Document qaOZmk1K7R7jooagBy7XKdbdj

DownloadRandom document
R226 - 3546 ATTACHMENCT italte Deoa0 000175 Ee LSORLEY)AY SaAlRih ie `Nove1m1,b2e00r3 `MGEsP.laLsytnincHsall 2148North 2753" Road Ottawa, IL 61250 Dear Lynn, Ihave attaachcoepdyof the C8 report. Please letmeknowif Icanprovide any additional information. el Regards, Tom Livese; Algoflon PTFETechnicalService retitaid 000176 | EXYe&R E! Ren | Analytical Report | Fluorochemical Characterization of Wastewater Samples Solvay Solexis PFOA Sampling 3/03 | Exygen Research Laboratory Report No. L34300 | Testing Laboratory Exygen Research St3a0te58CoRlelsegeea,rcPhAD1r6iv8e01 `Requester `Warren H. Buck, PhD. Solvay Solexis 10 Leonard Lane Thorofare, NJ 08086 RaEe BlTeer, usa cerors ia) 000177 i 1 Introduction LRaebsourattsoriaerse, Irnecp.o(rtdebda Efoxrygtehne Raensaelayrscihs)o(fExwyagleenr) fsraommpSloelsvaryecSeoilveeds.byThiCsenrterpeortAnparleysteinctasl resuls assigned to Exygen Researchstudy number L34300. `Speciic fluorochemical characterizaion by liquid chromatog/rtaapndhemy mass spectrometry (LCIMSIMS) was requested fralisamples. A single sample was receivedforanalysis. The samples were prepared and analyzed by LC/MS/MSfor the folowing ist of lorochemicals: Table 1: Target Analysis 2 Sample Receipt dTahteeswaamsplesuwppalsiesdu.bmTihteedsnamapplleastwiacsconrteacionenre,datonam/b1ie4n/t03t.eCmpheraaituorfec.usNioodsyamipnlfeorcmoaltlieocntioins presented in Atachment C. 3 Holding Times "T`shaemapnleasl.ytAiclaslammeptlheosdweurseedawnaalsyzveadliwdiattheidn a1g4adianyssatofmraexceiimptu.m holding me of 14 days in water 4 Methods - Analytical and Preparatory 4411.1 SLaOmpMleSPMreSparation for LOMSMS Analysis Wreamtoevresarmespildeusalwcehlroeriinen.itSalodtrepahtaedsewietxhtr2a0ct0iounl(oSfPE2)50wamsgIuLsesdodtoiupmretphaiorseultfhaetesaSomlpulteiosnftoor LThGeMcSa/rtMiSdgaenawlayssise.ulAofdorwtiyt-hm4il0i%temraptohratnioonl:ofwastaerm.plTehWoaselutraatneswfearsreddistcoaardCerda. STPhEeccaarrtrtirdigdeg.e wbyasLOthMeSnIMelSu.tedTwhiitsh t1r0e0at%memnetthraensoull.tedAin5amnLeipgohrtlfoonldofcomnectehntarnaotliownasofctohlelesctaemdplfoersanprailoyrsitso analysis. Pace20es 000178 UO/US/UD WEL 4b Lu ik 419448100 wee wos | 412 Sample Analysis by LOMSMS | A`aHnaolwyezet-tPhaecskaamrpdleHPe1x1a0c0tsH.PLAnCalsyyssitsemWacosuppleerdftoormaeMdicursionmgassselUelcttiemdaMreSactSiown amsoniutsoerdinfgo (SRM). Samples were extracted on 3/26/03 and analyzed on 3/27/03 and 3/28/03. Raw | analytical data can be found in Attachment D. i 5 Analysis | 5.1 CAca6l-ipoboirnattcihaolenraitiofnorchureveawmapsouannadlyzofedraetrth,e TbenginCnainlg iofnthpeoratnsaywtcealrseeqpurereceata2n5d 50, 100, 250, 500, and 1000 ng/L (ppt), as perfluorooctancic acid (PFOA). The instrument | rWeeisgpwhoetnirnsoge,evtteehrresmuSisinotpehade,cyoA-ncncateeinrbtcrreaaptitiooannncwduarcsovrepirlesolatatteicdonfcocroeeefpafcitchiepano>tibn(0t.)9l6aUe2nsdi(nc7goelfif0ni.eca9ir6e5nr)te.gorfedsestieornmwiintahti1o/nx | ---- Calibration