blk;ll 10-13-99 RBLI0139-Li-e@ b SEE I @ @0-13-99 I.tBLlIo0@139-5.ppb-@@, L.1 0- 3-9999 MLILOI 3:-l PPb-11, r-xtSEE 10:13- "LIOI 3 ,.Ippppbl_i@,@: 11t 1.1 11 13-:: RBLIOI 339;,:50 0-13- _ RDLIOI 9_ 1 00 ppb-11, Ext SEE 1 3 99 3 2 So ppb-11. Lxt SEE 100--1@13_99 RBLI013:-50 ppb-11, Lxt SEE 1 :,3-:9 L 0 3 -7500 p b- 11, Ext SEE 10 3- 9 RBLI0139-1 000 Pppb-11, rxt SEE 10-13-99 Type Std CA@ Standard Standard :t:ldlrd t ndard Standard Stan d rd Stsdrd & Stt:.drd 3 nd:rd 1.00 i.oo 1.00 1.00 1 :. I@1..0o0 1.000 oc 1.00 QC ta.d.@._ Standard .1t:.dard t ndar'i SSttaannddaarrdd SS t:nd r t nd:rdd Standard 1.00 1.00 1..0000 00 1.00 11I.-00.0D .0 RT :.'9152 6:96" 6.15 1 6.9s: G.:Sl :."a '56 .6:-9517 6.1349 7 6.18 6 6.9780 6.155 6.164 ::::4 6.9,8521 6.1030 ::::o 0 7 '1:.09.7.3,7 ..,.7 6.963 :.:59 1117 .6.:9"5G5l A- C-. riags ID.@ 22946 3.727 40 74 :@ll 461'2 3915,04 7., 3827 3201 30 31 31 32 2545 32 30 270 25 3 275: 2979 32981 3934.. :134 4085 3571 34937 3 3260 331428 0.74 bb -2: '1.:2"0 tbb 20 .o2 bbb 22 6 6 1.16 bb" 16 1.00 bb -0 00.:O:@6, bb I 4 0.83 bbbb -17 0.01 bb 0.:011 1 - 0.00, bd :919 bd 0.0615 klb -9: bb -35 00: 0 bb 0 bd 0 00,1@ bd 0.09 bd 0.0Go bb 0.75 bb b 0.893 bb ,-19. bb 1:04 bbbb 10.0930 bd 0.99 bb 0.87 bd 0.81 bb 0.84 bb dd :939, -100 -25 -17 ;l 0 4 _13 -0 _11 _13 -19 6 Page 4 cl) /,-@ no@ukA. A@lia062499Q:@titatedandPrintdbymh 10/20/99 Q,@tLfy CalibMU@ Rt R"@Ct Dy 1.4 =' ,r,- r - %-;Oi"i,i,p-1,noaumnrd, PIL)S ICoefficientof Determinafion:0.989844 icalibraticounrve:8.25151* x + 352.987 Response": ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:I/x,Axis 8.4le3- None Response- 0 0.0 ANalia 062498: Q@t&tated Ci()a) 200.0 and Prl@ntmd by mmh 10/20/92 400.0 600.6 00.0 Conc i 4),,antiry caiibcau@ 1,45. .t P"m,t Di a. bay 1. 4 llr-olillp-o"uPnFiO@SuAe: icoefficieonftDeterrninatio0n.:997888 Calibratiocnurve:26.5524* x + 23.6545 IResponse ripe:ExternalStd,Area Curve type:Linear,OriginE:xclude,Weighting:I/x,Axis t=: None 2.6Oe4- ftg. 2 Response- Ix 0. 0.0 Amlia 062490: 9@t&tated 200.0 ftlated by Emb 10/20/99 400.0 600.0 800.0 Conc Quantify calibrati- A.S..t ?*, 141; Compound3name: AA IResponseFactor.33.2811 iresponserype:Extemal Std,Area ICurvetype:RF 54.4- wage 3 Response- 0 Conc 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 A"lLa OU498: Quantitated m4 Printed W wh 10/20/99 ftg. a 7coimi@pn-o&un@n,a .ResponseFactor:3976.31 esponse e:Externalstd,Area Curve t)rpeR:F 4.86e3- Response- 0 -0.0 O'l 0'.2 0'.3 j@_lis og249@: o@titated and Printed kry -h 10/20/99 0'4 0.5 0.6 O@7 Conci 0.8 0.9 1.0 Matnod P@port Methtod Las wdiffitleed:: Compound: Printed: N'l:e\d@Octli2&0-r0a0t:s1-6F:R1C0\Me1t9h9D9BC\Iolggga.ndb 1: PMS Thu Oct 21 15:13:17 1999 CIompound 14@.: ncernal R*f.: Qu ntity Trace; C@&nc. of Standt": U r IkFValue: usser Peak Factor: i.t.qr*to Wind@ Factor: chr@toqrm mass windo.; LPoe-ackatlon i R.:1I:@nitvl:n..tT:i0.t1lonnTi" RTI.R..tW.,@ ...: T nd.- (.1-1: Peak Sal action: R65POn3* yp.: R":.$P"I*.::?: Calibration Cu"ws fPtoliynntmoif&loriTgyipn*:: Fit UTighting: Axis @msfo@tion; concentration Unit:: Note pe&k-ttho-peak amplitude: Smooth Sw wothlnq: Ind.. , Nu'ber c it: (StChasn:st: f s- thing -thod: B..:Iln.. i.i. valley threshold: R d co p :k t ilift R:Iuso ba: lift:@9i:@ Peak Separation Drtaawcvtertical threshold: D. shouldra: SR.h.*;@Id.,,. Tt@h,r@:,hhoold: d R.La.tivt: h @ght: Ab lu h:lqht: R.I.titv: a,::: Abs, lu r PMS IN." ) TIC co=. A 1 Disabled :0.*.*.,*0,., 12..00. 1.000ODa 7 ad 0:..70: Di's@'bl.d IN...] 0.350 "&lest Exte@l A..&. L.Ln at Lxcluda I/X lio- 100 rnbl*d 2 1 30.00 2.0.00 5 00 9,@-.0b,ld . 30.00 1.100., ll1:,b@l:d o. 0 0 ab d 2.00: Dl:abl:d 0.00 Di bl d 7r- Method aPOrt N*thtoLfLIO: i L.s dif *d Compamd; P@inted: :: od Oct 2 't' "Uftth9DO. 101999----lb .14:18 1 m 2: PROM Thu Oct 21 15:13:11 1999 C1,..P..nd t*rn. 1 Quant&ty Conc. Of NR :.f.: .: Tr:ce: St ndards; U::r RP.F.V.1 .: U tr k F ct*r: O'@.t. Fact*r: CIhr..t@9r" Wirmi"ca. indo.: L..k L*Clti*l t.n RT R*frn T w i.d.. onn STL" P..k 5.1 *Cti..: R..p.... ll:,p,.,:::Typl: . P. Calibration CU"*3 polynomial Type: F.in t f Origin-. Fit Wei hting; jlxis Tr9@sto@tion: Concentratio Units.: N.i Peak-to-pask Smoth &MPllt-d*: SM -othing: Nui".. do-r Soft..'th l@c&--): S-thing sas*ltn*s method:*: J.@ .Iley threshold: Redu-ce peak tailing: RALSO baseline @K 1---: Peak separation Dratwectv*rtical threshold: D. shouid*rs: S.h.,.uPl.dn*3@. Tthhrr::,hold: PROSA [No'.1 TXC Conc. 19 I o*,*,,, 21.:...000...0 1.000 Da Disabled 7:.121: 0 00 .2 I lmn, KDni&.b&lbl dId 3d.m6r..t ltxt*rml Areas Lin ar Exclude I/X 94 L.Abld 2 I 30.00 20 0.00 5.00 90 00 D@;.bled 30.00 Relativ: .t Ab Is luive AIb's*olutt* hh:lqhe: ght: &r i ar:::: I 0:@,oOo.o: 20.00, Di:&bld a &bL*d DDLi ob ad Di S&bi ad page 2 k4:thod AC:Port thc,d I.: Last wdified: Compound: Printed: N: @"elia-r&tS.pRO\No Wtd Oct 20 08 16:10 thM\lol999&.mdb 1999C 3: POM Thu oCt 21 15:13:18 1999 CO.IPOU@C, N'0-@Ct*i'l.y. ' T@*!..:: Conc. of Standards: U::r RF Value: u @ Ptak Factor; I.t*qrat. mind@ Ch@@ toqrm -as Peak Lmcation Factor: windo-: l,l:t:nl.l:,.Tl:t@lIlinIT,l: I ti ot on at PT T ltafer nca: @@ W,.do- PCAA I TI@Narlo Fixed I Disabled 1:.O.*o*.,O, 2.0 0 1.0000DA 9047 0.234 Enabld &bled Ptak selection: Atsponse Noar.st RR::Po.:::Typ*: Pon Calibration Curv*s Lxt:ml ILr ftlynmial Type: Li Point eioqf Origin: Lxclude Fit N I/X @y Axis Tranhstfionrqm:ation: None Concentration Unit :: 11.@ PO&lt-to-paak amplitude: 904 Smooth S-othing: w@.d.. $I.. I.c... Numbtr of S-: th ing B.. 1-.i.. smoths: method: i @ v.alley threshold: ll*.d' ..is'. beP*.:'-l@nt:i-'xiin@q:: Peak Separation Lnbl.d 2 1 3 00 zo0;.Oo 5.00 DratwectverticalI threshold: Da h.. d.@.: Shoulder threshold: Response Thr*3hold Ael3a0ti : Ab luv t Absolute h:ight: , ght: hr ar:a:: 90.00 Di@@bid 30.00 I so 0:.0 20_.00 0 ti:.bled aLb ad DOilllbl:d 1 .bl d Iddl5@ Page 3 method Report N.th"d file: La. t wdifi.d: Co.,po-d: Printed: N:\-Iia-r2ats.".O\MethlDB\lGI999&.Sdb lled Oct 0 08:16:1$ 1999C 4: IS (Ch2) Thu Oct 21 25:13:18 1999 CIoupoUnd Name: t*rl,e,l 11*1,: 'u'@ ,a...t Tr .. yf Standards: UU::r R:.Vo 1 4: @ p k Factor: Integrate Window Chro@togr@ @95 peak L.@.ti.n Factor: window: RR:taenti nat.ima,tilmi. 1: I ti@: t on Time RT.R.*fVir..C.: Ti nd.. (.1..): Peak Selection: Plesponse R 2pon::,Type: R:.P.. Calibration Cu@as lyn*ai al Type: 1P0oint Origin: Fit Heiogfhtin Axis Tr@sf,9:-tion: Concentration unit:: Not$ P-ak-to-peak AmPlitudO: S-Oth 5-. thing: Window 3LZ* (Scsns): Number of swaths: 5-* thing B..Olines Othod: J in,v.all:Y t r *hold: R:du pe k thaieilnq: I1 S (Ch2) M...l TF,IC .ad @ :O,O0.0.*oo0" 2.000 1.000OD& Disabled 6.910. 0.000, I 0N.o4.0 Enabled Disabled M..reat Ext.:r &I Li ar txclude I/X mno 94 E..bl.d 2 I 30.00 200.00 5.00 Dratwectvertical threshold: Do h.uld.r@: S"h.o,uPl.d.:.r l"@h,rr::hho.ld: id Re.loatitv: h:i,ght: Ab .t1@1.. ....9ht: R. : Absoluce area: 90-.00 Led Di 30.0&0b 1.50 0.00: 00 2. 0 0. 0: Dis@bl:d Di &bl d DL:,.,b,,I:,d, P.q. 4 AMELIA 062498:FACT Equipment Log,99114 Qua"ro II,#644SE PAGE DATE: 10/19/99 ANALYST: mmh STLIDY NUMBER:TOX145 MATRDC: ratliverDESCRUMON: dil FACT Method: ETS-8-7.0 injectivoonlume_:Lo_uL Mobile Phase: Cycletime1:0mitLElectrode:z:Rgy-- (A)N2H.,04mCMH3CO2 (B)MEOH TN-A- orstadrdnumber -(A) 99085-10-14 Prepared(datelby): (A) 10/16/99sah Expires: (A0)4/00@ (B)TN-A-2997 (B)10/16/99sah (B) 04/00 Storeatroom texw. M or N Other: Guard colunm: None Parlnwnber: na Lot number. na Analyticalcolumn: KeystoneBetasil Size:2 x 50 mm - TypeC:18 Partnumber: 055-701-2 Lot number:P9EI I Spheresize:5 um Serialnumber.0591816Z Analyticalparameters: Dryinggas(lJhr)3:00 ESI nebulizingas(Llhr)_LO LC Flow rate:300 ulJmiiL Back pressure6:2 bar Sheathgas(L/hr)_2._ HPLC solventgradient:10min-10-95 Time (niin.) 1)0.00 2)1.00 3)5.50 4)1.50 5) 8.00 %B 10.0 10.0 95.0 95.0 10.0 Tuning Method Report Method: C:\MAssLYNX\AMELIA-RATS.PRO\ACQUDB\PFOS1-6KV Printed: Tue Oct 19 10:25:49 1999 -if N,Si if, Page 1 :r ms SOURCE ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. Set 1.60 40 5 0.2 150 250 Rdbk 1.59 -40 -5 153 248 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.6e-3 Hsi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 15.0 15.0 2.0 0.0 4 8 650 Set Rdbk 14.0 14.0 10 11 2.0 0.0 40 39 0 12 650 scanning Hth@d Last Modified: Printed: R.Prt C: \MPA"TKK\AMLIA-RATS. PMO\ACQUDS\ Mon Oct 11 08:22-.17 1999 ICWN-FM-POPA- T- Oct 19 10:22:46 199 12-MMA fol@t r@tL@ Delay I ALAS :I DM of I N"o 0.00 ftir ( ROP- Inter Ch@.1 Delay C Sacs Sp-n i D&lt.ag ) : Start Ti@ I Kin& 0.:.00, 0.00 End Ties Him 1I0.00 Repeats Channel Parent Daughter Dwell (3*CS) Coll Energy (*V) Can@ V 1 413.00 169.00 0.30 30 FUncti" : 2 MM of I )ft.. P"r ( ZXP- I;EeriCh nnelSDalay t Seca I : Sn Ito. ) : 0: Start Time ( Mins End T"W ( Mina @el 1 Parent 499.00 Daughter 99.00 00-0.30 0 00 10.00 Dwell 0.30 (Sacs) Coll Energy (OV) 45 cone so VI rmatim :3 UM of I N"a ftic (RBP- Inter Channel Delay t 5... SSptaanrt (TDi.eIstoInKsim) :I End Ties Hins A.P.SC3 Channel Parent Daughter 1 427.00 80.00 0.03 0 . .0.00 1I0* .00 Dwell (Sacs) Coll Energy IOV) Cone t V 0.30 40 60 r-cti- @ 4 W" of I N"a pair t asp- Intner (Ch)@ :IsDelay S pa Start ?I-'It(nMin)e : End Ties i Him lkep*ats : Channel Parent 1 490.00 Se@ Daughter 78.00 . 00 0.00 10.00 I Dwell (Sacs) Call Energy (*V) Con. I V 0.40 is 60 Masslyrix-Sample Ust Sampie Ust:C:\MASSLYNX\amelia-rats-PRO\Samp[eDB\101999a.SPL Printed:Tue Oct 19 14:10:271999 Page 1 Page Posibon:(1,1) FileName FileText MS File 1 101999001 MEOH IOMIN-PFOS-POAA-IS-PFOSA 2 101999002 MEOH IOMIN-PFOS-POAA-IS-PFOSA 3 10199"3 Tax 145: RBL1013D4-120 bik-11.Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 4 101999004 TTaaxx 114455:: RRBBLL1I001133994-j5veprpb-bIl1k,-E11x.tESxEtESEE10-1103--1939-99 I10OMMIINN--PPFFOOSS--PPOOAAAA--IISS--PPFFOOSSAA 5 6 101999005 101999006 Tax 145: RBLI0139-10 ppb-11,Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 7 101999007 TTaaxx 114455:: RRBBLL1100113399--2550 ppppbb--II11., EExxtt SSEEEE 1100--1133--9999 IIOOMMIINN--PPFFOOSS--PPOOAAAA--IISS--PPFFOOSSAA 8 9 101999008 101999009 Tax 145: RBLI0139-100 ppb-I1.Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 10 101999010 Tax 145: RBLI0139-250 ppb-I1.Ext SEE 10-13-99 IOMIN-PFOS-POAA-IS-PFOSA 11 101999011 Tax 145:RBL10139-SW ppb-11.Ext SEE 10-13-99 IOMIN-PFOS-POAA-IS-PFOSA 12 101999012 Tax 145:RBL10139-750 ppb-11.Ext SEE 10-13-99 IOMIN-PFOS-POAA-IS-PFOSA 13 101999013 Tax 145:RBLI0139-1000 ppb-11.Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 14 101999014 MEOH Tax 145:9RO3237M, Day 4, Control,D:100 IOMIN-PFOS-POAA-IS-PFOSA IOMIN-PFOS-POAA-IS-PFOSA 15 101999015 16 101999016 Tax 145:9RO3245M, Day 1.5 ffig/kgD,:100 IOMIN-PFOS-POAA-IS-PFOSA 17 101999017 Tax 145:9R03246M. Day 1,5 nig/kg,D:100 10MIN-PFOS-POAA-IS-PFOSA 18 101999018 Tax 145:9RO3247M. Day 1,5 rnglkg,D:100 IOMIN-PFOS-POAA-IS-PFOSA 19 101999019 Tax 145: 9R03248M. Day 1,5 ffvfkg.D:100 10MIN-PFOS-POAA-IS-PFOSA 20 101999020 Tax 145: RBLI0139-250 ppb-11-2.Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 21 101999021 MEOH - IOMIN-PFOS-POAA-IS-PFOSA 22 101999022 Tax 145: 9RO3249M. Day 1,5 ffiglkgD,:100 10MIN-PFOS-POAA-IS-PFOSA 23 101999023 Tax 145: 9RO3251 M, Day 4,5 mglkg, D:100 10MIN-PFOS-POAA-IS-PFOSA 24 101999024 Tax 145:9R03252M, Day 4,5 mgfkg, D:100 IOMIN-PFOS-POAA-IS-PFOSA 25 101999025 Tax 145:9RO3253M. Day 4.5 mgfkg, D:l00 10MIN-PFOS-POAA-IS-PFOSA 26 101999026 Tax 145:9R03254M. Day 4,5 nig/kg,D:l00 10MIN-PFOS-POAA-IS-PFOSA 27 101999027 Tax 145:RBL1 0139-250 ppb-11-1.Ext S EE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 28 101999028 MEOH IOMIN-PFOS-POAA-IS-PFOSA 29 101999029 Tax 145:RBL1 0139-H20 bik-I1, Ext SEE 10-13-99 IOMIN-PFOS-POAA-IS-PFOSA 30 101999030 Tax 145:RBL1 01394jver blk-11. Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 31 101999031 Tax 145:RBLI0139-5 ppb-11,Ext SEE 10-13-99 IOMIN-PFOS-POAA-IS-PFOSA 32 101999032 Tax 145: RBLI0139-10 ppb-11,Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 33 101999033 Tax 145: RBL10139-25 ppb-11, Ext SEE 1G-13-99 IOMIN-PFOS-POAA-IS-PFOSA 34 101999034 Tax 145: RBLI0139-50 ppb-iI, Ext SEE 10-13-99 IOMIN-PFOS-POAA-IS-PFOSA 35 101999035 Tax 145: RBL10139-100 ppb-11,Ext SEE 10-13-99 IOMIN-PFOS-POAA-IS-PFOSA 36 101999036 Tax 145: RBLI0139-250 ppt@-I1.Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 37 101999037 Tax 145:RBL10139-500 ppb-I1,Ext SEE 10-13-99 IOMIN-PFOS-POAA-IS-PFOSA 38 101999038 Tax 145:RBL10139-750 ppb-I1.Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 39 101999039 Tax 145:RBLI0139-1000 ppt>-1l,Ext SEE 10-13-99 IOMIN-PFOS-POAA-IS-PFOSA Masslynx - Sample Ust Sample Ust: C:VA4kSSLYNX@amelia-rdts.PRO%SampleDBX1 ol999a.SPL PrintedT:ue Oct 19 14:10:271999 Page 2 Page Position(:2,1) InletFile Bottle injectVolume Sample Type Conc A Conc B Conc C Conc D Cone E Conc F I 10mir@-IG-95 91 2 10mir@-10-95 91 3 lOrt@r@-lG-95 1 4 10n@n-10-95 2 5 10min-10-95 3 6 10min-l(@-95 4 7 lOrr@r,10-95 5 8 10min-10-95 6 9 10min-10-95 7 10 10ftr@10-95 8 11 lomin-10-95 9 12 10mir@-lG-95 10 13 10min-IG-95 11 14 10niin-lD-9591 15 10niirl(@-9512 16 10n@n-lG-95 13 17 10n@r,10-95 14 18 10min-10-95 15 19 10niin-IG-95 16 20 lOrtiin-ID-9581 21 10min-ID-95 92 22 10min-lD-95 17 23 10min-lG-95 18 24 10min-10-95 19 25 10min-IG-95 20 26 10n@r,10-95 21 27 10niin-10-95 82 28 10min-10-95 92 29 10n@f-o-IG-95 1 30 10min-10-95 2 31 10mir@10-95 3 32 10min-10-95 4 33 10mirv-lG-95 5 34 10min-10-95 6 35 10mirlG-95 7 36 10mirIG-95 8 37 10niir@-lG-95 9 38 10mir,10-95 10 39 lOrr@rlG-95 I 1 10 10 10 10 10 10 10 10 10 10 10 10 10 - 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 - 10 10 10 10 10 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - FACT: DATA REVIEW SMMARY FORNI Date: Data Analyst: FACT Study I-le/,/s - Afplv Matrixrrimepoints:-7-aw 14@l, Sunple L@it- /o Set-upAnalyn*s DatelAnalyst Instrument 7,4 s Data Review Sip@Off AnalystReview Name IDate:. F46 TechnicalReview Name/Datc:,49r: ln5L;&@ QuaBly Assurance Review Name IDate: Data Entry-. A)" L4C- ioialigg Comnwnts Jusdfkations: Analytc:_-PAlt 11.1)(D AcceptaLbilnecaRrange.-11-30 Ztl LOQ: R^2: 0. ?figlri F-vuactioBrWt& Matrix B CafibmtionChecks- AIA NISINW:. ,DataStatus: A)IA A..140 r it t,.- k. u u v.,J- -A Iil-- 4,4 a L) d> I'll .1 Analyft: 7irOS rch,7 )'D AcceptableLinearRange. 12.30?3,1 -'> LOQ:_i-I -36 R^2: 0.177,1,z2- Exu=ttBdlank- MatrixBu.@- k. 100- CalibrafioCnheck& NA MS/UM. i))A aro,-J i-7L- 16174[tV 41,.- e." -L I -P.A,,K ).,,- r's V- -Pro;-4,j(a@ejty4v,c,44.1 4,1. A@lfa,/ L, 74@ le,. ZOQ. 7L *IZC41 Anslyte:. ':I@pec#3 AcceptableLinearRange: AIA LOQ: AfA R^2: CalibratioCnheckL 11/4 MS/MSD: ,DataSatw: ExtracteBdlank. MattixBlank- Nk LAC- tol@.qiqq- old, lixtae - ra *,7.1 eaooe le-ss A,, ".@ A61LIf A@OhVk L,/,, FACT: DATA REVIEW SUMNLKRY FORNI Date: Data Analyst FACT Study 7--,cli(5 - Ldv Matlix/Timcpoints: S"le Liit- /0 Z5,?l e- Sct-up Analysis Ditc/Analyst Instrument /0 izg /fl 1 oz Zf fg An.lyt.:PF-S,4 Acceptable LinearRAngc-. LOQ: .:?o R^2: CalibraCthieocnks:A/A MS/WD: NA idataS tus: Ex"ction BW& /,.,7 140 M.= BW@,k Data Review SiLrn-Off Analyst Review Nune/Datc: @-4s Technical Review Name tDate: 4'D PL'.Jt, ILz (Ac. Quality Assurance Review Name /Date: Data Entry: A@oeii@M u Corronents Justifications: LAC,10@.29/91 L--i )7--3) " I -&7L E)." k-@ /I -r- 4,14- 7s 4!gr- 4c)L- Anslyte: AcceptableLincirRange: LOQ: R^2: C&Hbmtion Checks: msmsa. Data Status: ExtracteBdWilL MitrixBB77Z- Analyte: A=cpptmtatabbjllcoeLihnear1R.aa.nnggee-:. LOQ: R^21 : @2. ULiiabb@mfoicok hcoZacrks-. ExtracteBdlank. MatrixBlanL- ta Satus: 0--ntity C@pound 2@ry "PO@@ T=45-r&bbit livex cw@- @t. ILO/22/99WW Staam.ptlemoLdiisfti:ed: @thad: x@t modified. Job Code: C:NMMym\mmlia*92498.PW\SWWIODB\lo2stoc T" Ot 26 09:34:39 1999 C:\Nkg$Lymx\a-li.012418.'W\MMthM\10259*c ?%@ ct 26 09:34-42 1999 pri.ted: T- ot 29 09:43-S2 1999 c@.pou.d 1: POAA gchl) I I 10259903S 2 102599036 3 11 0259 037 4 0259:039 5 11 0259:039 1 0259904 1 02 40 5:1.0 412 9 10 22599043 110 1025599044 @o255::0:5 @2 2 6 13 1025990047 swiplallat ?@t M*OH Blank KOOH Blank TOX145-RBL10229-K2O Blank-1. 10/22/99 IKWW TOX145-RBLI0229-Li,.r,b i..k-i, 10/22/99 R" TOXI:5S:RBL10229 -SPPB1 RBL10229-12ppb TOX145-PJ3LI0229-30ppb-I 10/22//9:gRWW 200/22/99 Rwd 1 /22 PLWII TTOCXX145-RBLI0229-60ppb-I 10/22/9999RHM TOX1145 RBLI0229-120ppb-i, 10/22/ RMW TOX 45:RBL10229 -300ppb-1, 10/22/:9 TTC.XJ1.45,-R.BLI0229-"Oppb-1. 10/22/9: - L 0229-90oppb-1, 10/22/ Rww TOX14.,-PSLI10229-12OOrPPb-1. 10/22/99 Rww TYP- Std C-@ RT 3t..d.@d 3stand rd tt@@d:rd Stan d rd dard Stadard St@dard St&ndard Stndard 6.13 12.30 3 601:'300 123.00 301 613 0 920.00 122 -7.00 :.-::"126 68 6.9731 :.:4'7 6.92 3 6 20 6:9121 6.918 6.924 A@ C..O. Fl.g. %D.@ iao 253.08 bb S.:: bb 1.11@ 119. bbX 42 21.77 bbX 3: 7:.o ma 5 .604 bb 59 3M IS1 454.03 bbX 20603 644.157 bb 25. 897-@06 bb 3 38. bb 877 77 -100 25 2: 4- -2 1 Amlia 092498: Q@titated and Printd by L.s 10/26/99 guantify CaM@nd S@tY_"PO", T=Idb-rMbbLt ll"c m@ "t. 10/22/99 MR $aW'. LL$t; ,.at .difid: w.th@d: ,..at_afid: Ppo\&.Wloa\lo2soo. C:\K%XSLTM\--11-062498 r_ - 26 09:34:30 C:\,,RUMTm\a..11.06241999:.Vpo\oftthDB\20259M T- Oct 26 091:34'-421999 Job Code: Printed: Ttm Oct 26 09:43:32 1999 campound 2: VFW 0 N@ 1 102599035 2 102599036 34 11025:9037 25 9:0389 5 10025 03 67 l1 o25990440 025990 1 6 102599042 9 102599043 10 102599044 11 102599045 12 102599046 13 102S99047 (Ch2) sampidai.t T"t HOOH Blank M.OH Blank T X145-IkBLI0229-H20 BIL..k-1, 10/22/99 Rvw TO 145 -RBLI0229-Liver Blank-1, 10/22/99 RWW TOXX145-FLBL10229 -5ppb-1_1,10/22/99 IkWw TOX145-KBL10229-12ppb :1: 1@00/,2222/,999 RWW ToXI45-PLBLI0229-30ppb- TOX145 ,.LL1@0.2222::'@2O.PPpB,@_,, To TOXI:S-ItBL10229 -300,ppkl TOXJ S-ROL1022"OQPPt TOXI:5- RBLI0229-90*PPb- 1, Taxi S-RBL10229-120OPPb-1, @.122/19 R- 1.012 22/1:: = 10/22/99 RWW 10/22/99 It"" Type Standard standard Standard Standard standard standard standard sSttaanndda&r d rd Std C@ 7. litt 6.14 12.30 30.70 61.40 123.00 307.00 9,4 :0o0 28.(,0 122 0 1.@44.1 7.11246 7:14 17 7 ..1121 7 .1 1: 77.11 119 7. it 7 1.:01916, 1 091 49 33 14 94 16 2 21 352 5 71 $23 2161 3114 445, 6026 C@ . fig. 0.00 bb 0.00 bb 0.00 bb 0.00 b "S bbX 22: 7 mm 3 116.494 bbb 1016.12 b 31 7:1@31 bl 46 bbX 611..,4 bbX 925 9 bbX 0D.@ -52 -2 4 1 4 -24 -26 -25 ftg. 2 gu&ntit&t" AmlLa 062498: printed by 1" 10/25/99 oumtify C-P--d 8-"ry-"P* t TOX245-rabbit llwc aut@ "t. 10/22/09 gample IA&t: Last modified: H.thodt IA&t modified: Job Cod.: C;\wkSSLYM'@mmli&06249.M\SBNPI-DS\10239*C Tue Oct 29 09:34:39 1999 c:Vp.SBLTMX\..&11.062408.rpo\Noth=%1023990 T" Out 26 09:34:42 1999 ftinted: 'r- C@t 26 09,43:52 1999 Caoound 3: 13 4Ch3) I u1 102599035 2 102599036 3 11025:9031 4 1025 9:0369 5 025 03 6 102599040 7 102599041 0 102599042 9 102S99043 10 102599044 11 102599045 12 102599046 13 102599041 sampigaist T"t N.CH Blank NECH Blank TOX145-ILBLI0229-H2O 91=k-1. 10/22/99 RWN T _RB L 11 00229-Liver 31-k-1, 10/22/99 RWW TOXI:L@ "L' 0 229:5ppb-1. 10/22/99 RWW TOX 145-P.BL 2 2Op"pr _ 1". 10/22/99 RWW TOX145-ItBLIO'2:-3 ' 10/22/9: ITWW X 145-"LlD202:2 :2@10p2p.bpp;_li,l1l1.2,12121/ ptww TOX @4@-.L@ :: RWN TTOOXX145-RBLI02229-300ppb-I 100 /22/ RON TOX1445 RBL 0229-600ppb-1: . 1(/122/99 RWW TOXI 5:RgLl10229-900ppb- 1 1 /22/99 RUN TOX145-RRL10229-1200ppb-il 10/22/99 R" TYPO Std C-0 RT Standard Standard Standard Standard .,@t,.r,."rrdd Standard tmdard Standard 1.00 1.000 0 1.00 1.000 0 1.00 1.00 9,: 6:960 :.9929 . 6.93546 :.9g31 . 32 6.:29 6. 12 A@ 371: 220 2692 2725 2635 2559 2230 24009 2 79 2044 1 20 0 c@c. fig. W>@ 1 bb 56 0:'1,'bb -7 1.13 bb 13 1.115 b iI s 1. 1 bl@ 1.09 bbb I 0.94 -6 1.01 bbbb I 0.:7 bb -13 0.966 -14 0. bbbb -14 p.g. 3 Amlia 062496: Quantitated end printed by Las 10/26/90 3-@y 1=14t56-fIy.bcbcwl-t^6li@r @- Report @t. 20/22/99 W" S&MIG LLgt: List modified: Noth.d: Last modified: Job C@": C;%NUSLyMX\&Nsli&0&2498."tO@SaWleDB\10239gc 7,@ Oct 26 09:34:39 1999 C:\b&JNMYMX\-.1i.09249$.M\No-hDB\10239M r@ act 29 09:34:42 1999 lprinted: 'P@ Oct 29 09:43:32 1999 C..P...d 4: IFIC" (ch4) 1 "1 102399035 2 1025::036 1. '01...031 5 1 02 5990035 19 5990 0 67 l1@02225990 4 1 5990 42 0 l(@2 9 10 25990 4 3 10 1025990:4 11 1 0 2599045 12 1 0 2599046 13 102599047 S..Pl&list Txt New Blank X*M4Blank OX@l.,_-.1@Ol@l-.0 10/22/99 RWH TOX ABLI0229-Lilor IOl@lon,l-l 0/22/99 RWN 5ppb- 145-RBL10229- I 22@9,9 Rtm TTO(XIX1145-RBLIG229-12 P - 10/22/ rox 45-ILBLI02291-O3PPpbb:11:. 100/22/:9:9 PRYuWN TOX145-RBL10229-Soppb 1 1 122/ RUN 145-RBL10229-12 Oppb-1: 10/22/:: RYN T" 145-RBLI0229-300P /22/9, RWW TOOXX145-RBLI022 " 00pppbb--1,1, 2100./22/ 99 RUN TCK1I45-RBL1022"00ppb- /22/ RWH Tax 45-RBL10229@1200ppb-1. 1 10/22/99 RWN Type Std C@ .'1ttn:,d:rd Stan d rd rd Standd&a rrdd Sstt@:dnadrd nd&rrdd Standard @21:13 30 30 61.3'0o 123. 307.0000 692103@.o0o0 1227.00 7.7 MT 7.1704' 7.7$73 7.7 7 7.774 7.777 7 772 7:.7'?S 7 .777 7 .773 7 77: 7 .77 6 7 71 07 350 2206: 242 336 644 11 233 S.9,39 1054654501 226279 C-. 71". 34.Oi w 15.55 bb 10.:: bb 7.40 bb @9l. 71 b 32:22 X bbl' 45.73 bb 105 bb 322:."7 bb ::9..4912 bb 12@ 4 . b" 1 39 bb ,D- 53 20 5 7 -14 -5 I 4 4 P". 4 Awaala 062496: O@tiLtated w4 printed by J" 10/24/99 QUUAtify PAV*VT TOX145-rabbAt li@r @- @t. ID/22/99 JWN ompoundIname:POAA (Chl) .CoefficieonftDetermination0:.996986 iCaIibraticounrve:0.253166 * x + 36.3287 ',Responsteype:ExternalStd,Area Curve t3rpeL.inear,Origin:Exclude,Weighting:I/x,Axis U=: 350- None Response- U. ---O.o Amila 0"498: Qu@titated 200.0 406.0 and printd by La. 10/26/tg 606.b 806.0 1000.0 Conc! 12FO.0 Cr-tify "Ilb-ts- R-P-@ TOX145-rabbit li@c m@- "t. 10/22/99 Mw C6-nip-6un2dname: PFOS (Ch2) CoefficienotfDetermination0:.992922 Calibratiocnurve:6.34685* x + 149.692 esponsetype:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:1/x,Axis U=: 7.94e3- None ftg. 2 Response- 0 o.o 20b.0 400.'0 Amlia 062498: C@k@titated A" printed by L@ 10/26/92 6'06.'0 8'06.'0 lodo.o Conc 1200.0 0-tity CaiibratA@ RePort TOX143-rabWt I&@ .- t. to/22/99 "w ,-Compou3ndname:IS(Ch3) Response Factor.2378.96 :Responsetype:ExternalStd,Area Curve t)rpeR:F 2.73e3- ftg. 3 Response- 0 0.0 0.1 0.2 0.3 0'4 0:5 -0.6 0.7 0.8 0.9 A@lia 062499: Quantitated and printed by Las 10/26/99 Conc gt@tify CalibMtlm PfflP*ct TOX243-tabbit IiWr @- *Xt- 10/22/09 RWW Coe@ficioefnDteterminati0o.n9:96087 Calibratiocnurve:17.5980* x + 76.6733 :Responsetype:ExternalStd,Area 'ICurvteype:Linear,Origin:Exclude,Weighting:I/x,Axis =m: None 2.26e4- Responsex 0 1 0.0---T A@lia 062498; Q@tLtatod 260.0 @00-0 WA psinted by 1" 10/24/09 600.0 800.0 1000.0 Conc 1200.0 M*Chod Report *thod file: L@st modified: Compound: Printed: C:\MSSLYNX\-li&0624 :$.PRO\MethDB\102519c.adb Tu* Oct 26 09:34:42 1 IC 1: POM (Chi) Tu, Oct 26 09:44:34 1999 C1ll,po.-&d N 9 t@.ri - ,I "T*r!-:; Cone.t Ofy stancdoards: U::r RpeF.Val e: tr r ctor: u n egratek @dow F!ct r: Ichromotogr,wl mass I.Z.: Peak Location ::t:tntion Time @.i") 1 i@* Retention Time ItT Rafor*nca: Time Window [sifts): Peak Selection: Response R.:p@ a. Type: R. P.Z.: Calibration Curv*s Polynoui&l Type: Point of Origzn: rit W*l )Lxls'rqrhotnisnfgo:@tion: Concentration PORA TICN Com. (Chli s 11 .00000000, Disabled 2..000000 0 1.0000D. o ooo: 0INOel .252 Dilb s&bl.d Nearest Lx @l Alto.. Li ear Ide Lc IN/oX- u.0n@i.t:: Peak-to-pook amplitude: S=Oth Sw thinq: minzw SIZ* lscans) 14u'bter,of amo ths: 5-o h ng method: Be.. i vall*y threshold: JRoeduce peak tallinqRaise baseline Peak Separation Dratwacvt*rtical threshold: D. shoulders: Shoulder threshold: Response Thrtshol R.latuit,: h.ight: Ab.@i ight: he 04 R*Iative or : Absolute area: 91 Lmblod 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1 50 Disabled :: &bld 0@.o-o-, -Dii..b ad 0.00, Disbi1.d 1/t2 Method Report method file: Last modified: Compound; Printed: C:\MASSLY)IX\@li&062490.PRO\XethDB\102599C-Odb Tue Oct 26 09:34:42 1999C 2: PROS (Ch2) Tue Oct 26 09:44:34 1999 Compound Name: R.t.: Quantxfy Trace: conc. of Standards: User Rr value: user Peak Factor: integrate Window Factor; Chro@togran,@ss window: Peak Location Retention Time lnins): FtelativeRetention Tim.: RiT.R..fir. c.: T N ndow (man3): Peak Selection: Response R:sppoonss*e: Type: C.I@brati_,nCu-40 poiynmiai ?Ype: Pointeoif Origin: AFxiits NTraqnhstfionrqm:ation: Concentration units: N. peak-to-peak amplitude: Smooth s@ t ing: Windowh Size (Scans): mumoor of smooths 3moth,ng method: B.@eli ... in valley threshold: jo Ik:d,ce R is. p "'q: Peak Separation Dratwecvtertical threshold: D. shoulders : 5.,h.,.:iOdn*.r.tThh@r::,ho,ldd: Relatitv: h:ig t: "30 Relat'ive h r!qh:t: Ab..lots at*&: PFOS ICh2) (man*] TIC r-o= . A 1.000000, 1.000000 2.000 I.OOOOD. Disabled 7.109, E"bled 0.000, Disabled IN...] 0.227 nearest zxto=al Area. Li *or Exclude I/X Mon. 96 C..bld 2 300.00 2 0.00 5.00 '@0...*bol.d 30.00 1 50 D :.bled :00, Dii. bl*d 02.00, DL &bid 0.00, Disabled page 2 Method Report Method file: Last modified: Compound: Printed: C;UWSLYNX\&"11&06249@.PltO\N*thDS\102599c..db Tu. Oct 26 09:34:42 1999C 3: IS ICh3) Tug Oct 26 09:44:34 1999 Cmpound N"O: Internal R.f.: Quantity Trace: ConC. of Standards: user RF Value: Ustr Peak Factor: Integrate window Factor: Chro@togran mass window: Peak Location ecention Time FRtelative Retention Time RT T Reference: &.. Wind- (sins) Peak Selection; Response Response Type: Response; Calibration Curves Polynomial Typo: Point a in: Fit U41ifghotriingg: is Transto @ tion: ACxoncentration units: Note. Peak-to-peak amplitude: Smoth 3-' thing: (scene): umber f moths: Sm tIhin ng method: as Bas: i J i C:all:y thrals@h ld: R:dn bpasel)itnteai"x noq: Rai u a Peak- Separation l@: Dratwocv* rtical threshold: D. t shoulders: Shoulder threshold: Response Threshold Relati : h iqht: Abso luvt h:ight: Relative r.@: Absolute area: 13 (Ch3) (No..] TIC rixd 1.000000, 1.000000 2.000 1.0000D. Disabled 6.924, 0.000, Imn.) 0.252 Enabled Disabled Nare.t zxtaz@l Areas Linear C.Clxw I/X Mae 74 2 I 23000-.0000 5.00 90.00 Disbi.d 30.00 D1)i:&blod '0o-o": 20..0.0.,, .i abl d Di..bid Method Report I Method file: C:NKOLSSLYNX\@li&062496. PRO\MOthDB\102599C 'NAb Last modified: Tu* Oct 26 09:34:42 2929C compound: Printed: 4: PROSA (Ch4) Tu* Oct 26 09:44:34 1999 Compound Ninternal Rot.: ouantify Trace: Conc. of Standards'. User RF Value: User Peak Factor: Integrate window Factor: Chro@togr@ mass window: Peak Location I,- Time: Relative ltecenti.n RT Rtf.ftnC*: Time Window loins): Peak Selection: Response a.sp.". Type: R.Spo...: Clibratl_*" CIM" Polynomial Type: point Of OrigLA: Fit Weighting: AXLs Transto @ tion: Concentration Unit.: ".I.- Peak-to-peak amplitude: Smooth 3- thing: Window sa iz: too@l: Number f Smoothing mth@d-; : B ...It... Join valley threshold: R duct peak tailing: R:@@. b... line prom lch4) [on*] TIC co.c. 3 1.000000, 1.000000 2.000 1.000OD& Disabled 7.851, 0.000, IManel 0.311 Enabled Disabled U..r..t zxt.@l Areas Linear Kxclude I/X Mon. ]is Enabl*d 2 I 30.0000 2 0. 5.00 t... I threshold: Da - shtoculder.:1: esho Shoulder Response Thh@reshol1d Relati@ : h lght: Abse lut h:iqht: Relsaotiuve :r:aa Ab 1 t. r 90.00 DISbl*d 30.00 1.50,, 02 .00, o.'oo, Dlalbl*d Di abled Di:abl*d Ci b ad p.g. 4 AMY,LIA 062498: FACT Equipment Log '99114 Quattro11,#644BE PAGE DATE: 10/25/99 ANALYST: ias STUDY NUMBER. T0145 MATRIX: RabbitLiver DESCRIPTION: Curve FACR Method: ETS-8-7.0 Injectiovnolume: 10 uL Cycletirw:10min.Electrode:i:@@. MobilePhase: (A)2.0mM NH4CH3CO2 (B)MEOH TN-A- orstadrdnumber '(A)99085-11-3 (B)TN-A-2945 Prepared(datefby): Expires: (A)IO/21/9s9ah (A)04/00 (B)10/20/9i9as (B) 04100 Storeatroom temp? [flor N Other: Guard coloimn:None Partnumber.na Lot number-na Amalyticaclolumn:KeystoneBetasil Sizc:.x2 50mm - Partnumber:055-701-2 TypeC:18 Lotnumber:P9E II Spheresize:5 um Serialnumber:0591816Z Analyticaplarameters: Dryinggas(L/hr)3:00 ESI nebuhzingas(L/hr)0 LC Flow rate3:00 uIJmin. Back pressure6:2 bar Sheathgas(LJhr)l HPLC solventgradient1:0min-10-95 Time(min.) O/oB 1)0.00 10.0 2)1.00 10.0 3)5.50 95.0 4)7.50 95.0 5) 8.00 10.0 Tuning method Report Method: C:\MASSLYNX\AMLIA-RATS.PRO\ACQUDB\PFOS1-6KV Printed: Mon oct 25 10:13:58 1999 Page ms SOURCE ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. Set 1.60 40 5 0.2 150 250 Rdbk 1.60 -60 -6 151 250 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.5e-3 msi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 15.0 15.0 2.0 0.0 4 7 650 Set 14.0 14.0 10 2.0 0.0 40 0 650 Rdbk 46 39 48 Scanning method Rupert Method: Last Modified: C: \K%MYWC\ANKLIA-RM. M\ACUMB% Mm Oct 11 O8z22-.17 1999 P..nt.d: Mm Oct 25 lO:l3t3* 1999 ICBM-F"-POAA- 12-PyD" gol~t Delay I &no I : 0.00 runction : I "M f I Mae. ft&. t ILAY@ I.c., Channel Dl.y Span ( Daltons ) : Start TL&e I Hins I End Ties Mi.@ 1 Sacs 0.03 0 ....0o0 10.00 Channel Parent Daughter I1>@ll (Se") Call Energy 4@V) Cone V R&pe&ts 1 413.00 169.00 0.30 30 is FunctiL@ : 2 MM f I No. ft.@ ( Ksp- I.t.r Channel Delay I S... Span ( Daltons ) : start @I.e,'* I Hlns 1 En. T n 0.03 a- 00 ..0 0 00 jk*p*atsChannel Parent Daughter Dwell JS@) Call Energy (.V) C... V 1 499.00 29.00 0.30 45 60 function : 3 Mm of I Mass ftir 4 tal@ Intenr (Chom:l Delay SP& start It ns ) : T@Do. I MLns ERnd Ti.* Hin@ Socs I : 0:*3 .0 0 ..o 10.00 *p Channel Parent Daughter Dwell fS*" Call Energy I*V) Con. V 1 427.00 00.00 0.30 40 so F@c"cn ;A )am of I Has. F"r (asp- Inter Channel Dlay Sacs 0.03 SSp. n ( Daltons ) : tart Ti@ ( Min3 End ,aTies t Hins 01 ..00.00 0 00 . .p Channel Parent Daughter Dwell (S@) Call Energy (.V) Con* V 1 496.00 70.00 0.40 45 60 method Report Method File: Last Modified: Printed: c,\maoslynx\amelia-rats.pro\acqudb\10min-10-95 Monday, October 25, 1999 10:12:15 Monday, October 25, 1999 10:13:44 RP1100 LC Pump Initial Conditions Solvents At B 96 C96 Dt Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Oven Temperature Right(OC) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 EP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are Time A!k B ?4 cir 0.00 90.0 10.0 0.0 1.00 90.0 10.0 0.0 5.50 5.0 95.0 0.0 7.50 5.0 95.0 0.0 8.00 90.0 10.0 0.0 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are Time Initial 0.00 0.10 Column Switch Off Off Off Contactl Off On Off Contact2 Off On Off D% 0.0 0.0 0.0 0.0 0.0 Contact3 Off Off Off Flow 0.300 0.300 0.300 0.300 0.300 Contact4 Off On Off HP1100 Autosamplar Initial Conditions Draw Speed Eject Speed (Al/min) Draw Position (mm) Stop Time (mins) Injection Volume(Al) Vial Number 200.0 200 0.00 9.00 10.0 13 Page I Pressure 400 400 400 400 400 Masslynx -Sample Ust Sample Ust:C:WASSLYNX@amelia-mts.PRO\SampleDB\iO2599c' .SPL Printed:Mon Oct 25 10:13:121999 Page I Page Positon:(1,1) FileName FileText MS File IOMIN-PFOS-POAA-IS-PFOSA 1 102599035 MEOH Blank 10MIN-PFOS-POAA-IS-PFOSA 2 102599036 MEOH Blank TOX145-RBL10229-H20 Blank-1,10/22199RWW 10MIN-PFOS-POAA-IS-PFOSA 3 102599037 TOX1 45-RBLI 0229-Uver Blank-1,10IM99 RWW IOMIN-PFOS-POAA-IS-PFOSA 4 102599038 5 102599039 TOX1 45-RBLI 0229-5ppb-1,10/22199RWW IOMIN-PFOS-POAA-IS-PFOSA IOMIN-PFOS-POAA-IS-PFOSA 6 102599040 TOX145-RBLI0229-12ppb-1, 10/22199RWW 10MIN-PFOS-POAA-IS-PFOSA 7 102599041 TOX145-RBLI0229-3oppb-I 10/22/99RWW a 102599042 TOX145-RBLI0229-60ppt>-I: 10/22/99RWW IOMIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 9 102599043 TOX145-RBL10229-120ppb-1. 10/22t99RWW 10 102599044 TOX145-RBLI0229-300ppb-1. 10/22/99RWW IOMIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 11 102599045 TOX145-RBL10229-600ppb-1, lor22/99RWW IOMIN-PFOS-POAA-IS-PFOSA 12 102599046 TOX14r>-RBL10229-900ppb-1. 10/22/99RWW 13 102599047 TOX145-RBL10229-1200ppb-1. laramg RWW 10MIN-PFOS-POAA-IS-PFOSA InletFile 10min-10-95 lomin-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 lomin-10-95 10min-10-95 10min-10-95 10min-1,0-95 10min-10-95 10min-10-95 10min-10-95 Masslynx - Sample Ust Sample ListC::\MASSLyNX\amelia-rats.PRO%SampleDB\102599@.SPL PrintedM:on Oct 25 10:13:12IgN Boftle InjecVtolume 1 92 10 2 92 10 3 12 10 4 13 10 5 14 10 6 15 10 7 16 10 8 17 10 9 18 10 10 19 10 11 20 10 12 21 10 13 22 10 Page 2 Page Position(:2,1) FACT: DA'RA REVIEW SUNILNIARY FORNL Date: Data Analyst 5@s FACT Study t/qs- Matrix/Timepoints:-7@,. SampleL.@L- Set-upAnalysis Date/Analyst Instrument OZf f2 Anslytw 7oA,* Aczcpt&MeLinearRinse. LOQ: EdmtionBknicAIA_ R^2: CalibmfionCheck& Matrix Blank WA nk- 4Lwe- i/- Data Rcview Sign-Off Analyst R"icw Name/ Date:-sit-$ I.I.-flfz Technical N somm Qua0ey Assurance Review Nam /Date: Data Entry- poko-r CAnwbents/Jusdfkations: 7r, !@'0-2ggL-,j tl W& i@ ltss- 7L &r,, I iA Ctiltyi1i ID&taStiaw. Anslyte: A=cptitbiLcinearRange- LOQ: /o/ R^2: ExtractBeldankNA MatrixBik IVA CalibratiCohnecks: Ilk - P4.@.4@ NISCASD- 0)@ / /100it 004 Idof FA VLJI AoCfWFT-1@7 DatSatRhw. 7L-5,--:3 L A-1 eU 4.;,./,25S -4 Analyte: A=cptableLinearRAnge: LOQ: _ 7<.,b 411 R^2: CalibratioCnhecks-. n:L ExtractedBlank t44 MatrixBlank m&NmDID.t. St= L9.2/ @Q. Ivm- -7va /Lrw f &v &bN* IV,It, Ale k #,k4l 7@/ #15 DW- * erixiv;"] ,4,c- i@t 7L lp)v@.L T a 0445,rj, /a" c/ 4.,Jel L,- FACT: DA,RA REVIEW SUNliNIARY FORINI Lkc Data Rcview Sign-Off Date: DaL2 Analyst l@K AnalystReview Name / Date: FACT Study#: Matrix(Timepoints: Smnple L@sL- /o 57A-d',-, Set-upAnalysis Date/Anaiysr. Ilzrit@ Instrument: -e-i 4YZZJff TechnicalReview Name / Date: Quality Assurance Review Name I Date: Data zany. Canmwnb IZMtions: Ana": AcceptableUn=r Range: LOQ. NA R^2: NA CalibratioCnhecks- A-14 MS/MM),DataStatus: E=wtion BWk Nk Matrix BWk 7r, Z,.,/ A,e.. loll i-- -7@ ZA4Te. X,.- Analyte: AcceptableLinearRange: LOQ: R^2: CafibmtioCnh=ks: E=wtod BW:BkwBk,Wk' MatrixBWk -14. sa-21/1 r. f I.-i 911,@ DatiLStatus: Anslyte: AcceptableLinearRange: LOQ: R^2: Uibmod@on Ccc7occZkkLsmsims Data tus: ExtractedBlank-. Matrix Blank: ?=&S-t@ to 6060 -fix@tim- rpm/VVGWWPC" @t. 10/28199 1" Samio Litsit: : &net modi ad method: L@t modified: Job Caft: C:%IQSSLT=N@"020199.pro%Samgaa=%102699& 0= 29 07:02:5:11:99 Fri c:%m"xLyxx%-vo2 9 V-%Mtb0b%202099@ Fri O@ 29 06:33:25 1999 P.L@.d: Fri Oct 25 07:37-.23 1999 compound I- VO&A (cha) f1 n@ 102099001 2 3 11 02:9999000032 s 102:9990004 10a 28 99 00 5 6 2899 006 78 1002 8 9 9 0 0 7 9 1 .22 . 9, 0 .1, 1 90 10 10a 2:::010 11 1 2 Oil 12 102899012 13 102:99013 14 1028:9014 15 102 ggg9o015 16 102 16 1IL7 102899017 3 102899018 19 102899019 201 100 2:::0020 2 1 2 aggo 21, 22 102 22 23 102899023 24 102999024 25 102:990a25 26 1 2 99 26 27 102:999027 2 2.:,02: 2: ll*.2 02 samplelint Text MI.OU Dik M.09 lk rCKix399086-43-1. lpvb- :/10/99 IMM rcxi.:9:00:6-43-2: Sppb- /10/99 RW FCPL- 9 6-43-3 loppb- :/10/99, RW Mux-99086-43-4. FCK@-99086-43-5. 21]ppb- 110, soppb- 911.199, RrWa,@4v : IOOOPP - 9/10/99 RWW rcr_- -43- 25 ppbb- 9/10/99 RW FCKix 99086-43-8, SOOPPB- :/100/:9 RWW TCR-- -99086-@L3-9. 750ppb-K.OH Olk /1 / 9 MM TOX145-5,PPC)S / PCI*A in T@-da'a-2ppb-0120/28/99, ZAS T03U4 - rOS/PGAA in 4,ppb- / I/ 9 TAS rCRix-9k9096-41-4, 25ppb- 1/10/9, no I N.On al TOla4 5-PPOSA in T@-d@.T200VP- 10128/19 XAS TOX245-PrOSA in T@@- 100ppb- 10/28/99 TAS rCXi.--99086-43-7. 25OVpb- 1/10/19 MW M.09 Rik rCKi.-99086-43-1, lppb- 9/10/:9 mm /10 rFCcK,i,xL-i:9x9:0.8,6:-:433--3,:, @Q.V1pb- 110/9974M -43-4 25ppb- 91//10/9, ?aw" rCMix :900:6-443-S: 5..01 111*11 :,1 rcm@ - 9 6- 3-6 Oppb- 1/ 0 RW ?C&i.-:90:6-43:7: 250OPPb- 9,/I(C,,/9O:W rCKil-,:00.6-13_98. 7SOopob- :,1.,99 rcx"- 6-43 ppb- 1 9 MM 231 Standard Standard S, and@d Standard t,-,@d 's@---Id S.5tandard Standard t---@d oc QC Standard Standard t..dard S tandard 5 tandard Standard tandard :tand@d Std C@ RT 1-00 12 05*0100 IL5D0'O":2oo0 2SI.0000 5052.00 7 2. 25.10 7 01 43 7:.0807 7.OBS 7 ..009827 75 7 110 7.:102 7 ill 7 10360 7.1 7.125 7 L29 .00 251 7.111 7*106 7.132 1:.2Il 5 .00 10 10 2550.20 100.00 251.0000 17@12:.o 2 7:121 7 .22 7 . 130 7 .157 7.L25 7 130 7.133 7-12: 7.12 A@ TI.G. c@ . %D- 17 M 378 bb NK @1a3 36& bb 713 bb 1IO7O8S0 bb bbX 39919 bbx &47 bb 415 bb 229 m 413, bb 43 5 m 77 bb 1: m 4 bb 21925 Mbgb 1g2l2 bb bb bb 34105881 bbXZ -15 0.:s9 26 10.39 -4 24.79 1 48I-064 2:. - 1'3 407:3 541.426 0.00 515.33 .07 28.36 4 -1-'4 -289 13 55 5.45 7.55 240.01 -4 1.1,0 105 1 &.7 a - 2r.71:.1420 1529 10 6.0 .:.:' l2' &28.0 0 -1-5 553.150 -26 SOUP 020121: Q@titated and printed by Lee m 10/21/1, Q@tify compound am---Y a"-= T=45-t-- so dome omfi@tim- "ON/Pro"/POAA @t. 10/24/99 1- &mW%. List: C:UUSSLTMZ%20WC20199.pm%SMMIo=%ID2899& L@t ="ifi"; rri Oc-t 29 07:02:56 1999 ez%MBSLTSM%sOW2013D.PCO%Mth=%1"2@99. lfttb".. l@t modlfi*d: Pvt Cat 29 06;33%35 1999 Job oDd.: p.i@.d; Fri Oct 29 07:37223 1920 compound 2: pros (CU2) 0 s@ 1 102399001 2 102599002 3 102099003 & 102B99oo4 5 102899005 6 102899006 7 102899007 8 102899008 9 102899009 10 102099010 11 102899011 12 102899012 13 102899013 14 102899014 15 102899015 16 102899016 17 102899017 18 102899018 19 102899019 20 102899020 21 102899021 22 102899022 23 102899023 24 102899024 25 102B99025 26 102899026 27 102899027 28 102899028 29 102899029 5-pi.list fmt N.OK Rik N.OH Alk FC]L--99036-43-1. PCX_-99056-43-2. rcx_-99006-43-3, PCXix-99096-43-4, FCltix-99046-d3-5. rcxi_x-99086-43-6. FCKi.X-92086-43-7, FCKix-99086-43-8. YCKix-99026-43-9. lppb- 9/10/99 RNW Sppb- 9/10/99 RW lovpb- 9/10/99 RW 25ppb- 9/10/99 RW 50VVb- 9/10/99 RW IOOPpk@- 9/10/99 RW 250PPb- 9/10/99 RWW SOOVPB- 9/10/99 RW 750ppb- 9/10/99 RW NOON Slk TOX145-pros/poAA TOX145-PPOS/POAA in T@-dos*-2ppbin T@---4ppb- 10128199 LAS 10/28/99 L&S PCMix-99086-43-4. 25ppb- 9/10/59 Rw X.OH Blk TOX145-VTO" In T@=-fts&-200ppb- 10/29/99 ILS T=45-PPOSA in ?@n-M-300ppb- 10/29/99 XAS rcRix-t9O86-43-7. 250ppb- 9/10/99 RW K.OH Blk F-i--99086-43-1. FC3Li--99086-43-2. rcmix-99086-43-3. FCmix-99086-Al-4, YCKi.--99086-41-5. FCXix-99086-43-6. rcxix-99086-43-7. FCXix-99086-43-8. FCKix-99056-43-9. lppb- 9/10/99 Mm 5ppb- 9/10/99 XWW 109pb- 9/10/99 RW 25VVb- 9/10/99 ON 509pb- 9/10/99 RWW 2009pb- 9/10/99 RW 2SOppb- 9/10199 RWW 500ppb- 9110/99 RW 750ppb- 9/10/99 Bw ?"* Standard Standard Standard Standard Standard Standard Standard Standard standard oc QC St Standard Standard Stod"d Standard Standard Standard St---rd standard ftd c@ 1.01 5.03 10.00 25.20 50.30 101.00 252.00 503.00 755.00 25.20 252.00 1.01 5.03 20.00 25.20 SO.30 101.00 252.00 501.00 755.00 RT 7.243 7.265 7.226 7.268 7.247 7.248 7.25& 7.247 7.272 7.287 7.290 7.289 7.291 7.287 7.292 7.294 7.273 7.267 7.294 7.288 7.283 7.287 7.268 7.295 7.286 7.291 7.355 7.289 7.266 A@ 9s 33 109 442 905 2086 4177 8256 21703 39235 54526 167 29376 30229 2326 55 30004 29852 22582 AS 141 514 987 2248 4459 9735 22119 38876 53247 F2&9& xx nt bb bb bb bb bb bb bb bbX bbX bb bb bb bb m bb bb bb bb bb bb bb kb bd bb bd bbx bbX c@. 0.63 0.14 0.79 4.67 10.07 23.83 48.19 95.72 252.39 456.65 634.82 1.47 341.79 3SI.73 26.62 0.16 349.11 347.34 262.63 o.s4 1.17 S.51 11.02 25.71 51.17 101.29 2S7.24 452.47 619.91 %0" -21 -7 1 -5 -4 -5 0 -9 -16 6 4 16 10 10 2 2 0 2 -10 -19 P@. 2 SOW 020199; Q@titated and printed by i- m 10/29/910 9%@tif cmwou" sum@ry T=45-ty@@ go do*. oonfi~ti-- rvos/ryo"/POA& amiole ust: L"t xw"fiod: l@t modifid. Job C.": I.L.t.d: Pri Oct 29 07:02:56 1229 Fi at 29 06@33.33 1999 rcL Oct 2$ 07;37z25 1999 16/24/99 1- Cc.ipo%md 3: Pro" tC3L3) 0 a1 102699001 2 102899002 3 102899003 4 102899001 5 102::9005 67 1 0209:006 a 1 2899 007 10 2 006 102899009 10 102:9:0010 11 102 9 11 12 102:9:0012 13 10239"0 13 it 102 14 15 102699015 16 1 2:9:0176 17 1 002.9,go01. 1: 1028,901 1 12 19 201 102:99:002201 2 102 2 102 99022 23& 102809999002243 256 10022899999002256 2 102 27 2899027 289 102899028 2 1 2899029 a-ml.li.t 1-t NOOK Rik K.OH Rik rCMix-99086-43-1. lppb- 9/10/99 SW rCMix-99086-43-2. 5ppb- 9/10/99 RW rcmix-:900:6-433-3 IOPvb- 9/10/9: FCMJX- 9 6-4 -4: 25pyb- :/10/" RWW "ix- 990:6-4,3-:: 50ppb-_ rcm@ 990 6 Oppbb- rcKix-990 6:133-7. l2o5opp YCMix- :90:6-43-:: 755O0p0pPVbb-rckix- 90 6-13- 1101199RW PMW 9//1100/99 RWW 9/10/99 RWW 9/10/99 MM K.OH,BSlk To= 45 -pro ://poak Taxi -pro POAAL FCKix-19066-13-4. J. T-.-ds :-2ppb-0120/2:/99 XAS in ppb- I / B/ 9 IRS 25pTp@b--/-9- 10/99 RW MOOR Blk T=15-:1. i..T@.-do..@200ppb- TOXI 5- ROSA L. T-.---300PPk-- 10128/99 10/28/99 I.AS rcmix-99066-43-7, 250PPb- 9/10/99 MM KP.COXH,-:a:lOk ix :::43-1: llppb-:/100/;9- 3-2 5ppb- /1 / 9 RWW rMix-::00::-113-1: -9'...-13-_4 . rCKix -990&6 -43 5 rCKix-ggo$6-43_6 ycnix -99086:43_ 7 3 "ix-99-086-43 llgvb2SPpbS1O0PPB - 0250ppb- Sooppb75OVpb- :110@1,:' 911 0": /I10/99 PW :9 /100//9999 Yyw" 9/10/91 "r&Wv TYP- Standard st d SS ttandard Standard Standard St,@@d andard St QC ()C Standard tavad&rd 5 tandard s Standard S.-d"d andard Standard tand@d a" C- 1.01 5.03 10.10 25.10 1 501.30 0 -000 503*00 754:000 10 25. 251.00 1:001 @L..1.@,1 25.100 ..510-3000 251 *00 :00 !S03 75&.00 UT 7.811 7.802 7.766 7.786 7.764 7.765 7.771 7.71.5 7 7:.:26 7 $31 7*:293 7.45, 7:441 7. 3 7.$S 6 7 335 7.IS2 7..68323, 7 7.:2-Il 7 7:.2: 7.836 7.:21 7:@31 7.830 7 . 30 7 806 A@ 559 204 762 2539 4612 '1L1o7g.o: 3375 1'17.1 2005809 301294 2511 4293752 4315922 63186 12460 1302369 4271995 139170 24236 :217 Flag. db xm NNX bbX MM NK bb bb bbbb bb M bb bb MM M bb bb "mH OU c@ 0.00 0.00 0.00 0.00 2.11 17.23 39.600 %D- -100 -100 -79 -31 -22 2:6 - 14 -4 499 - 806 -21 7273.:0106 -4 104590.7S 105385 37 141.:25 479 10525.215 10&301.2 .802 379 .093 51 27 10.972 91181 921:10 IMM= 1:95554 bb 1 .7 41 150011 bb 2 2 701.01 bb 301AS90 bb 1130. 11a 343 31 -29 25 :26 115a47L.60 186 2 12@.'.@0l' 1' 73S.'21 -2& p- 3 Soup 020199: Q@titated and rclatod by i@ m 10/29191 gt@tity Comwound S@@Y VAV=T TIC=45-t@ SO DOSO 0=91-ti"- Fros,,=WpCAA om. 10/2$/gg i- @.MIS List: L"t modified: kftth.d: L-t "Lfld: Job co"; C:NWMSLTM%ao.PO20199.PM%SMMISM%202@99& rri Oct 29 07302.36 1999 C:%MUSLMM%.OUV020191.pro%mth=%IL02411. Fri Ot 29 Of@S3.35 1919 ftint.d: irriOct 21 07:27s23 III$ Coopm-d 4: 12 (CbA) 0 MW- 1 1028,9001 2 102899002 3 102899003 4 102899004 5 102099005 6 102099006 7 102899007 0 102899008 9 102899009 10 102899010 11 102099011 12 102699012 13 102899013 14 102399014 15 202899015 16 102899016 17 102899017 15 102899018 19 102399019 20I 102:9,9020 2 102 021 22 102B99022 23 102899023 24 1002:99:002& 25 102899025 26 26 27 10223a9:027 28 102 9 028 29 102899029 2.0101tat Tm ti.OH Blk R.Off alk rCXix-99096.&]-I. rCXi..-99086-43-2. FCXx-99086-&3-1. lppb- 1/10/91 M Sppb- 1/10/99 nm loppb- 9/10/19 ram TCKix-99086-41-4. 25PPb- 9/10/19 FMW TCPLiz-99006-43-5. SQVPB- 1/10/19 ON PCKix-99086-43-6. IOOPPB- 1/10/1, RWW rCKi..-99086-43-7. 250ppb- 9/10/99 sww r-i -99066-43-8, 500ppk, 9/10199 mm rCmi.-99086-&3-9. 7SOppb- 1/10/99 MM U.= Alk 7=45-FrOS/POAA 1=45-pros/POLA in To@-d-e-2ppb- 10/28/19 US in T@n-m-4VPb- 10/28/99 XAS F-@ -99086-43-4. 25ppb- 1/10/19 ymw M.= Blk T=45-ppoSA I. l@-d@..-20OVpb- 10/20/99 XAS 7v=&S-PrOsA in T@---300VPb- 10/20/99 'As rCkLix-99086-43-7. N.OR Slk TCRi.X-99086-4L3-1. PCnix-91006-43-2. rCUix-19086-41-1. 250ppkl 1/10/11 MM lppb- 1/10/19 PW 5VPb- 1/10/91 MM loppb- 9/10/91 MM rCXix-990:6-43-4 rCKi.-990 6-43-3: rcx_-99086-43-6. PCKix 9,90:6-43-7 250ppb- 9/10/19 AW S ppb- '10 /99 lww 100OPb- /10/99 RW 20500ppb- 9/100/99 MM rcx_- 5'appb- 1/10 1:.,.-:4"3--:. 7 vpb- 9/1 111: RW TYP- standard Standard Standard Standard Standard Standard Standard Standard standard QC oc sS@t.-@d d Standard Standard Standard Standard t SS tandard std c@ ar 7.081 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 7.083 7.102 7.101 7.103 7.109 7.102 7.105 7.120 7.124 7.124 7.120 7.L24 1.00 1:00 1 1.00 1.00 1.00 1.0000 1. 1 1 *00 7.L2$ 7:1274 7 7.145 7.143 7.12S 7.151 7.141 7.147 7.141 7 145 7 L21 A@ 71.0. 16 bb 4165 bb 4646 bd 46&3 bb 4SI4 bb 6546 bb 4172 bb 2878 bd 2479 bk. 2203 bb 3463 bb 3528 bb 3185 bb 3671 bb 35&5 bb 2681 bb 3119 bb 3041 bb 2979 bb 2937 bb 2907 bb 2950,7 bb 244S bb 22.11 bb 2 2 bb C@. %o@ 0.00 -100 1.26 26 1.40 40 1.40 to 1.45 45 1.37 37 1.26 26 0.37 -13 0.75 -25 0.67 -33 1.05 5 1.07 7 0.96 -4 1.11 11 1.07 7 0.81 -19 00.14 -6 .92 -8 0.90 -20 0.99 -11 0.88 -12 0-13: -122 0*74 -2: 0'64 -3 P.g. 4 Soup 020191: 0---titated A" printed by i@ 10/29/19 Q@tit C&"brati= ROP@ 1=4s-ty-" so d... pmo/pro"/VO" -t. 10/24/99 1- Compound 1 name: POAA (Chl) Coefficienotf Determination:0.996938 Calibratiocnurve:7.35186 * x + 10.5814 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighbng: 1/x,Axistrans:None 5.54e3- Response- x n 0.0 Soup 020199: Q@tit&tod -ionn prtated by L" m 10/29/99 @60.0 Conc o@tity c 2=45-t-t ibwatim 90 6- R@m omfi-ti-- '"a/ "ow"m . to/28/99 I- Compoun2dname:PFOS(Ch2) CoefficienotfDeterminaflon0:.999345 Calibratiocnurve:85.8285 * x + 40.9705 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighbng: 1/x,Axistrans:None 6.48e4- P@ 2 Response- n 0.0' Damp0201991 guantiltatod &ad prista4 by L" m 10/29/99 300.0 400.0 500.0 600.0 . . . r7 Conc 700.0 so do@ oongl@tim- VMS/VoWp"A @t. 10/28192 1" Compound 3 name:PFOSA (Ch3) Coefficienotf Determinabon: 0.995986 Calibratiocnurve:409.188 * x + 3750.14 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighbng: I/x,Axistrans:None 3.12e5- Response- n@r'll'i'll'i'll 0.0 100.0 200.0 &mp 020129: go--titated mLd priated by i@ m LO/29/99 300.0 400.0 500.0 600.0 r--T 700.0 Conc o@tity calibratim ROP@ FMN/Py*"IP"h "t. 10/28/29 L" Compound 4 name: IS (Ch4) Response Factor:3310.11 Response type:ExternalStd,Area Curve type:RF 4.81e3- Response- Roo. 4 x x x x x x %n 0 0'0 .1 O@2 O@3 O@4 S~ 020199, -A prifted by i" m 10/29199 0.5 0.6 0!7 O@8 Conc o@9 zi K.thod file: Last w@dified; Comipound; Printed: C: \YASSLYMX\mmpC20l99 -PrO\NethDS%102899&-mft Fri Oct 29 06:53@35 1999 1: PCAA (Chi) Fri oct 29 07:38:25 1999 C--P-u.d N- int*r@l Re Q@mt !.:: C.-. io'fy lStl=.@d.: U or RF Value: U:er Peak Factor:Factor: Int grate Wind@ Chr=togr= =as windw: OCL" I(Chi) (m@ TIC C@ . A 1-:00..0..00,Disabled 1. 2.000 I.OOOQD. R,L:t:tnti:nTi" t (mi-) Reten ion Tim RT 1Re iovronce: Ti- wfid- (-i-) Peak Selection: 1R*1:"p*o".:::Typ*: 7.152, Zn&bl*d 00(.M0.0-0. DiSbled .356 n@ *at awt@l Polynmial Type: Point of Orig@: Pit Weighting: AXis Trs@fo@tion: units: mwludo itx is- P..k-t.-P..k Mlit.d.: 63 S-@thi.g: Windw s.ize (se@ Mu.Lber , f @ ths; S@th ng @thod: i i C. .11.y threshold: R;O:Idsune p.:k tai"n@: b.@ l@.e - -: 3@.bld 2 1 20.;00*.. 5 Drta.w@tvertical threshold: De shoulders: Shoulder threshold; Rel0ativt: h ig9h Ab. lu h:i ht Relative are&: Absolute 90.00 Disabled 10.00 1.500 Di:.b d : DDiisaabblleldd 02 '00. 0.*00. Disabled .e, Method Report Method file: c:%KxSSLYMZ\saupC20l99.P@O\M*L=lg%102899&-midb I L@t modified: Fri Oct 29 06:53:25 19919 CCmmpound: 2: Pros (CIL2) Printed: Fri Oct 29 07.38225 1999 CMpound Internal Quantify Conc. of M@ Ref.: TR&CO: Standards: U :r RP V U: r Peak Integrate Ch@-t.gr- lue; factor: Wind@ -SS Factor: Window: Pros (c2L27 [no-] TIC C@ . a 1.000000, 1.000000 2.000 1.0000D. Disabled R.@:n,ti...ItTi-t( ..) : R. i.. Time RT 1 It.itv.@.n@-t.. Time Window ';ti") Peak Selection: Type: RR::Pp*o".'::.. poly...i.1 Type: Point of Origin: Fit Weighting: Axis Tr&@fo@tion 7,335. 0I.00 0. 0 NO..) .334 Rnabl*d Disabled *e-.St Zt.-I JL@- Lixcld. I/X tinits; Window Number Smoth, . 190 (se of @thA: no method; i in valley th ..hold: R:d.@e peak tailing Raise zaseline @ @: Dratwctvertical threshold: D. shoulder.: Shoulder threshold; Relat.ve Ab.o&l.t: Rel "V Absolutt height: h-al&ght: ar ; area: is M-bled 2 I 300.00 2 0.00 5.00 90 Do Dis'.abled 30 00 1. 02 .0"o0:. 0.'0o0. Disabled :abl*d Di D' abl'd Dis@bld Page 2 Method Report Method file: Last modified: Compound: Printed; C; %miLSSLYNXNSQUP020199.pro%xethvs%102899&.Edb Fri Oct 29 06zS3:35 1999 3: PPOSA (Ch3) Fri Oct 29 07:38:25 1999 Compound tJ@ internal Ref.; Q@ntify Trace: C@.c. of Standard.: User RF V&lut: User Peak Factor: Integrate wi@@ Factor: Chr@togrm =as wind-: Retention Time imi@) : Relative Retention Time RT Time W;ndow (mi=) Peak Selection: Response Type: R*.ponse: Type: Point of Origin; Fit Weighting: Axis Transformation: PPOSA (ch3) in@ I TIC C@ . C i..oooooo, Disabled 1.000000 2.000 1.000ODa 8.053, 0.000. IN.-] 0.4&5 Z@.bld Dis&bld at Bt.@l A- I/X u.it.; P..k-t,-p*.k .plitud.: Smoth-ng: Wind@ size (SC@ Number of @Oths: Smothing method: Join valley threshold: Reduce peak tailing: R.i.. - -: Draw vertical threshold: Detect shoulders; Shoulder threshold: Relati-.@eheight: Ab..I,-. b.ight: 147 U."Id 2 I 30.00 200.00 5.00 90.00 DLmkbled 30.00 I.SO, Disabled 0.00, D.S@bld 2.oo, Diabld o.oo. Disabled P.O. 3 ::ttwd Report .4th*d f@le: t -difi.d: CoMa@nd: Printed: C:@y hSSLYXX\:wD02,019:.pro\Mthoa\1022994--db Fri Oct 29 0 :53:3 1 99 4: IS (Ch&) rri Oct 29 07;18;25 1999 CI@..d Kg t.r..lR.f.: antify Trace: C.=. e St.W.rds: U or Rr valuoi U:er Peak Factor: Intograts Wind@ Factor: Chr@togrm @s. wind@ is (Cbd) T(IoC ne] FLxod 1.0oo0,0,0O0o0. Di.@bld 1. 0 2I-.0.*.1O@. i..): RR:@@aetn@t@i.,'.n.ItT.sti.@..tIi.n Ti- : RTT R.f@ : i- W,@d.. Peak Sel.eti..: tnabl 'I0'-'o0":Dis@bld )0 .29 U.".Gt It:P:opn*,:::T"*: Polynmial Type: Proint 01 Origin: it W.@ghtig: . Tr."fo@tion: ilxi Units: Mlitd.: Smoot-%ing; Wi@d.. @i.o ( c@ )z Numb. f -:the: Smot@.--ng mthod; JRoinucvalley threshold: ":d i.e- p -k tai-li-n:g: Drtaow.vertical threshold: De dtershoulders: threshold: RA@tl@at--,@,:height; he @ght: Re-l""-t @e.: 1 lud, no" 70 --hld 30.00 2.0.00 5 00 90.00 Disbld 30.00 Di:.bid Di. bld 2).0G0o., Di @b d Di@.bld Quattro13,#6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE-LID:.28-99 ANALYST.i-as STUDY NUMBER. _TOX145 MATRIX: Tween samplesDESCRIPTION: doseconfirmation FACR Method: Injectiovnolume: 10 uL Cycle time: 10 min. Electrode:Z-Sp-ray Mobile Phase: (A)l.2MMIM4(M= (B)McOH TN-A- or stadrdnumber (A) 99085-11-3 (B) TN-A-2997 Prepared(datelby): (A)jQala2_mmh_ (B-)LQLL@/s9@9 Expires: (A0)4100_ (B) 2010 Storeatroom temp? l@ or N Other: Guard column: None Partnumber: na Lot number: na Analyticalcol,2mn:Keystone Bctasil Size:2 x 50 mm Type: C18 Partnumber: 055-701-2 Lot number: P9E II Sphere size:5 um Serialnumber:0591804Z Analyticalparameters: Dryinggas (LJhr)3:50 ESI nebulizinggas(IJhr)JL- LC Flow rate3:00uLJmin. Backpressure: 65bar Sheathgas(LA'r)0 HPLC solventgradient:10min-10-95 Time (n@n.) 1)0.00 2)1.00 3)5.50 4)7.50 5)8.00 %B 10.0 10.0 95.0 95.0 10.0 Tuning MetbLod Report MatkLod: C:\bl&SSLYNX\SOUP020199.PRO\JLCQUDB\PFOS3 Printed: Thu Oct 28 15:21:34 1999 Page 1 ms SOERRCE ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. ms Set 1.60 60 5 0.2 150 250 Rdbk 1.59 -60 -7 153 249 Pressures Analyser Vacuum Gas Cell Rdbk 6.le-5 4.le-3 KSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 multiplier NS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multi plier Set 14.0 14.0 0.9 0.0 4 650 Rdbk 3 Set 14.0 14.0 60 2.0 0.0 40 0 650 Rdbk 28 38 28 Method Report method yi1s. Last Modified: Print*d: C i\M"BLYNXkBOUP020199. PRO\JLCOMMkIOmin-10-95 Tbz=sday, October 28, 1999 l3s44x34 Thi=s"y, October 28, 1999 l3z44:44 ZPIIOO LC Pump XzLitial Conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Oven Temperature Right(OC) EP1100 L4CPuM gradient Timetable 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 The gradient Time 0.00 1.00 5.50 7.50 8.00 Timetable A% 90.0 90.0 5.0 5.0 90.0 contains 5 entries B% 10.0 10.0 95.0 95.0 10.0 which are C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 Spiloo LC Pump zxternal zv=t Timetable The Timetable contains 3 entries which are Time Initial 0.00 0.10 Column Switch Off Off Off Contactl Off On Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off EP1100 Autoa&mVler XzLitial Draw Speed Eject Speed (Ul/min) Draw Position (mm) Stop Time (mins) injection vol=e(iii) Vial Number Conditions 200.0 200 0.00 9.00 10.0 41 Page Pressure 400 400 400 400 400 notb@d: L"t moditid: Pri"od: %@ % 2003191:, CM, Oct Is 11.2s: 22. act 28 13.44,18 Itt: not@t D.Iy 0.0: aw- rwwtlm tI um of I N"s Fir I tar Cba@l Delay S@s 00 .03 S= ( D.It.- ) t .00 Start Ti- ( Ki- 1 NM Ti- Ki- 0@..0O.00. X.P..t. Ch@l P@@t Daughter Dmll (S*cs) Coll Z"rgy (6V) COm V 1 413.00 169.00 0.30 30 15 P%Uwti- , 2 um f I N-. P.LT iSp..t.r tChD@ellta_ D)lay: 3@. .0 Start Ti@ Rod Ti- ( Ki@ Ki- 0.00 Rop..t. M-nn.1 P@"t Daughter Dmll (S@s) Coll MOrgY (@V) C@ V 1 499.00 99.00 0.30 45 60 yucti- .3 of I Mae IP&LR 4 =P I.t.r (CbD@allto@ Span Start Ti- t and Ti- : t R.P.Ats Cb-1 Dlay P--t S@s I; 0a .0030 . Vaught 0@O-.0.0O I 1 498.00 78.00 0.30 Ll 3-rgy 45 I-V) C60 CV r..Cti- :4 of I U..x P.Lr ( mffp- xSp.@t.r (CDb&-lt:@I Dl)ay: 3@s 00 .03 .00 Start Ti- ( Ki@w 00 it.d TiR"e&tS gi-, I@0..00 Ch@al P@ent Daughter Dmll (S@s) Coll ftsrgy (*V) CO- v 1 427.00 SO.00 0.30 do, 60 Masslynx - Sample List Sample Ust:C:\MASSLYNX\soup02Olg9.pro\SampleDB\102899a.iPL Printed:Thu Oct 28 13:44:09 1999 /0/@2,F/V57 Page 1 Page Position(:1,1) FileName FileTe)ct MS File 10MIN-PFOS-POAA-PFOSA-IS 1 102899001 MEOH Bik IOMIN-PFOS-POAA-PFOSA-IS 2 102899002 MEOH Bik 3 102899003 FCMix-99086-43-1, lppb- 9/10/99RWW 10MIN-PFOS-POAA-PFOSA-IS 4 102899004 FCMix-99086-43-2,5ppb- 9/10/99RWW 1OMIN-PFOS-POAA-PFOSA-IS 5 102899005 FCMix-99086-43-3, 10ppb- 9/10/99 RWW 1OMIN-PFOS-POAA-PFOSA-IS 6 102899006 FCMix-99086-43-4,25ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 7 102899007 FCMix-99086-43-5,50ppb- 9/10/99 RWW IOMIN-PFOS-POAA-PFOSA-IS a 102899008 FCMix-99086-43-6, 100ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 9 102899009 FCMix-99086-43-7,250ppb- 9/10/99 RWW IOMIN-PFOS-POAA-PFOSA-IS 10 102899010 FCMix-99086-43-8,500ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 11 102899011 FCMix-99086-43-9, 750ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 12 102899012 MEOH Blk IOMIN-PFOS-POAA-PFOSA-IS 13 102899013 TOX145-PFOSIPOAA inTween-dose-2ppb- IG12at9g IAS 10MIN-PFOS-POAA-PFOSA-IS 14 102899014 TOX1 4-r,-PFOS/POAA inTween-MS-4ppb- 10/28/99 IAS 10MIN-PFOS-POAA-PFOSA-IS 15 102899015 FCMix-99086-43-4,25ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 16 102899016 MEOH Blk IOMIN-PFOS-POAA-PFOSA-IS 17 102899017 TOX1 45-PFOSA inTween-dose-200ppb- 10/2at99 IAS 10MIN-PFOS-POAA-PFOSA-IS 18 102899018 TOX145-PFOSA inTween-ms-300ppb- 10/28/99 IAS IOMIN-PFOS-POAA-PFOSA-IS 19 102899019 FCMix-99086-43-7, 25oppb- 9/1Q/99 RWW IOMIN-PFOS-POAA-PFOSA-IS 20 102899020 MEOH Bik IOMIN-PFOS-POAA-PFOSA-IS 21 102899021 FCMix-99086-43-1, 1ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 22 102899022 FCMix-99086-43-2,5ppb- 9110/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 23 102899023 FCMix-99086-43-3. 1Oppb- 9/10/99 RWW IOMIN-PFOS-POAA-PFOSA-IS 24 102899024 FCMix-99086-43-4,25ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 25 102899025 FCMix-99086-43-5, Soppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 26 102899026 FCMix-99086-43-6, I00ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 27 102899027 FCMix-99086-43-7,250ppb- 9/10/99 RWW IOMIN-PFOS-POAA-PFOSA-IS 28 102899028 FCMix-99086-43-8, 500ppb- 9/10/99 RWW IOMIN-PFOS-POAA-PFOSA-IS 29 102899029 FCMix-99086-43-9,750ppb- 9110/99 RWW 10MIN-PFOS-POAA-PFOSA-IS Masslynx - Sample Ust Sample Ust:C:\MASSLYNX\soupO2Ol99.pm\SampleDB\102899@.SPL Pdnted:Thu Oct 28 13:44:091999 InletFile BotUe INJW Volume Sample Type Conc A Conc 8 Conc C 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 1 4 10min-lG-95 2 5 10min-10-95 3 6 10min-10-95 4 7 1Omin-1 D-95 5 8 10min-10-95 6 9 10min-ID-95 7 10 10min-ID-9S 8 11 10min-10-95 9 12 10min-10-95 92 13 10min-10-95 10 14 10min-lG-9& 11 15 10mir,10-95 4 16 1Omin-1 0-95 92 17 10min-lG-95 12 18 10min-10-95 13 19 10min-lG-95 7 20 10min-lG-95 92 21 10min-lG-95 1 22 10min-lG-95 2 23 10min-lG-95 3 24 10min-10-95 4 25 10min-10-95 5 26 10min-10-95 6 27 10min-10-95 7 28 10mir,10-95 8 29 10min-10-95 9 10 10 10 10 10 10 - 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - Page 2 Page Position(:2,1) FACT: DA'I'AREVIEW SUiNfiNIARYFORNI L)2(C L),2 /D DataAnalyst: FACT Study0: t-latnx/Timcpoinu: S-unplLe@iL. -1109ff4, Set-up AnWy3i3 DatdAnalyst: Instrument DataReviewSiLrn-off AnalystReview Name/Date: r4-c @flff Tochakal Rcvkw NamolDatc. QuentyAmurance Review Name /Date: rl\ A Date tour. cc'T An&": ;POA.4-,rAll LizmwRaW LOQ- -----I-r-/2z2!5" E=wbm BW& e-,,4,.@ IM 2L7AU2@: Cafi'bSbmu@fbCi=@ohn Chockirt', Ok NL%IvfSD- 4.o, L/ hfatrix Bhudc /eAs ;4. IOQ DataSw= lm@klkt,,jT A, 51 LO h' -TI Analyte: cccptablLeinearpjmgc. c)) LOQ: L0FC"QP. R^2: E=wtd BW& !e NiatrixBhudc CalibratioCnh=im ox A. --A-1, idataSW- ll)kfk@4 Anglyte: AcceptableLinearRangw y@q LOQ: R^2: (;Alibra6oCnheek3. AtA. MS,MSD: IDauS.n-- Exu=tcd Blanic AIA Matrix Blank.- Aht- LW le.1 2.:J Lil z rb 0 r,t--#dz-x7 4,-@4 Zl a l@4,.@@ -all 4@5 -14, 5 FACT: DA*I'AREAIEW SUiNliN[ARY FOP@NI Date- Data Analyst l@t 5 FACT Study 9: -rox 1.1-5 Matnx(Timepoints: W,@L;" Sample List ots- -f - Set-upAAal* DatdArtaiysr Instrument :rA -<"1.5r At.@;,. Oiz Y@ff ri) Analyte: 7)-@05(-cn4-fF AcceptableLamm ITAW -107-0;,L LOQ. E=sctim BW& 4, 100 R-2: Matrix BW& 1---,s C4bmtonCboci= Data Rcview Sign-Off Analyst R Name / Do TecbnL-of Review Name / Date: Rt@, 4, QuaHty Assurance Review Name /Date: Date Entry- m@, Comnients /Jusdikations: (? L., LAC-li/oilg@ li/oi)ii ,Data tatm tv-- Analyte-. Acceptable Linear Range: LOQ: R^2: Calibmdon Checks: MSIMSI> iDatiLStamr. Anglyte: Acceptable Linear R&ngc-. LOQ: R^2: (;Alibmdon =ks: MSIMS ,Data Satus-. ExtractedB MAtrix B ExtractedBlanic Matrix Blank- Q",tlfy c@@ g@ry -P.. TOX143-f&tLIWC, D&Y2'0000 and 11/4/99 MM 2'aplo Lijsrti: : C:\NUSLYMX\amali&06249$.P=\SmwleDB\lIOSgta Last @" ad method: Last modified; W,o:n Nov 08 02:34:11 1999 \&Ml L0a0 b.0C6k:U2p0 :s"g :\S@lia-ratm.p=\"SthDB\IlCSOPO bi- m- 27 1 99 J.b co": Printed: Won Nov 00 09:141:20 1999 C--P-U-d 1: POAA (Chi) I "l 2 11105 99002 3 11 05 99003 4 11 0'599004 5 1100599005 6 110599006 7 110599007 8 1I1 D59:00: 9 1 059 00 IC 110599010 11 110599011 12 110599012 13 110599013 14 110599014 15 110599015 16 110599016 17 110599017 le 110599018 19 110599019 20 110599020 21 1111059:021 22 059 022 23 11105:9023 24 1105 99024 2 5 11 05 9:025 26 11 05 026 27 11 05:9027 28 05 9029 29 110599029 30 110599030 31 110599031 32 110599032 33 110599033 34 110599034 35 110599035 36 110599036 37 110599037 38 110599038 39 110599039 40 110599040 41 110599041 42 110599042 43 110599043 44 110599044 3"01:liat .:OH .*0O.H 1@..1 TT o 145-ROL1k 1049-IMIk-1, RWW- box 99-211 OXLI45-IkBL111104:-RBL Dik-1, RWW- Box 99-211 TOX 145-RBL T.. 45-RBL 04 -GIppb-1. RVN- Box 99-211 g- 04 2ppb-I 11 TT o X145 -RBLI1049-30ppb-1 RWW- box ::--2,11 5_FkBL 1 9 OXI:' -RB L '@10.49:2@0oPppp.b-I-1 TOX 1I45 -ILBLI1049-300ppb-I TTOOXX 145-PLBL11040 9-:00ppb-1, 'rOX 45-"Lll 49- Ooppb-1, IRUMN-RNWRW- RWW- .BoXx '999-'-@21'1 Box 99-211 Box 99-211 box 99-211 TOX145-RBLI1049-1200ppb-1. RWW- Box 99-211 nk H-M 31-,tTL. OR03240-300ppb-KS. 11/4/29- Box 99-211 TOX14I5-FLTL: TTOoXx,:5:R T L, 5 RTL :1.1.*12:.0-3,0*ppl"l..t@.1.,1111919, . 19-211 ,to3 Da 29/Con r 1 4/;9 32241//HH/Dyy2g/Contral. 11/419 TOX145-RTL, 9R03242/M/Day29/Control, 11/4/9: TOX145-ILBLI1049-300ppb-CCl-L. ltvw- Box 19-211 H.OH Blank TOX114.5-,RTL: :R 0.3243/H/D.a.y2:/ n.trol: ll/:/9: TOX 4 - TL 3244/K/ Y2 /ccootr 1 Il/ TOX14154-5R_TRL. 9RO3255/M/Day2915=g/kg TOX TL, IR03256/M/D y 9/5.9/k 21/4// :, 11/4/ 1I45-RTL, IR03257/H/D:y229/5.9/kgg TTOOXX 45-REL11049-300ppb-CCI-2. RVN- 11/4/:: box 99-211 4*CH ank 145a-l tTL TTOX 145-RTL: :RD323:/N D.yY22://5509./gk/qkq: R0325 /M//D. 111/4/9999 1 /4/ T QOXX 145-RBL11049-300ppb-CCl-1. Ru" - Bo. 99-211 M,OH Blank TOX I 45-RBL11049-WBlk-1, RWW- Box 99-211 45-RBL1110149-PLBL Blk-1, TTOOXI I@:1 -PBL l@ 01 99-1,;1 b-li, RKW- Box 9 211 9- X S-RBL 04 - 2ppb it.- .. 9: 211 T.X 145-RBL11049-30ppb-p1, - 1, RRUwN-- 5B0o.x 9:--211 TTOaXx 11 45:RBL11CIO)49-60pIpb- Rw_ Box 99-211 T 45 ELBL 20ppb-1: Aw- box 99-211 T OXX 1. 15_ RIIL l 04499:-300rppb-I T0 RBL 1 I@04 9_90 Oppb-1: X 145_ RSL 104 TOX Oppb-1 TOX145-FLBLI1049-1200ppb-1, RWM- Box 1: IW PKNW Box RUN- Bx 9-211 ::-2111 2 9;-211 Type Standard S3 tandard tandard Stander d S3 t- rd Stt.ndda.@d ends @d St "dard rd Stand& oc oc oc Standard Standard St:ndard St ndard Standard Standard Standard Standar St@dardd Std Ca- 6.13 12.30 30 70 1261 30 0 3 00 3. 7 01 9203..0000 1227 00 307.00 307.00 307.00 6.13 12.30 30.70 1261-30 301 37 :. 0000 6 3 . 00 92 12207.0000 AT 7.00645 7,011 7. 5 7 0,9 7 ..0I2@, 7 .9 1 3a :.:72 . 65 :.:9_,3 6 ols 7:018 7 6 90 7 0115 7:.0 109 7 .01.2 :.919 6.994 7.0195 :-:91, 7 Oil1 7:.02 6 '67.:o:l.,4 6. 99:7 6 *997 6 9651 1 96 6'96: A@- Conc. Flags %Dev Mod C@t 61 79 100 115 171 234 442 766 1292900 0 00 b 0.:00 bb 0 00 bbX 0 00 mmx 0 Oo mm ,2 .597 11 0 bbbb 33 7 -89 bb 6840.65 bb 094.00 bb 1138.49 bb 37: 2:@,5-761 bb 37 2 . 2 bb 09 0.00 bb 94 0.00 bb 40944 291.00 bbbb 93 93 1 918 390 77 4.9@ 6 00 .00 bb 0 .00 0 .00 0 .00 b 00 bb 277.30 bb 0.00 bb 030 b 2.90.- 9 bb 87: 76 104 120 173 240 46680 l@707 1260 0.00 bb 0.00 mm 0.00 bbX 0.00 mmx 0.00 mmx 1 54.77 bbbb 23.52 357 bb 657.1.2.870 bb 911. 1 2 bb 1179. 9 bb -100 - 00 oc 14 -4 128 -3 -7 -5 -10 -6 -1100 -,00 --00 11 10 7 _7 -4' A@lia 06249*: 0-@titated and rvie@d by is& Ii/l/99 a,".tlfy acompo@ TGX145-. t 3o7xry, RM-ZT do* and @t"l- "t. 12/4/99 "W a-Wi. LLet: "at madi fid: Nlth*d@ f..: jzt mocli Code: C:\MNULYMX\@..IiaOG2499.PM\---P'-DB\110599- Mm Nov 00 00:34:10 1999 r:\@lla aba0cil@p:o2e7pg1:\a@lia-rats.pro\lftth0g\lIOSgga Won 14ov 0 9:20 99 PrL.t.d: Mn N@ 09 09:18:10 1999 Compound 2: PFOS (Ch2) I N- Smgl*ll.st . T-t TYP- 2 11105 99002 3 111100559:003 4 059 004 5 110599005 6 110599006 7 110599007 8 110599008 9 110599009 10 110599010 11 110599011 12 110599012 13 110599013 14 110599014 is 110599015 16 110599016 17 110599017 is 110599018 19 110599019 20 110599020 21 110599021 22 110599022 234 111105::023 25 1105 024 26 110599025 2 110599026 27e 11 05::021 2 05 028 29 110599029 30 110599030 31 110599031 32 110599032 33 110599033 34 110599034 35 1110599035 36 0599036 37 110599037 38 111059903: 39 059903 40 110599040 412 1110599041 0599042 43 110599043 44 110599044 M*.COHN BlIank k M H li..kl T*0145-B tSL 1049-WBlk-i, tVw- Box 99-211 OX 14 S@-R.BLI@I@O.:9 -"L Illk-1, I,.- .. 11-211 TTOOXX14 ILBLL I 9-6ppb-1, TOX145- - 1049-12ppb- RNW- BOX 99-211 TQX14145-FLBLI101410:-30P b 'tWW"-"- "SoOx. -21 TO X S-RBL 4 -60p pb-1. RWW - box 99 -211 TOX1145-RBLI1049-120ppb-1. TToOxX,454-5R_BRLB1L1I0491 -300ppb-1: 04 9-600ppb-1 TOX1:5:MLJIJIOO::-@1020ppb-@i, RWN- Box RWW: box RWW Box .-_.x 99-211 ::-211 -211 91-21@ TOX N.OOX H 5 RDL B5 lank 00ppb- RVW Box 99-211 4 T 32400-300appb-XS 11/4/9:; box 99-211 1 5_-RTL':, 032:0-3 Oppb-KS 11/4 TTOOXX14 RTL 9R032 /M/Dy2 /Control B4O/X999-211 TCX145:RTL. T 1 5 RTL, OR03241/MF/MIDOyS2Y:/Control: 9lt03242 9/C. tr , Ill,/.1:9 ToOxX M.OH RBLI1049-300ppb-CC 81&.k 2I-1, nRWN-ol B..ll/9:/-Z9911 TOXI 1:5 TL: :.R.032:43//MM//DDaayy29/Contral, 11/4/99 TOX S--RTL 32 /Control, 11/4/99 TOX145-RTL, TOX145-RTL, 9R032SSfM/Day2 2: /5.9/kg. 9R03256/K/Dy 9/5.4/ 145-RTL, 9R03257/N/Dy229/5@g/@,,: g TTOOXX145-IkBL11049-300ppb-CCI-2, RWW- 11/4/99 11/4/:99 11/4/ box 99-211 M*OH 81. k TOX 14 5-ITL: R0325@/M/Day29/Smq/kg, 45-RTL :R03259/N/Day29/5.9/kg, TNOOX"I 01_R"Ik&Lllo4g9-_30:ppb-Ccl-1, RUN- 11/4/ 11/4/:: Box 99-211 r.Xl45-RBLJ @.4 WB k-1. Rw- Sox 99-211 1I:5-REL110441:-RBL Blk-1. PIWW- Box 919-211 TOX I-PBL1 '0O'g--6Ippb- 1, IKWW- Box 99-2 1 TTOCXX 5-RBL1 2ppb 1: 11- Boxx 19: -2@l,l TOX145-FLBLI1049-30ppb: Rww- So -2 11 45:"LllllO:9-160ppb-li,nww-_Boxx99-21 TTOOXX 45 "L 0 9- 20ppb- RKW so 99-21@1 TOX145-Rl3LI1049-300p,l, , IR ,,- 1,. ::-21@1l 1I45 -RBL11104:4-600ppobp-1, WW- Bx -211 TTOOXX 45-RBLI 0 -90 ppb_ IKWW so 99- 2 TOX145-"LI1049-1200 p b-1 1, Rw*@ Ba x 99-211 Standard St:ndard $t ndard Standard St-d' @d It-da rd 3tmd' rd Standard Standard oc oc oc Standard :t.nd,.rd tand rd Stan d@rd St.ndrd St:nd :rd 3t nd rd t..dard Standard std Conc 1 6.14 2 30 30:70 1203...00 3 1 7.00 6 9214..00000 1228 307.00 .00 307 307.oo 6.14 0 12.3 30.70 1261-40 361.7'..0O0o 4:00 92 1228.10000 7.2 RT 7.2 56 392 7.24 4 7.2 7.2113 7.163 7.11:1 7. 19 5 7:1.4 7 .17 3 7.161 77.24: 7 1:1 7:1 3 7. -11' 7.11."4 7 1 65 77.1163 7.191 7.1:2 7 175 7:.11671 7 .18 7 7.116676 77..11477" 7 .16 2 3 77..11760 7 .16 4 7 .1576 7 60 7.116 '. 7.1137 7 5 7 :1642 ftg. 2 Ar" 77 55 39 93 14 2459 36 502 .4: 1539 3586 6303 8Ll3 9947 52 23 211 3 20 1159716 2388 , 69 1 405 4 1916493 10 4302 12714 67 726 107695 130162 2016 96 136 191 296 355 545 078 1600 3661 :459 26@12 5 Cme. 0.00 0.00 0.00 0.00 0.000 10. ,0 riago bb bb b bbb bb bbx 20 .91 MM 1' - 1 bb 134,29 bb 349,39 bb 634.97. bb .25. 8 bb 1017 0:'o'o m, .0103 2@9540 bb 0.00 bb 0 bb bb@ 223:5000 mbb 0.00 m 0.00 bbbb 0.00 bb 11 0112.21 bb1983.63 bb 11403 79 bb 253:7. 8 tb 0. 112. 0 .34 bo 136590..2: bb 68 2 0. 4 0. 00 bb 0. 00 bb . 00 b 29. 64 bbX 93 bb 29. bb .4 526 bb bb 141. .98 357 bb 65,1 32 bb 14 :414 bb 7 2 bbX %D@ bi@d C@t -100 -114 -I 19 4 _l 3 0 -17 17 -13 :57 19 16 5 17 -91 -12 I OD A-11. 042496: Q@tit@td and c.@l.@.d by L.s II/l/99 Quantify Cv@cu@ TOX145-rat li@r, 2,@ry Report DaY29 doe* w4 @@l- -t. 11/4/99 mm sample List: Last modified: m.tt.d: L..t .dtid: Job C,.d.: C:VGMLYNX\amoliaOG2498. M\SMMIODS\110599& bion O&W 06 00:54:16 1999 r:@@1L& bactup sep99\a@l,.-,.@.P"\NothDB\IlO$99& lin M.@ 09 06:20:27 1992 Printed: m- m- ce 09:28:10 1999 Compound 3: Burr fCk3) s@lell.t Text Type 2 1110599001 2 5 900 4 1100599004 5, 111105:9005 78 11,005599990000768 9 11005 9 900 9 10 110 5 9 900 0 5 ,901 5 go 12 110599012 13 ILOS99013 14 110599014 15 110599015 16 110599016 17 110599017 is 110599018 19 110599019 20 110599020 21 1110599021 2 2 0599022 234 11 105::023 2 5 II1C0)5Sgg024 2 6 110599 025 2 7 110599002276 2 5 110599 599 02: 2290 1111005990032 0 3 31 110599031 2 32 059903 33 110599033 34 110599034 35 110599035 36 110599036 37 110599037 389 1110599038 9 3 059903 40 110599040 41 110599041 42 110599042 43 110599043 44 110599044 HIteo Blank T=1415-RBL12101:9-VBlk-l@ Ryw- sox 99-211 TOX, :5-RBLJJ 9-FLBL Dl 1, RwW- ft. 99-211 5-RBL 0 4 pb 99-2LI TMOXX 14 5-FLBL 0049-G1p2p pb- L, RW _ Box ::-211I 7=14I5-RBL1101149-30ppb- 1, RRNWW_ SBoox, -21 1 99-21 TCX 1 45-RBL 0:"Oppb- T 'I-.Ll1. 9-12.ppb-@ TCC)1XX145-IkBL101049-3a00ppb- .- 5- -21@1l NM- BO. ::-2 TOX 45-ItBL11 49-6 Qppb :9-211 TCX145-RBLI1049-90OPPb -1: RMRNwNwW-_-BB:O:'x 9-211 1 TC)EI45-RBLII*49-1200ppb-1. 9-21 M*OH 4B5lank Tax @_-RRTTLL: =' @4 r=14145-RTL, TOX S-RTL, rT=CIXI:S-SR_ITKLB ::.031:0:31.@llppb-.;,@@/41199- Box 99-211 32 0 3 Oppb-M 11/4 9R03240/M/D. Y2 /-Cnottrr:1l "03241/WDOY2:1 A 0490_3242/WDay2g/Control 99 Box 99-211 111//44//:: alanl i@9" 300ppb-CCI-1. RWW- 99-@i, NECH t ?CX1145-RTL: 03243/M/Day29/Contr.1 1/4/9: r= 45-RTL ::03244/M/ ray29/Contral: @1/4/9 TOX1I45-RTL TOX 45-RTL: gRo 3255/M/Day2g/5.9/kq 9R0323 6/M/Dy29/5"/Icq: 111 /4/9999 1 /41 TOX1I45-RTL 03257/M/ D.y2g/5.9/kq, 11/4/99 TCX 45-RBLi@9.4R 9-300ppb-CCI-2, RWW- Box 99-211 HOCH 951;Tnk TCX14 - L, 9R03258/M/Day2:/5.9//kg 111/4 11:5 -RTLil!P4R03259/H/D.y2 /5.9 ic : 4/99 TTOCXX 5-RBL 0 9-300ppb-cci-il RNN-g a1..'.9-2@l Nc Blank Tcx'.:5-R&L,11 10::-WBlk-1, RWW- Box 99-211 S-RBL I RBL Olk-1, RVW- Bx 99-211 TCX1I45-RIIL l@1049-,lppb-1, I.- Box 19-211 5-"L l@@0..,- 2ppb-1, Rww- Box 99-211I -X @45-RBL 1 30ppb-1. RNW- Box 99-21 TC@X 145-RBL l@49-loppb-l,,Rmw-_Bx.99-211 TTCO"X145-RBL11049-12 Oppb- 1, Im Be -21111 'roxI45-RBL11049-30 ,Pb- RW_ B.. :: -2 11 45-RBLIIO::-:00ppppb- Rww- Box 99-211 TT'GOrXK I45-RBLI1J..0 4,):,000pb1. RWW- B.. 99-211 CX 45 -RBL 0 20 pb--1, RWW Box 99 -211 Stad@rd Standard SS t:ndard t ndard SSttaannddaarrdd at Stand atd Stand Standardd oc Standard Sta.ndard St da d Sta.d..d SS tand rd Staannd rd t O:rl Standard Standard std C- 1.00 1.00 1.00 1.00 1 1:.000o 1.00 1 .000 1 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1:., 1.00 RT 7 52 7:.00.2: 7 20 72 7.00 7. 32 0 " .0 7.,07 6_,.(1.30 7.03 0 7.0041 7.012 7.002 7.00 7.00 5 7.0051 7.003 7.007 7 021 7:,00a3 76.090 6 5 7.006 7-,006 S. a 7 0022 : 77 ..000039 7 .905 :.9:1 7.00: 7.OC2 1-9741 7 0000 4 Page 3 A- Cone. Flagg IDv )OodC@t 4714 35003 ::@' 4445S 5132 5052 4750 4715 4022 3891 263 0 23.8'l 2619 2695 2496 2769 2439 225795 3a3 453 564 46964 33770 4449@'2 349363 36 5129 5309 48211 5250 5 72 4975 5000 4346 4149 0..7939 bb 0.1)1 bb bb 10 93 bbb 1:08 bb 1.006 bb 1. bb bb 0-:49 0.8.20 bb 0. 55 bb 0. bd 0.55, bb 0. bb 0 52 bb 0:58 bb 0 51 bb 0:46 bd 0 74 bb 11. 02 MM 0.13 bb 28 bb 0.71 bb 1.04 bb 0.92 bb 0.873 b 0. 2 bbb 11 .07 bb 1 bb 11.'011. bb 1-@l. bb . bb 11 .04 bb 0 '05 bbb -:'7b b -1 27 I 7 a 6 -0 _-I -16 _@.01 :50 45 44 :492 4 :49 54 26 12 3 -2 -29 -6 -17 -26.7 111 11 0 0 4 -5 _l 9 3 Amlia 06249B: Quantitated &M r@l by I.. II/s/09 ().z@4tity c@nd TOXI 5-T. t llwr, @ry F@rt Day2g do:: nd @=ol- @t. 11/4/99 POW SmWlo last: Last rld: thed: Z,.d: MLOast madi Job Cod.: C:\mkSSLYWX\@llsOILI2s4::. MW\SmplaDB\lIOS99& man Nv 08 01:54. 19 F:\ ILA b-@-.p op99\@lia-mtm.pm\MsthDB\IlOS99& N@n= 08 04:20:27 1999 printed; Mon Nov 08 02:18:10 1999 Cc-POU-d 4: PFIDIM ICh4) 2 110599002 3 110599003 4 111059:004 5 059 005 6 110599006 7 110599007 89 1110599008 10 11 0599009 0599010 11 110599011 11 2 11105:90121 3 05 90 3 14 110599014 is 110599015 16 110599016 11 1 11105990171 8 05990 a 19 110599019 20 110599020 21 110599021 22 110599022 23 11 ,105::023 24 05 024 25 110599025 26 110599026 27 110599027 28 110599028 29 110599029 30 110599030 31 110599031 32 111059:032 33 059 033 34 1110599034 35 0599035 36 110599036 37 110599037 38 110599038 39 110599039 :0 1105999040 1 059 041 42 110599042 43 110599043 44 110599044 me"owWlBllaa@,ilIt.t M 0. :I&ank H:om I n TOX1I45-RBL11049-WBlk-1, Rww- box 19-211 roX 1 4S-RBLll1O40::RBL Blk-1, RWW- box 991211 T X.1.45-RBL 11. 4 _6-.,-11,11.-_..XI99-21 Ta 5:RBL,,.44,_12ppb-1. TOX145 RBL 30ppb:" RWW_ RWW _ 11445- RBLI1110049 61 *p b RWW TOXx 5 RBL 49: 20P 1, RNW- TToOX145- -RBL11049-30 Oppppb-b-1, RWW- Box 9,. So box box :-211 -211 .9-21 99-211 99-21 T 1I45- RBBLLII1J0O449:6 Cppb-1, TOOXX 14455- R 9 9000ppb-1, TOX . R_BL11:::-12:Oppb-1, RVV- box 99-211 RWW- box 91-211 RNM- Box 99-211 OOH 1k TOX145-RTL, 324 -200ppb- , 11/4/19- Do. 99-21111 XIl:5 -RTL, 9RO3240 -3 00ppb- KNSSD, 11/4/99 Box 99-2 To To 5 -RTL, 9R03240/WDay2:/Control, 11/4/99 r0oX1145-5RTL: 9lt03241/M Day2,/Cntratlr ll/:/:: T X 4 -RTL 9R03242/M'/Da 2 C =@l: 11/9/ TOX145-RBL11049-300ppb-CCI 0 Sx 9 -211 M.CH Blank 145:RTL TTOX 145 RTL :,tRo03243/M/DD:yy2 ://CCocnntrto@lol llll//:/:: 3244/M 2 : TOX145-RT 9R03255/M//DlDyy 2:/5.9/kg ll/:/:: OX 145-RTL, . TOX 114455-_RRTBLLII TTMeOoXx xH 551,.lk 9R03256/M/ 2 /5.9/kq 9RO3251/M/Dy29/5@g/kq, 049-300ppb-ccl-2. RWN- l11l//4/9 box 99-2911 '100 4 -1.141 TI: :,tR0321:Ml.,2:/!,..Ikg : 111/4 R TL 032S /M/Day2 15.q/kg 1 /4/ THOoXo1M45-BRI31, Oppb-CCI-1, RWW- 9 Box 99-211 I..k T X)1,415:FLBL111:,,0::-9,:,WoBlk -1@ -RWW- Box 9 -21 TO0 45 RBL RBL Bi , 1, Rww- box 99-211 145:RBL11049-6ppb-I TOX 1:5_RBL11049-12ppb-1, TOX 114 5 OLBL1I1104:-30ppb-l: 1 To TOXX S_RBL 04 -60,ppb- RMIWT-WW_Box 99-211 Box 99-211 RNW- Box -211 RVW- Box ::-211 XXII45-RBLllII044::12*ppb-1, RWW- Bx To 45-RBL 0 I, RWW- Box To 145-RBL11049-60CI3p0p0bp-pb- 1: 1- Ix TT - 145-RBLI1049-900ppb- Fkw!- box 99-211 99-21 :9-21@1 9-211 TOOX145-RBL11049-12 Ooppb-1, RWW- Box 99-21 Type Standard Standard t and& rd Standard Standard tandard 3t:-Iard st ndar d tarwrd oc oc oc St:n" rd St nd @d St.nd:rd Stand to Stand:rd SS tandard tadrd Standard Standard std Cmc 6.13 12.30 30 70 1261:.30 1 .*.1o 307 113-.O@O 1220:00 21 307.00 .00 307 307.00 62 .13 .30 30 70 61:30 123.00 301.00 13-.00 :20. 0 00 1221. RT 7.71, I'll. 7.756 7 714 : 506 77.1722 7.7447 7.7 55 77 .7 46 7:'717 7-77,1 7 7:.7.115. 7 .7 50 7 .7 7 .7578 1.7 3 7.7746 '71..7741989 77 7.774 7 7.:7764 7 .7 $1 7 .I 7 752 1.712 7.7116 7:775 7.751 7 7891 7.730 77 7.749 7.752 7.7473 7.7 0 7.7524 7.77 7 'l-14@ 7.75 7.750 pg. 4 At331 255 is 158 1566 1:1 211 12529 2 12 63447 1205901 204104'7 6302 5982 176 1462 4 651 32 4 13 134 1631 35329 1971 4071 C1o1nC.56 NrKl,90 1' o1:.',I.,. ,bb mm 1.476 M 3.69 PM 259.57 MMX m 63,60 132 1 02 M 04 360' M ::2 71 m so @@-IOS...0l0 M m 36 0 33 .24 M 2 1 370@0'-0"164 N 0.1 0 a1 mm m 19.07:.'353 bb J.:.1" bb mm 228.17 MN %D@ Mod C@t -308 -3 17 4 11 1 13 -3 -4 21 -26 265525 140 .00 M 3 3@.61:1"9 b 62453 15 143161 0 MN .0.4011 MMN 1 I29s3 59 11572 22499 57 a 2 I. 24@ 207514 29.03S7, MMMM 24.18 MMX 60.20 NK 125.5949 MMM 324 : 363 -36 NK 119 3*-41 M 2.13 Mm -53 -24 -1 92 -2 6 - 'I -3 JU-1@& 062498: g@Lltatod and r-A by Las - II/l/99 QT%OMXn1t4i5t-yraCtalib@r&,tl@DayR2o9podrotse &.d @@l- -t- @1/4/99 mm 'Compound1iii-mPeO-A.A (Chl) ii coefficienotfDetermination:0.989198 ,Calibratiocnurve:0.973462 * x + 119-913 "Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:I/x,Axis trans:None 1.3le3 x x Response- 0 16.5- x %Conc x -13.8 0.0 A@lia 062498: Ot@tltated 200.0 &W rwiewed by i" 40b.0 II/l/99 @Ob.'O' 8'06.'0' i666.o Conc 12TO.0 2 Quantify Calibra"@ Rs"rt ,ox243-rat liwt, Day29 do.& AM @t"l- "t. 11/4/99 mw icompound 2 name: PFOS (C ,Coefficienotf Determination:0.982749 @Calibratiocnurve:9.51640 * x + 260.801 ;Response type:Extemal Std,Area Curve type:Lincar,Origin:Exclude,Weighting: I/x,Axis tmm: None 1.19e4- Response- 0 i 16.6- < x %Conc x x x -57.0 0.1.1(o A"Iia 042490: Q@titated 200sO 406.'0 askd rw4ow" by Las m II/l/09 @Ob.'O iob.'o' i666.6 Conc 1200-.0 0,@tify Calibrati@ PAPOrt .=145-mt llwr, Day29 .. .d -@l- -t. 11/4/99 ow Compound 3 name: Surr(Ch3) -ResponseFactor:4773.57 Response type:ExternalStd,Area Curve type:RF i 5.3le3- Response- P.g. 3 x %Conc - 18.5 Conc 0 oi 0.2 0.'3 0.4 0.5 O@6 0.7 0.8 0.9 l'O A-lia 092490: ousnutatad and m@l ' ky Las m 21/c/99 ou@@fy CALLbratim Report 7OX245-rat llwr. Day2t do.. " -t-l- -t. 11/d/to3@ icoeicieonftDeterTnina0t.i9o8n9:845 !Calibratiocnurve:17.2655 * x + 13 1.101 !Response type:ExternalStd,Area ICurvet)rpeL:inear,Origin:Exclude,Weighting:I/x,Axis t=: 2.13e4- None @g. 4 Response- 0. 17.3- %Conc -53.2 o.-o k@lia 062498: Q@titated 200.0 400.0' arbd reviewed by I&. m 11/9/99 600.o 8ob.o.... i666.o Conc i2oo.0 Method file: Last wdifiecl: compound: Printed: F:\@ I,& b&ckp Sep9,:\@lia-ratS.pro\.MothDB\1105998-,Bdb Man Nov of 08:20:27 99C 1: PWA (Chl) Ron 140v 08 08:56:38 1999 conm@u cl Name: , e....,1 Re 0Co"nc.t Ofy St&nLrds: U::r RF Valu*: U r Peak factor: I t*qrate Window Chnr@togrm M33 Peak Lc.ti.. ractor: window: R.:1:11,1.on,.Tl* I- I ti t: RT Reference: Time Window (sins): T I@, Peak Selection: R.Sp.@.. R :Pon.:::Type; P. C-@Libr.t@.. C.-.@ POL,Yn-ial TYPO: P..itntU.of Origin: ighting: Axis Trnsfo @ tion: Conc*ntration Uni,tse: NO 3 Peak-to-peak S-Oth amplitude: s- thing: W@.%- @Ll. (.C.ns@: Number of th Ing 5-0 B.S.1ine@ swaths: ethod: j I cv ll:y th.rIe"sh Id: R:dun tap. k t no Raise b&201lnG g: Peak Separation Dratwecvtertical1 threshold: , h* :a.re: DS*hould. 'hr hold: R..P..@. Thr@.h.ld R.I.t@V : Ai3 IOitu ve "kb*30&lu't. h:"ght: h reaght: & P43M fchl) T[No a C.I.Cc 1@-.000.0.000,0 2.000 I.OOOOD& Disabled 6.976, Enabld 0I.000, Dlsabltd N.o2el71 me& ... t Exte Area. Li ..1l0u1d,' I/X un. 530 E.-bled 2 I 20.00 200.00 5.00 9V0i-s0a0. d 30.00 1.50: 0.00 , 2.00 0.00 11@l::Ill:d D @,bbiI d D ad 0 &b, ad method Report Method file: Last modified: Compound: Pr@.t.d: F:\@alia backup 2OP99\@lia-r&ts-Prc\MathDB\l'0599*'mdb Mon Nov 08 00;20:27 1999C 2: PMS (Ch2l "on Nov 00 08:56:38 1999 C@pound Name: InternalFief.: Quantify Trace: Conc. of Standards: User RF Value: Use@ Peak Factor: Integrate Window Factor: Chro@togr@ mass window: Peak Location Retention Time 4min3): Relative Retention Time: RT Reference: Time Window (.L.s): Peak S.l.ct@o.: Response R.SP..3. Type: R.3POnS@: Calibration Curves Polym@.1 Type: Point of Origin: Fit Weighting: AXIS Transfo @ tion: Concentration Units: Noise P*ak-to-pook Smooth "Plitude: S-.th@ng: Wild,,@ 11r1, .0. ".. t Smooathing 3 method: B&3 line Join vall y threIs_hqo:ld: R*6,c.a pl:k t.I b ... 1 n. Peak Separation Draw vertical threshold: tect shoulders: DSohoulder threshold: lk.@p .. a Thr.sh.1 Rel.a0tiv : h iIgritt: Ab lut h: gh Ilel,litv: :r::: Ab lu r PTOS (ChZ) [won.) TIC Conc. 5 1.000000, 1.000000 2.000 1.0000D. Dix&bld 7.149, 0.000, [No.el 0.299 Enabled Oi..bi.d 14.&rU3t External )Lreas Li..&. Exclude I/X No.. 56 Enabled 2 30.00 200.00 5.00 D9i0x-a0b0led 30.00 1.50: 02 .00 0 .00 .00 DI.Ilblld Di bld Di '&bled &bled Method file: Last modified: Comi)ound: Printed: r:\@lia b-cxup sepgg\&Mlia-rats.pro\M*thDB\IlOS99..pdb Mon NOV 08 00:20:21 1999C 3: Surr (Ch3) Mon Nov 00 06:56:39 1999 Co.pound N@e: Internal R.f.; Quantity Tr@c.: Cone. of Standards: Us*r RF Value: Vser Peak Factor: Integrate window Factor: Chro"t.gr- M.@ window: Peak Location Retention Time (mi-5): Relative Retention 7-0: RTI.:et r.nc*: T window lalft$): Peak 5.1 et@.n: Fk..Po... Response Type: Response: Calibration Curve$ poly.-i.1 Type: Point of origin: Fit2W?.Lqhtin : Axt r ansfo9@tion: Concentration uNoniistes: Sur@ (Ch3) 1)60nel TC fIixed 1.000000, 1.000000 2.000 1.0000DO Disabled 7.023, Enabled 0.000, olsbl.d IMn.] 0.310 U.&@.st raternal )Lr*as ]Lxclude lix No- Peak-to-peak @plitude: Smoth Smooth ing: window size tscanal: Numb. r of @c ths: Swathing noth0d; S.@.lin.. join valley threshold: RReadiuscee bp.e3:kIi.t:i-l1i-ng:: Peak separation DratwecvterticaIl tt@r..h.1d: D. shou do rs: S@,h.,",.Ind.,,r tT"h@r:3'hnoo,ld: d R,,.I,tt,,: h:@19 t: AbialUve hrogaht: Flesotito :r*&: A b lu so r@bied 2 I 30.00 200.00 5.00 oi.o.,bled 30.00 1.50 Disabl:d 0.00: Disabled 2.00 D bl d 0.00 D@ bl d p.g. 3 method Report Method file: Last modified: Compound: Printed: F:\Mell& backup sgpgg\".Iis-@.ta.pro\X.thDB\IlOS99@Jdb man Nov 06 08;20.27 1999C 4: PROSA (Ch4) mn W.. 00 08:56:38 1999 compound Internal Quant&fy Cone. of N-.: ltef.: Trace: Standard.: User RF Value: User Peak Factor: inteqrat* window Factor: Chro@toqr@ mass wind-: Peak LOCAtion Retention Time fains): Rtiative Retention I RT R.f.,@.C.: Tin* Window imins): Peak S*lectlon; Response R..po ... Type: R..Po ... : Calibration Curves Polynomial Type; Point of Oriqin: Fit Utiqhting; Axis Tr"sto@tion: Concentration Units: Noise p.ak-to-peak S@otri amplitude: 5-othing; Window of W.., 3 t :=o t1 hltn3q method: _...@in*3 i cva":y threls@nhgold: Jlok d-. . p. k t i R:,@. b@..Ii.. - -: Peak Separation Draw vo@t@.@l threshold: Dehtouect shoulders: S lder threshold: Threshold Relsaotivt: h iIqhtt: M lu h: gh Rel.a0tllt: A b lu PFOSA (Ch4) IN .. I TIC Conc. C i.cooooo, 1.000000 2.000 1.0000D. Disabled 7.770. 0.000, [No..) 0.226 E..bid Disabled Nearest Linear Lxcld. itx 16o.e 82 Enabled 2 300.00 2 0.00 S.oo '3oi-.0@0bl.d 0.00 1.50 0.00: 2.00 0.00 Dis3abled D@ &bl.d ODt .bld 1 &bid P.q. 4 AMELIA 062498: FACT Equipment Log 99114 QuattroII,#6448E PAGE DATE: 11/05/99 ANALYST: ias STUDY NUM]BER: TOX145 MATRIX: mt liverDESCRIPTION: Day 29 controalnd dose FACT Method: ETS-8-7.0 Injectiovnolume: 10uL Cycletime:10 niinE.lectrodeZ:-Spray MobilePhase: (A)2.0mM NH4CH3CO2 TN-A- orstudrdnumber (A) 99085-11-6 (B)McOH (B)TN-A-2997 Prepared(date/by): (A)10/30/9s9ah (B)10/29/9m9ee Expires: (A)04/00 (B)04/00 Storaetroomtemp? M or N Other: Guard column: None Partnumber: na Lot number:na Analyticaclolumn:Keystone-Betasil Size:-x2 50 mm - TypeC:18 Partnumber:055-701-2 Lotnumber P9EII Spheresize:5 um Serialnumber:089815S Analyticaplarameters: Dryinggas(L/hr)3:00 ESI nebulizinggas(L/hr)_!O LC Flow rate:-30u0L/min. Back pressure6:2 bar Sheathgas(Libr0) HPLC solventgradient:10min-10-95 Time (min.) %B 1)0.00 10.0 2)1.00 10.0 3)5.50 95.0 4)7.50 95.0 5) 8.00 10.0 Tuning method Report Method: C: \MASSLYNX\AbMLIA062498. PRO\ACQTJDB\PFOS1-6KV Printed: Fri Nov 05 09:43:09 1999 Page I 41 ms SOURCE ESP- Cap4-llary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. Set 1.60 40 5 0.2 150 250 Rdbk 1.60 -40 -3 151 253 Pressures Analyser Vacuum Gas Ce'-l Rdbk 1.2e-4 4.8e-3 Ag msi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 15.0 15.0 2.0 0.0 4 650 Rdbk ii Set Rdbk 14.0 14.0 10 12 2.0 0.0 40 ;10 0 10 650 S@Lng Mthod ROPOCT ..at lPrtnt6d M. Oct 11 07:22:17 1999 r@@ N@@ 05 09:26:14 1999 "1-.t Delay I -.. ) : 0.00 rUnct,@@ : I MM f I No.. ftzr ( ZSIP- Inter Ch AnCazlns Sp.n t D:i Start TL.. End I--.. re-ai i S&C3 0..0.30 0:00 ID.00 gap-&..Channel 1 Parent 4.3.'@, Daughter 169.00 Dwell IS@cs) Coll Energy 0.30 30 (aV) Can* I V I is r-.t,.. : 2 MM 5l@terf :C-i. @f I He. Sacs St d ime M.@.3 ft.r I ESP- 0.03 0.00 0.00 10.00 Chanr.al Parent Daughter DW*ll (SeC3@ Coll Energy IeV) Cone V 1 499.30 99.00 0.30 45 60 F@t.@. :3 MRM of I buss ftic t3P- Ipntenr Ch:@nel.De-&/ S t:r@ 5End Ti.e M-- Sacs 0.03 0 .00 1 .00 0.00 Daughter Dwell tsocs) Coll Energy (oV) Cons V 1 $0.00 0.30 40 so 4 HRK of I bass ISpnatner @ChanInelans D*-ay Da Star', Ti.. ' M,.,@ End T..,e ..P.. , M@n. I :Iiar.nel Paren- i 43-, Socs Daughter 70.00 ftic ( ESP- 03 0-.00 1 .00 I 0.00 DOOII (SOC3) COLI Energy 0.40 45 I*V) Cone C V 60 Method Report thod File: NL:st Modified: Printed: c. \bLxSSLYNX\AMZLXA062498 -PRO\ACOUDB\10=in- Friday, November 05, 1999 06s22s24 I Friday, November 05, 1999 09:26&28 10 9 5 Page SP1100 LC Pump Initial Conditions Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(*C) Oven Temperature Right(OC) 0.300 10.0 0 400 30.0 30.0 EP1100 LC Pump Gradient Timetable The gradient Timetable contains s entries which are Time A% B% cps 0.00 90.0 10.0 0.0 1.00 90.0 10.0 0.0 5.50 5.0 95.0 0.0 7.50 5.0 95.0 0.0 8.00 90.0 10.0 0.0 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are Time Initial 0.00 0.10 Column Switch Off Off Off Contactl Off On Off Contact2 Off On Off Dlk 0.0 0.0 0.0 0.0 0.0 Contact3 Off Off Off Flow 0.300 0.300 0.300 0.300 0.300 Contact4 Off On Off Pressure 400 400 400 400 40C HP1100 Autosamplar Initial Conditions Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(Al) Vial Number 200.0 200 0.00 9.00 10.0 32 Masslynx -Sample Ust Sample ListC::\MASSLYNX\ameliaO62498,PRO\SampleDB\110599a.SPL Pnnted:FriNov 05 09:25:341999 ige Page Positior FileName FileText MS File 1 110599001 MEOH Blank IOMIN-PFOS-POAA-IS-PFOSA 2 110599002 MEOH Blank IOMIN-PFOS-POAA-IS-PFOSA 3 110599003 MEOH Blank 10MIN-PFOS-POAA-IS-PFOSA 4 110599004 TOX145-RBLi 1049-WBik-1,RWW- Box 99-211 10MIN-PFOS-POAA-IS-PFOSA 5 110599005 TOX145-RBL1 1049-RBL Bik-1.RWW- Box 99-211 10MIN-PFOS-POAA-IS-PFOSA 6 110599006 TOX145-RBL1 1049-6ppb-1.RWW- Box 99-211 10MIN-PFOS-POAA-IS-PFOSA 7 110599007 TOX145-RBLi 1049-12ppb-1,RWW- Box 99-211 10MIN-PFOS-POAA-IS-PFOSA 8 110599008 TOX145-RBLI 1049-30ppb-1.RWW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 9 110599009 TOX145-RBL1 1049-60ppt>-IR,WW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 10 110599010 TOXI 45-RBL1 1049-120ppb-1,RWW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 11 110599011 TOX145-RBL1 1049-300ppt>-lR,WW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 12 110599012 TOX1 45-RBL1 1049-600ppb-1.RWW- Box W211 10MIN-PFOS-POAA-IS-PFOSA 13 110599013 TOX145-RBLI 1049-900ppb-1.RWW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 14 110599014 TOX145-RBLI 1(349-1200ppb-1R,WW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 15 110599015 MEOH Blank IOMIN-PFOS-POAA-IS-PFOSA 16 110599016 TOX145-RBL, 9R03240-300ppb-MS, 11/4/99-Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 17 110599017 TOX145-RBL, 9R03240-300ppb-MSD. 11/4/99Box W211 10MIN-PFOS-POAA-IS-PFOSA 18 110599018 TOX145-RBL, 9R03240/M/Day2giControl,11/4/99 IOMIN-PFOS-POAA-IS-PFOSA 19 110599019 TOX145-RBL. 9RO3241/M/Day2g/Control,11/4/99 IOMIN-PFOS-POAA-IS-PFOSA 20 110599020 TOX145-RBL. 9R03242/M/Day29/Contmi, 11/4/99 10MIN-PFOS-POAA-IS-PFOSA 21 110599021 TOX145-RBLi 1049-300ppb-CCI-1,RWW- Box 99-211 10MIN-PFOS-POAA-IS-PFOSA 22 110599022 MEOH Blank IOMIN-PFOS-POAA-IS-PFOSA 23 110599023 TOX145-RBL, 9R03243/M/Day2g/Control,11/4/99 10MIN-PFOS-POAA-IS-PFOSA 24 110599024 TOX14-r,-RBL,9R03244/M/Day2g/Control,11/4/99 IOMIN-PFOS-POAA-IS-PFOSA 25 110599025 TOX145-RBL, 9RO3255/WDay2gl5ffog, 11/4/99 IOMIN-PFOS-POAA-IS-PFOSA 26 110599026 TOX145-RBL, 9R03256/WDay29/5mg/kg, 11/4199 10MIN-PFOS-POAA-IS-PFOSA 27 110599027 TOX145-RBL, 9R03257/WDay2g/5mg/kg, 11/4199 10MIN-PFOS-POAA-IS-PFOSA 28 110599028 TOX145-RBLI 1049-300ppb-CCl-2,RWW- Box 99-211 10MIN-PFOS-POAA-IS-PFOSA 29 110599029 MEOH Blank 10MIN-PFOS-POAA-IS-PFOSA 30 110599030 TOX145-RBL, 9R03258/M/Day29/5rng/kg,11/4199 10MIN-PFOS-POAA-IS-PFOSA 31 110599031 TOX145-RBL, 9R03259/M/Day2g/5nig/kg,11/4/99 10MIN-PFOS-POAA-IS-PFOSA 32 110599032 TOX145-RBL1 1049-300ppb-CCl-1. RWW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 33 110599033 MEOH Blank IOMIN-PFOS-POAA-IS-PFOSA 34 110599034 TOX145-RBL1 1049-WBIk-1,RWW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 35 110599035 TOX145-RBL1 1049-RBL Bik-1,RWW- Box 99-211 36 110599036 TOX1 45-RBL1 1049-6ppb-1,RWW- Box 99-211 37 110599037 TOX145-RBLI 1049-12ppb@-1,RWW- Box 99-211 38 110599038 TOX145-RBL1 1049-30ppb-1,RWW- Box 99-211 39 110599039 TOX145-RBL1 1049-60ppb-1,RWW- Box 99-211 40 110599040 TOX145-RBL1 1049-120ppb-1,RWW- Box 99-211 41 110599041 TOX145-RBL1 1049-300ppb-1,RWW- Box 99-211 42 110599042 TOX145-RBL1 1049-600ppt>-lR,WW- Box 99-211 43 110599043 TOX1 45-RBL1 1049-900ppb-1,RWW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA IOMIN-PFOS-POAA-IS-PFOSA IOMIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 44 110599044 TOX145-RBL1 1049-1200ppb-1.RWW- Box 99-211 IOMIN-PFOS-POAA-IS-PFOSA Masslynx - Sample List Sample List:C:\MASSLYNX\amelia062498.PRO\SampleDB\l Printed:FriNov 05 09:25:34 1999 10699a.SPL Page 2 Page Positior(,2:,1) InletFile Boftle InjectVolume Sample Type Conc A Conc 8 Conc C Conc D Conc E Conc F 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10min-10-95 3 7 10min-10-95 4 8 10min-10-95 5 9 10min-10-95 6 10 10min-10-95 7 11 10min-10-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10min-10-95 11 15 10min-10-95 92 16 10min-10-95 12 17 10min-10-95 13 18 10min-10-95 14 19 10min-lG-95 15 20 10min-10-95 16 21 10min-10-95 24 22 10min-10-95 92 23 10min-10-95 17 24 10min-lG-95 18 25 10min-10-95 19 26 10min-10-95 20 27 10min-lD-95 21 28 10min-lG-95 25 29 10min-10-95 93 30 10min-lG-95 22 31 10min-10-95 23 32 10min-10-95 24 33 10min-10-95 93 34 10min-10-95 1 35 10min-10-95 2 36 10min-10-95 3 37 10min-10-95 4 38 10min-10-95 5 39 10min-10-95 6 40 10min-10-95 7 41 10min-lG-95 8 42 10min-10-95 9 43 10min -10-95 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 - 10 10 10 10 10 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 44 10min-10-95 11 10 FACT: DA'I*AREV'IEW SUININIARY FOPNI DataAnalyst: FACT Study0: 7o)IeY5' Matrix/Timepoints: Sunple List- o- Set-upAnalysis Date/Anairt Instrument Anabrte: TOAA (",L., t)o AcceptablLeiam Raugm ti LOQ7 R^2: 0.?.io.154 CalibmtionCb-ks: Exewdm Bb& les-,4irAl Blank lss -1,(A,/00 DatitReview Sign-Off AnalystReview Name / Date: i;@ T-bakal Review r Nana / Date: gq QuaRty Assurance Review Name /Datc: Data tntrr. LAC, Camumats IJusdfkstio= Z.,w lettl @6v-b-qi liil,,Iql /2- DataSton: tAL 1111.5191'j Anslyte: 7,GS L/6Ae7- AcceptablLeinearRaW. LOQ: 3-7ge4 R^2: /Z..3oiZeA tl T;vtracteBdbuik-- e3s 4. zo,2 Matrix Bl&nL -elL. CiklibmtiCohnecks- MS/MSD- No@ 4uk Data Stamr 0 y@ 4@Lp- roLmota -IAG llllrlqi Auslyte: pcbS.4 ( ri,,L3c Ac-ptablc LinearRange-. LOQ: fi Exuwtcd Blank- R-2: Matrix BL&nk-. C.alibmdonChecks: ---P -/J DCt@a ho@ LA-IPA , felltr4 @on, caal ii ID&ta Satus: On itit)sl@R LAC, itlisiq@- -)e@h "&k IllAaIW74 J,#@vA -ILI@OZ 4L e&@lle-Ag.,eiL.Z-/eJaaZL-/ vni PDAA it@O-L /Wz- FACT: DA'I'AREVIEW SUtNIiNIARY FOP.@LNI Date: Data Analyst: i j@!s FACT StudyIt: M3trix(Timepoints: Sunple List. Set-upArWysis Date/AnalM Enstrument @6,b 0211? 1 Analyte: @5aky A=pubia Lamt RaW #A LOQ. HA R^2:. "A CalibratiCohnecks: AIA MSIMSD. Nolr." ,DataStihm EV=.&n Bkk Ma&m BW& AIA AlAf anrAl,,A LA DatikReviewSign-Off AnalystReview Name/ Date: 3@W fLi ZU TechnicalReview u Quouty Assurance Review Nam / Date; Ds taEntrr. Conumnts Jusdikations: A-- Antlyte: AcceptableLincarRange: LCQ: R^2: CalibratioCnhecks.msaam. [DataStu= ExuactedBWk Matrix BLan Analyte: AkcceptableLinearRAnnggcc--. LOQ-Q:p. R^.21. k@02/ CaliibbmdmL i-ccccakkrlMS, M Extmtcd Bla@ Matrix BLank. .C@D Sft. Q@tify CompmSbd @%MMCY ROPM@ T=43-cot ii"rl day 29 d... samim Litsti: Last no4i ad Nothod: L@t nodigi": Job Code; @i.t.d; TC,huUUAASlLwVIM1%1*wA0p7O92069l3939.0pr.1%9N9-9tb= Thu 11 07:08,22 1999 Th. 11 07.26:3S 1999 lll4/99 Mm %11102ta Cool,@,,A 1: PoAk (POW 1) S2 "ii-iollool 3 11120990032 11109900 0 4 5 1110990 5 6 111099006 7 lllo99007 B lllo99008 9 111099009 10 111099010 11 Lllo99011 12 lllo99012 13 111099013 it lllo99014 15 111099015 16 lllo99016 17 111099017 is lllo99010 19 lllD99019 20 111099020 21 11109g9)021 22 11111100990 022 23 23 24 111099024 25 111099025 267 111099026 2 a 111099027 2 , 11109 028 2 0 111099029 3 1 111009,9030 3 3 2 111109;003312 33 111099033 X.Ml.ii.t T@ X&OH Blank NOOK BBllaannkk N-OH TOX145:RBL12049:WBlk-2. _2 RWW TC)XL&S RDLil a 9_ RDL51k . RWW TOX145 RBLII 119 6ppb-2. Rw -MXIAS-RBLII049-12ppb-2 BMW TC)XI45-RBLJ1049-30ppb-2: YMW TOXIAS_RBLII049-60ppb-2, MVW TToonn,&5- RBLII:49-1200ppb-2: RW S_RBLII 49-30 ppb-2 mw TOXI&,S-RBL 1049:60OVgb- 2 PW TOXI 5-RBLIII 49 900ppb-2. RW TOX145-RaLliodg-1200ppb-2. RW X.On alnk ToXiAS-RTL. TC=45,-*TL, TTO.X"I _ S-RTL: 9903255/X/Day3g, lk4 1@.00 .0: /99 9R*32S6/N/Day2 :1Ol2"l*"Y2';,I=,I@kg.:D".@00 : 11.1.14.1.99: Tents-RRTn L. SR03259/MiDay29/5M/kg-DIOO, TOIJAS-RikLllo49-30OVpb-CCl-2. RWW 11/4/99 RTC.X0I9,5B_lank IOXI,S_ RS 11004:-Wzlk-2, RWW L -2. RW 7OX115-"LRIZZLOl6l1-6&pp-bR-kB2L,DI RW TOX145-RSL13LO19-12ppb-2. AW Ton&S-RSLI1049-3OVpb-2. FMW TO.X.I@S"__R.a,L*Ilolg-60ppb-2i,RWW TOXI&S-RDL l11lo&49g-3000pvppbb-2. rpm TTOoX14S-ML11049-60OPPkl- 2. RMWWW X14S -RBL11049-900VPb-2, RW TOX145-RDLIJO&9-120OVIpb-2, RW TYP- Standard Standard Standard Standard Standard St,@Ard Standard Stnda.d oc sSt-m-@d t,@,@d Standard Standard Standard Standard S tm,rd Standard Standard Std C@ itT 6. 12.30 30.70 61.30 32 '610'7o0-o0" 3-00 @.292,0-.o 2 7 125 7 :. 1a 6 7 110 7.0093 7. 83 7.00:7 "7:.6, 7.:6" 7:0.1 77 307.00 62 .13 3601:*7,0.* 30 123.0 3 07.00 613.000 121207. 00 20 7.089 7.1006 7.1 5 7.10a4 "7.:0*68s 7.0 7 56 7.064 7 66 7:.00.14 7 6& TA A-. 71.9s C- %D" IS hb 116 PM 104 bbX 137 bbX III -a 54 bb 4 5: 1797 MN 12047 Mbb 00 .00 -01 75.4@.5 _23 350.9 651.926 14 993.50 1164.17 -7 382 bb 9 bb 101 NK Jos2 bbX 12 mm 154 bk.X 9 bbX 221 bb 444 bb 693 bb 1 71 bb 12a37 bb 274.09 -11 0.00 0.000 I- 00 13:605 49.5 111.55 336.3 586.960 966.64 1134-04 -100 -150 -9 1-04 5 -8 IW4 saup 020199: gq----Itatod&ad pristod by I" m 11111/11 O'@tity COMWOUVA S%Mmmxy ROD* T=45-rat li@r, day 22 600* 417,Uzi@- @. 11/4 s@PI 0 List: Last modified: mLe,thod: = modified: cod.: ?in E" 11 07:02:30 1299 Ct%M"SLYMX%SoIW*20199.P"%Mtb=%Lll*99& Thu Haw 11 07:06:22 1999 Printed: Thu now 11 07:26.-315999 C@.v@@=d 2, PPOS (P@ 2) 1 @..99001 2 1110099,0002 3 111 9 3 d 11100:9004 5 111 9005 6 111009:00076 7 111 9 11109:00809 lllo9 0 101 111099:0010 12 ilia0"0 11 13 ill 12 lllo:9013 14 110 9014 15 1110990015 1176 111099'a16 Is 11100990 17 III is 190 lllo9:019 2 111009 go0201 21 22 I11l1l0:10222 23 11109"90203 24 111009990 24 25 111 25 26 111099026 27 111009999002287 2: 2 0 I11l1l009999002390 31 111 099031 3332 I11l1l0099990032 3 111 33 a.Ml.lLst T@ HOOH Al@.k M.0 :lank K.OHN lank To xi45-RSL.11049-WSlk -2. MXI&S-RaLilodg-"LBlk-2. RW YaN =XI45-RAL11049-6ppb-2. RW TDX145-RaLL10409,-192p pb-2. XWW TOX145-RD 110,9-30PPb 2. RW TOX145-RALL1111049 -60pOpppb--2i.XW WX145 S -RAL -12 b- ON Toxia 5 -RB 11011:-1**,2: 1 T4DX14 -ROLL11 a -6 Ooppb-2 RW TOX14 45-RALI 1049-900VPb-2. PW TIC= S-RBLIJO49-12 Ooppb-2. ON N.OH 'SIII&nk 70XI,S-RTL: TOXI -RTL :ItRo03255:/ IDy29ISm/kg-DIOC. 32 /.,Dy2:IS.9/kq-0100. TOXIAS-RTL TO]Ll,5S-RTL: IOXIA 5 -RTL 9RO32S7AUD-Y2 /SM/kg-DIOO, 3255:/AKUD/WDY" 29/5"/'kg-DIOO. ::0.32 29/SM/kg-DIOO. TOX 4 -RBLllo4g-3ooppb- = -2. RWW moo 2R blank TOXIIS5-RBL 1049-IMIk-2. SW 1 k-.. T.TOO@XXL1I4"5-_.R-BLRlDlLo".0:04&:9p_ 6-pMpLk*-s2l. EW III 12ppb.-Z. Rw TTOIXO1XJ4,5S__RKBBLI10409-30ppb-2. XW III 9-60 ppb-2. Rmw T.O4X,14_S.-RSI 10&1:-1211: Rw 11 4 -300ppb-2 RW TTO.X.1@45"-_R.ZLLlL 1.019-:0000vpb--2 RW TCX145_RBL1110149-4192-00vpbp-p2b.-Z RWRWW 11/4L/19 ii/d/99 11/4/99 11/d/919 11/4/9 IN standard Standard Standard Standard standard Standard SS tandard tandard Standard QC Standard St.-,@d Standard standard St .drd andard Standard Standard anclard mtd C- 6.14 12.30 30.70 1261.400 3.01. 307.00 :14.00 21:00 1228 307.00 126.11 .30 30.70 61.&0 123.000 307.000 614.00 921. 1223.00 7..2,W7$r 94 7.26 7.263 7.263 7 7.:"2,43", 72 7:.23510 7.251 7.2 7.238 7 229 7 26& 7 245 7 .2 ,4 7 2 a1 7.263 7.267 7 25608 72 7.263 7.2&5 7.243 7.249 7.244 7.251 7 2107 7:248 7.229 7 22 7.221 P." 2 Fbblags 47 16 bb "1 1' 'bb 213 bb 271 bbX 333 db :So NbKb isI2s 35706 bb 7216 bb 11229 bb 13298 bb 27 UK 2496 2774 bb 2615 bb 3176 bb 36042: bb 3 19 bb bb 109 UK 185 bb 236, bbX 33 9 bb 54 13$33 bb 35 703 bbt bb .91a2 bb 1129653 bb 127 bb e- . %D0.00 00 00' E- 16:..4'76 12 1 3 22 ..0,0 A 65 6 6 117.79 -4 303 4.:3 -1 6 g 2. a 3 3 2 1184" 3 o 207.31 232.358 225.2 .262.60 311:12 255 32 -17 01.00 l@1I--0,0' -11 3 31 93 57:,o 106.17 -1@6L 304.1,4 -1 :90.,5 -1 15 9 11325. 7 a Ld tA soup 020111: W@titated A" wlated by A" an 11/11/29 gu"tity compound smom" R-P@ TOU465-tat ii-, day 29 6." iii4igg XM S&MVIO Ust: Last modified: method: @t 0041910a: Job Cod.: C INMUSLYIM%"upO2Ol 11. P"%SSMI&VS%ll Tbu Now 11 07:02:30 1191 Tbu U" 11 07-08-.22 1119 Printed: Thu U@ 11 07:26-.3S 1991 lot'& cmwmra 3: PROBA ir@ 3) 0 X1 illog9col 2 111099002 3 111099003 4 lllo99004 5 illo9loos 6 111099006 7 111099007 3 xllo99008 9 Lllo99009 10 lllo99010 11 illo9goll 12 111099012 13 111099013 14 lllo99014 is lllo99015 16 11LO99016 1I7S 1111100:99001187 190 illo99019 2 111099020 21 111099021 22 1110990g2o2 23 111009 go 23 24 111 9 24 25 111099025 26 111099026 27 111099027 29 lllo99028 29 111099029 30 111019030 31 111099031 32 111099032 33 111099033 O.Mi.ii.t T@ N.OH Sl&.k V.OH Blank DI.OU Blank TOX145-RDLI1049-Wblk-2. TOXI&S-RDLI1049-6ppb-2, TIDX145-RXL11049-12ypb-2, TOX1415-RAL11049-30ppkl-2. TOXI&S-LBLI1049-60VPb-2. TOX14S-RDLIJO49-120ppk@2, ?=AS-RDL11041-300ppb-2, TOXI&S-RBLIIO&9-600ppb-2, W)U4S-RBLII049-900ppb-2. TOXIAS-IBLIJO&9-1200ppb,2. RW MW RW MM RW RWW Mw RW MO MM RW moon Blank ?=AS-RTL. 9R03255 /X/D&1,29/SM/kg-DICO. TOX145-ETL, ?C3a45-RTL, IMI14S-RTL. IR032 S6/MID.V,21/Sm/ko-DIOO. 9R03257/X/Day,21/5m/kg-DIOO. 9RO3258/K/Dy29/5M/kg-DlCO. TOX145-Wn. 9R032S91M/Day29/$M/kg-0100, 7 = 45-RBL11041-3009pb-CCI-2. RWW X&CH 45Blank TO]a -RBLII049-WBlk-2, TOX14S:RBLII049-R0SLXlk-2. RW RW ?oXl4S RBLII 049-GPPb-2i,&W MTX=I&A5_RSa_RIBLII 49-12ppb- MOW LIIOAS -309pb-2. MN TOX145-RBLIIO&9-60ppb-2 TOX145-RMLIIO&9-120ppb-i TOX145-RiLlIO49_3 Doppb@-3 TOXI&S-RBL11049-60OVpb-2: . Rw MN RW . RW TTOOXXJ145:5"LRIB1L0I4J9O-&9,0oppb-2 a -1200ppb-2. Rww XWW 11/t/99 11/4/99 11/4/99 lli4/99 11/4/99 c, @.r@ Lnai@,,W ona@eff 231 Standard Standard Standard Stardard standard Standard Standard Standard Standard oc Standard Standard standard sta"rd Stndrd Standard St..drd Standard Standard on Std C@ 6.13 12.30 30.70 61.30 123.00 307.00 613.00 920.00 1227.00 307.00 6 13 132:.300 0 70 61 3 0 123:0 00 -307. 613.000 920. 1227.00 7.848 7.857 7.810 7.948 7.829 7.833 7.837 7.825 7.911 7.812 7.825 7.813 7.923 7.935 7.348 7::357 7 7.84 4 7.9&457 7. 2 7 7:,.,2: 7 30 7:0.30 7.$a21$2 7. 7, 8 23 7 7:.882150 71 7.681 7. 123 7.832 LA r@ A@ Flag. 276 M 107 "H 55 m 94 34M 122 MN 284 NK 492 "H 1134 NK 2097 M 3052 NK 102$S M 20144 NK 31969 m 35&71 NK 44 mm AS NK 73 M 46 NK As0 m 7 bb 8529 1 NK 2 NK 64 mm 04 bb 27a 85 21100292 NK 3948 MK 10281 M m 19121 UM 3 1659009 NK 3 & mm c@. 5.63 0.39 0.00 0.00 0.76 5.85 12.42 32.63 62.98 118.26 321.02 631.56 1004.08 1114.40 0.00 0.00 0.00 %.D- -5 1 6 3 -4 5 3 1 -9 0-0.0 0.'0 0 265a.63 a -13 .00 00-000. 5 @.2 .514 29 13 63 35 121*29 320.82 599.31 999.04 1146.96 -101 :5 _3 I s -2 -79 Soup 020111: Quantitated and printed by im m @@'@"4t5Lt.ygaCt--lPl-wU-rd, "0Y--y at d"oPg*&- "luti@- "t. 11/4/99 OM to," B..Pl. List, 9.8t modilled: n.tb.d; t@t modifiod: Job C.O.; C,@"saLT=XsouPC20199.p"%@SMlg=%Illogta Thu Owr 11 07,09.30 1299 Thu @ 11 07.00.22 1999 @Lntod: Th. @ 11 07.24:35 1999 Compmnd 4: s@ 0 1 lllo99001 2 111099002 3 lllo99003 4 illOS9004 5 111099005 6 lllO99oO6 7 111099007 a lllo99008 9 111099009 10 lllo99010 11 lllo99oll 12 111099012 13 111099013 I& lllo99014 is lllo99015 16 lllo99016 17 lljo::017 le9 11100,900189 I III 20 111099020 21 111099021 22 111009,990022 234 i11l1l0990 23 25 24 2 111099025 267 111009:0026 ill 9 27 28 111099028 329 lllo99029 30 111099030 31 111099031 32 111099032 33 111099033 (p@ 4) B.Mi.list T"t K*OH N*CH H.Om Blank Blank Blank TOX145-RBL11049-WSlk-2. TOXI&S-RBLIIO49-"LBIk-2, RWW RW TOX145-RBLlIO&9-fippb-2, ToxitS-RBL11049-12PPb-2, TOX145-RaLlio4g-30ppb-2, RWW RWW MN TOX145-RSLIIO49-GOPPb-2, RWW TC)XI&S-ILBL11049-120VPb-2, TOX145-"LI1049-300ppb-2, RWW RWW TOX145-RBLI1049-600VPb-2, SM TOX145-"LI1049-goopob-2. AW ToXl&S-RsL41049-L200ppb-2, IMM MOM Blank -mn45-ItTL. luX.145-ItTL, 9RO3253,rM/Day2915"/ka-0100, 9RO3256/n/Day2t/So .9/kg-DIOO, MY29/5001ko-nioo. TTOOXX1I4&5S-WrLR:TL :lRt3O2O32557'.DD.&. y2:/SMlkg-DIOD, Toxi4s- 9RO3259/WDOY2 I /Sm/ka-DIOG, TOX145-RSRLT1L1049-300ppb-CCl-2, RW N*OH 'BSlank TC)II -RaLI1049-WZlk-2. 'TOMXI114455-RaLI1049-RBLBlk-2, _RBLII049-6ppk@2. TTOo)EI 4S-"LI1049-L2ppb-2 XI&S-RDLI1049-30VPb-2: RWW sw SW aw RW To 45-"LI1049-60ppb-2. 'M=X4l15-RBL11049-120ppb-2 TTO,CX)145-RDLI.1049-3009pb-2: X145_RBL11049-600ppb-2 IWW FA#W RW RW TO 45-"LI1049-900VPb-2: RWW ToXnl&5-RnLllo4g-1200ppb-2, RW 11/4/99 11/4/99 ii/t/99 11 /4/99 ii/t/99 CAn Oll CICLKG. no@ TYP- sta C- RT Standard stndrd Standard st&nd"d standard Stan"rd stan"rd standard stand"d oc standard standard standard st&."-d Standard standard Standard Standard Standard 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 7.120 7.100 7.103 7.110 7.099 7.093 7.085 7.100 7.084 7.094 7.093 7.097 7 .09 & 77 .118 7 .122 1.00 7.1006 7.1 1 7 101 7:100 1.0000 1.0a9,9 1.00 7.@ol 1. 1.00 7. 0 7.00674, 1.00 7. - 1.001. 7-00:0 1*00 7,03,k 1 1. "7:Os,0 LAC, A@ Fig. C@ %D- 3832 bb 4057 bb 4828 bb 4819 bb 5133 bb 4720 bb 4662 bb 4633 bb &860 bb 4630 bb &57S bb 13 NK 64 bb 76 bb 9 bb 7 73' bb 3S70 bb 9m 102&2 bb 4 0 It bb 5 .0.7 bd S4235 bbt 600 bb 54106 : bd 47 I bb 5115 7 bd 5471077 bbbb 0.19 0.83 0.99 0.99 1.05 0.97 0.96 0.95 1.00 0.95 0.94 o.oo o.oi -21 -11 -1 -1 5 -3 -4 -5 -0 -5 -6 -100 -99 0.0022 0:02 -98 o00 @.o07l3 .0 .83 -:9291 100 -17 0 .es 1 .03 1.0I4 1. 1 1.0,4 0. 4 0.91 1.005 1. 95 0. 8 -12 3 4 6 -3 5 5 2 S@p 020199: Q@titatOd MA ICiut*d by 1" M 11/11/99 oamt1ty CalLbrati" R"OM T=45-r.t li@, bw 29 do*. diluti@- ext. li/d/99 WNW Compound 1 name:POAA (Fune1) CoefficienotfDeterminabon: 0.980656 Calibrationcurve:0.993942 - x + 109.996 Response type:ExternalStd,Area Curve type:Linear,origin:Exclude,Weighting:1/x,Axis trans:None 1.33e3- Responsex 0.0 200.0 mmp 0201992 Q@titated and Printsd bY i" M 400.0 600.0 800.0 1000.0 Conc 1200.0 ou@tity C&Iibr&tim ROPD@ %lo=45-rat li"r, "Y 29 d.- I.tL-" -t. 11/4/99 som Compound 2 name: PFOS (Func 2) Coefficienotf Determination:0.991927 Calibrationcurve:11.1011 * x + 194.545 Response type:ExternalStd,Area Curve type:Unear, Origin:Exclude,Weighting:1/x,Axis trans:None 1.38e4x Response- x 0.0 200.0, -@oo.0 S@p 0201991 Q@tit&tsd =kd PrLUt*d by i- m LI/11199 600.0 800.0 -- - - - - 1000.0 Conc =ttfy C&Iibwatim RAIMOM OM 45-Tt li"r, "Y 29 "a* oliuti@- Compound3 name:PFOSA (Func3) CoefficienotfDetermination0:.989396 Calibratiocnurve:31.7417 - x + 97.7287 Response type:ExternalStd,Area Curve type:Linear,Origin:Exclude,Weighting:1/x,Axistrans:None 3.9Oe4- x Response@- ....... 0.0 200.0 400.0 "UP 0201991 Qu@titat" Print.4 by i@ M 11/11.199 606.o 806'0 1000.0 Conc 1200.0 Q"@ity calibratim JLOPO@ ii-, day 29 do.. 4LLI@tio"- Owt- OW Compound 4 name: Surr (Func 4) Response Factor:4875.54 Response type:ExternalStd,Area Curve type:RF x 5.42e3- x x Response- 0-1 0.0 0.1 0.2 ------ 0.3 0.4 0.5 0.6 -0.7 0.8 0.9 Soup020129: gwotitated wd printd by L" m It/Ll/gg Conc Method R*POrt method file: last modifi*d: C@.g4.nd: printed: C:\WSLyNX\smpoZO199.pro\NothDS\111099&-=O Th@ *@@ 11 07:00:22 1999 1: PC" (T@ 1) Thu NOV 11 07:34:44 1999 co.p@..d uinternal Ref.: Qu-tify Trace: c.nc. f Standards: U r Rr V.I..: U.er Pak Factor: inta4rat. Wind@ Fsct-@: chr@togr= @as wind@: PC" (I r@ 1) in@ TIC C@ . A 1-.0.0.0.000.0.. Oig",*d 2.000 1.0cooz). Ret...tti@. Ti@w (.iw) R a U i@e Retention Ti@ RT I T- Wid- I-Ii-) Peak golection: Re Typ*; 7 Bn&bled 0:0"..'Q: Disabled o N- .246 ve"eat mt real Polynmial Type: ipointof origin: pit w.ighti-9: Axis Tr@fo@tion: R=Iud. I/X no- unit.: Peak-to-peak awlitude: 82 S@thing: Wind@@ i.6 (sc MU.ber of s@ths: Smothing Method: a-bid 2 I i in valley threshold: R:duce Peak tsiling: Rai.. b ..line -rtical thr"hold: DrD.tac t shoulders; Shoulder threshold; R.1 tiv: h*ig.h Abxaoluc h.i ht: .I.ti@. "..: J.t. r..: 30.00 2 0.00 5.00 90 00 oi.*. .bld 30 00 0. o.: 2.00, 0.00. Disbld Di..bld Di-&bld Di.&bld "thod RePort method file: L.St modified: C@.W@.nd: Printed: c@NNASSLYKZ%B"po2o,99-p,*%NthDB%Lllo99---ft Thu m,@ 11 07:08:22 1999 2% Pros (r@ 2) Th. U., o7z3t,44 1999 compound uInternal x.f.. oumtify Trace: Conc. of Standard@: U..@ RF Val..: U.sr Peak Factor: Integrate Chr@togr@ me& W& Pros(P@ 2) [No-] TIC cow . 5 I.o0o0o0o00oo. 1. 0 2.000 1.000ODa Di.@bld ti@. Time (.i-) ; ti- Retention Time RT Time WiAd@ (P-i") Peak selection: 7.2 o.o.0 tmm I 0.279 anabled Di.@bld N.-.Xt R.Op@". Type: R.op.-O; wAl"t-e@l Polynemkial TYP-: point of origin: Fit Weighting: Axis Transformation: B=Iwle I/X No" Units: Peak-to-P." awlitud*: 98 s@thina: wind- ,is. Number f smooth.: s@thlng method: .I*i.Valley threshold: Reduce peak mi.. b ..line a.-i-: Dr- Vertical threshold; Det@t shoulders: Shoulder threshold: Rel&ti@. height: ilbsolut.height: R.Isti.. -..: Absolute are*: 2 I 120.-00.0.. 5.00 90 00 Di.'. .bld 30 00 1.50, Disabled 0.00, Disabled 2.00, Dis@bld o.00, Diabld N.@h@d K.thad fil*: L@.t mdified: comoura; C:-%MMS.S@ LYNX@2MV020199'9"%M'tbDakIL109 11 07:09:22 1999 Thu 6: S.- tru@ A) Tt. U.@ 11 07:34144 1999 Ref.: Q@tity Trace: of Stand"d. @ us.r User Rr Value: peak Factor: Wid- Factor: ch.-twr- -.4 iw-l Ratentio. Ti@ (.im) jtsl&tive IL@t.ntio. TiM; RT R.fOr*=*: Ti- Wi-d@ (-'-): Peak Selection: s@ (Fu= TIC pi-d 1.000000. 1.000000 2.000 1.0000D. ois&kld 7.161. 000 0(1 0.M2OW78 gmbled Disabled N.-.St Ramp*-* Type: poly@al Type: point of origin: Fit ighting: A@i:*W@fo@timt axterml Axe" ti"" X=Jud. 2/X Pm unit.: P.,k-to-p.ak SMJitud.: s-thi.a: wind- ): U..,b,r :i .a (.C@ S@tbLi:., -@t"; join valley@tht*hdrleshold: Reduce P..), -ili-0: Raise b .. line Draw "rti@.1 thr"hold: Detect shoulders; Shoulder threshold Rol-tiv- AbsolutO R.1-ti@. Absolute height: bmight: area: 92 --bid 2 I 30.00 200 00 S.0; go.OD Disabled 30.00 Di &bl*d -,00,.oi=ld 02 ' 000, Disabled 0.-00, Di..bld ga.ndb Quattro11,#6414E _JA P SOUP 0201":FACT Equipment Log 99092 PAGE 1/1 DATE:.- 1-@0-99@ ANALYST-i-as DXI_4j5 MATRIX:MLlive-r DESCRIPTION.- diju-tio-ns--d-a-Y2-9 STUDY NUMBERJ FACT Method:El&-8-7-.-g Injectivoonlume:-i2-u-l- Cycletime:10ff@n.Electrod_eZ:ap-r-al- MobilePhase: (A)LQMMEK4LU202 (B)Ne-QH-- TN-A-orstndrndumber-(A)Dk&L-LL-2-1- (B)JA-A-Ui Prepared(datelby): (A)11&12@@ (B_)LI&9La@sh Expires: Storeatroom temp? @i or N Other: Guard column: N2ne Parntumber:-na- Lotnumber:-ni---------@ Analyticalcolun2n: Size:-ZzjQ-rnM----@ Partnumber:-925:2a!:2- Type:_Cl@_ LotnumberP:9El_l Spherseize:-I-um@ Serianlumber:0591804Z. Analyticalparameters: ESI nebulizinggas (LJhr)_j2_ Drying gas(Llhr):35Q- LC Flow rate_:IQQ_U_V_M@i-n-. Back pressure:-O-bar- Sheathgas(LJhr)0 HPLC solventgradient:10min-10-95 Time( ,t'in.)- %B@ 2)J-903)J-D4)2.@O 5LLQ.0- 10.095.0 95.0- 10.0- Tuning mothc>d Report C:@KkSSLYM\SOUP020199.pRO\ACQUDB\pFOS3 met]2od: Printed: Ned Nov 10 10:49:41 1999 Page ms SOURCZ ESP- Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. MS2 set' Rdbk 1.60 40 5 0.2 150 250 1.61 -60 -6 150 250 Pressures Analyser Vacuum Gas Cell Rdbk 6.0e-5 4.le-3 msi LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 multiplier NS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy RamP Lens 8 Lens 9 multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 3 650 Set Rdbk 14.0 14.0 10 37 2.0 0.0 40 38 0 40 650 method Report Method File: Last Modified: Printed: Ct%M"gLYNXV80UP020199.PRO\ACQ=8\10=in-I w"nosday, movamber,10, 1999 lOs43tO7 w"nesday, November 10, 1999 10:49t2O 0-95 RPIIOO LC Pump XiLitial Conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(OC) Oven Temperature Right(OC) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 UP1100 L4C Pump gradient Ti@tablo The gradient Timetable contains 5 entries Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 10.0 10.0 95.0 95.0 10.0 which C% 0.0 0.0 0.0 0.0 0.0 are D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 RP1100 LC PumV Zxtexn&l Z"mt Timetable The Timetable contains 3 entries which Time Initial 0.00 0.10 colunm Switch Off Off Off Contactl Off on Off are Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off RP1100 Autosamplar XzLitial Conditions Draw Speed Eject Speed (@il/min) Draw Position (mm) Stop Time (mins) Injection Volume(lil) Vial Number 200.0 200 0.00 9.00 10.0 91 Page Pressure 400 400 400 400 400 Masslynx - Sample List Sample Ust:C:\MASSLYNX\souPO201 gg.pro\SampleDB\l1 1099a.SPL Pdnted:Wed Nov 10 10:48:561999 Page I Page Position(:1.1) FileName FileText MS File 10MIN-PFOS-POAA-PFOSA-IS 1 111099001 MEOH Blank 10MIN-PFOS-POAA-PFOSA-IS 2 111099002 MOOH Blank IOMIN-PFOS-POAA-PFOSA-IS 3 111099003 MEOH Blank 1OMIN-PFOS-POAA-PFOSA-IS 4 111099004 TOX1 45-RBLi 1049-WBIk-2,RWW 10MIN-PFOS-POAA-PFOSA-IS 5 111099005 TOX1 45-RBL1 1049-RBLBik-2,RWW IOMIN-PFOS-POAA-PFOSA-IS 6 111099006 TOX1 45-RBL1 1049-6ppb-2.RWW 10MIN-PFOS-POAA-PFOSA-IS 7 111099007 TOXI 45-RBLI 1049-12ppb-2,RWW 1OMIN-PFOS-POAA-PFOSA-IS 8 111099008 TOX1 45-RBLI 1049-30ppb-2,AWW IOMIN-PFOS-POAA-PFOSA-IS 9 111099009 TOXI 45-RBL1 1049-6oppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 10 111099010 TOX1 45-RBL1 1049-120ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 11 111099011 TOXI 45-RBLI 1049-30oppb-2,RWW IOMIN-PFOS-POAA-PFOSA-IS 12 11109901 2 TOX1 45-RBL1 1049-60oppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 13 111099013 TOX145-RBL11049- goOppb-2,RWW IOMIN-PFOS-POAA-PFOSA-IS 14 111099014 TOX1 45-RBL1 1049-1200ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 15 111099015 MEOH Blank 1OMIN-PFOS-POAA-PFOSA-IS 16 111099016 TOX14-r-RTL, 9RO3255MMay29/5mg&g-DlOO, 11/4/99 10MIN-PFOS-POAA-PFOSA-IS 17 111099017 TOX145-RTL. 9RO325&M/Day2g/5mgtkg-DIOO, 11/4199 IOMIN.PFOS-POAA-PFOSA-IS 18 111099018 TOX1 45-RTI, 9RO3257MMay29/5mg/kg-Dl 00. 11/4199 TOX145-RTL, 9RO325&WMay29/5mg/kg-DIOO, 11/4/99 10MIN.PFOS-POAA-PFOSA-IS 2109 111111009999001290 TOX145-RTL, 9RO3259AA/Day2g/5mg/kg-DlOO. 11/4/99 1100MMIINN.-PPFFOOSS--PPOOAAAA--PPFFOOSSAA--IISS 21 111099021 TOX145-RBL11049-300PPb-CCI-2. RWW IOMIN-PFOS-POAA-PFOSA-IS 22 111099022 MEOH Blank lomIN-PFOS-POAA-PFOSA-IS 23 111099023 TOX145-RBLl Io4g-WBik-2.RWW IOMIN-PFOS-POAA-PFOSA-IS 24 111099024 TOX1 4-r-RBL11049-RBLBIk-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 25 111099025 TOX145-RBL11049-6ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 26 111099026 TOX1 4-r,-RBL1049-12ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 27 111099027 TOX145-RBL11049-30ppb-2, Rww 10MIN-PFOS-POAA-PFOSA-IS 28 111099028 TOX1 45-RBL1 1049-60ppb-2.RWW 10MIN-PFOS-POAA-PFOSA-IS 29 111099029 TOX145-RBL11049-120ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 30 111099030 TOX1 45-RBL1 1049-300ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 31 111099031 TOX1 45-RBLI 1049-60OPPb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 32 111099032 TOXI 45-RBLI 1049-900ppb-2,RWW JOMIN-PFOS-POAA-PFOSA-IS 33 111099033 TOX1 45-RBLi 1049-120oppb-2. RWW 34 111099034 TOX145-RBL11049-900ppb-2. RWW 10MIN-PFOS-POAA-PFOSA-IS Masslynx -SSMPIO Ust SaimpleUst:C:\MASSLYNX\souPO20199.pro\SampleDB@l Printed:Wed Nov 10 10:48:561999 I IOgga.SPL InletFile Bottle injectvolume Sample Type I lomin-10-95 91 2 1Omin-1 0-95 91 3 lomin-10-95 91 4 lomin-lG-95 1 5 1Omin-1 0-95 2 6 10min-10-95 3 7 10min-10-95 4 8 lomin-10-95 5 9 10min-10-95 6 10 10min-IG-95 7 II 10min-ID-95 8 12 lomin-10-95 9 13 10min-10-95 10 14 10min-lG-95 11 15 10min-lG-95 92 16 10mir,10-95 12 17 lomin-lG-95 13 lg 10min-10-95 14 19 10min-10-95 15 20 10min-10-95 16 21 10min-lG-95 17 22 10min-10-95 92 23 10min-10-95 1 24 10min-10-95 2 25 10mir,10-95 3 26 10min-10-95 4 27 10min-10-95 5 28 10min-10-95 6 29 10min-10-95 7 30 1Omin-1 0-95 8 31 10min-10-95 9 32 10min-IG-95 10 33 10min-10-95 11 34 10min-10-95 12 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 - 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 Conc A Conc B Conc C Page 2 Page Position(:2,1)