standfoarMrSd/MsS analysis were prepared using the same SPEprocedureused Fortra resus reported hrs, calbration teria wera mat. | 52 xBEtxltrraaanccitkoisonnbbllaannkkssshWoeurlodprnoopahraevdeaannydatanragleytzaendaWliyttehsepverryeextasrlaocertiaobnnobvtaetcthheofcosncaemntpraltieoTnsh.oef ho low-level calbraton standard. Forthese samthpeextlracteionbsla,nkswere complart, | oInvseircuamlebnrtatbiaonnksstainntdahred,foarnmdofafctlreaknnmoewthhaingohl-lseovlevlesnatmwpelerse.alsAogaainna,lhyzeedblaafnekrsesvheroyudhingoht | hSaamvpeleasnyprtaasragneitecanhaalryetetsheprIonssetnrtumeanttbolraanbkosaverethcoomlpolwadrotv.al calbraton standard. For the 53 Surrogates `Surrogate spikes are not a component of the LC/MS/MS analytical method. 55 Duplicates ATthaecshammepnlteA.was analyzed in duplicate. Resuls ara given along with the sample results in 56 MLialbiowraatterorwaysCsopnitkerdowlihSaPmFpOlAeals50 and500 nL. with each exiracton set. All laboratory control samples shoved racovaries between70and 130%. 6 Data Summary Please seoAtichment Afor a cetaled lstng of the analytical esuls. Al resuls are reported in (nglL) parts per trilion as PFOA. raceaoes 000179 7 Data/Sample Retention `SaacmhploensccarleadlisopoAsTecdhWofedoonenmroenttihoavfatebretheedreapoarnt dis ihsasrudedcoupnylersespoothsearwriesessopreecidfiied.atAall folders maintained by Exygen. 8 Attachments 81 Aachen A Rests 82 Attachment B: Chain of Custody 83 Attachment C: LC/MS/MS RawAnalytical Data 9 Signatures . Paul Gomnoly Tears Loader, LYS John. FancyV,i rac 25 Banse Date 3 Other Lab Mambers Contig o Data Karen Smith pacers 000180 Exygen re ResReaErchSEARCH raven Ress. a Pes Analytical Resiits Solvay Solexis Wastewater Sampling 3/03 Solvay SolexisSaiple Identification PFOA (nglL) 00330088533 (oratory duplicate) 7745010000 Limit of Detection (LOD) for the procdure is appoximely 10 nglL Limit of Quaniaton (LOG) or ihe pracodure is 50 ng ND - Compound not detected NG - Compound detected at level Batwasn the LOD and LOQ. Results not quantifiable. ND<LOD <NQ <LOG REE8 ERs Bihan, usa IHs14T2721035 000181 7% soivar| SOLEXIS Mach 13,2005 . JBoahgngeFaRbeescmyrc, Inc. 30S3u8eRCesoelaergc,h PDAi1e6801 Dea Joa: rhetcLoiadaet9s3c0sa83ci.one1edwoGuralomdmpPlheeVoDf10vhaacaesvsttahelay|rzoehmdaavegoaer mopfeoesout,oAclwgsooifunloodsigc P3sTdFtEhPahFtOtehAe)cc,uosintncomsdeuapcclsai.ctaothen.viegBgahisvebedenon he arnegteinof5temesofapnudeMslpeAsccoluinoens bPuatyi|bldeotusndneopwosipnetcisaoldyewsha#t12h3e07c0o7s,tomPelcseopraolcleisf.thleeessaeseanndy ttons shBoeeugt Since, 030F3 AacyceanlH.SBeurcvikc,ePshManD.ages L350 | 2/14 (ices 1235 Sew 16 LEONARD LAN + THOROPARE, ) shane 000182 I. Co a pe - | a To = mr ee pe omm TeBa e Tackingh___ 1963 1r put Oter expan rpgesetoer m | sEe2yEre--n---- eoS mrymE mzE rw2x |||rngBTOsFRRmE fee r[oe Be ere ili a ee[7 ee i | !i r TeT oevee ooenm I -- Samplesreceivedwitinholdingtime? OYes ret 0No(asplain) Wf 1 fost sooo ] ue Lfus 150 n Contacted ONo --_-- ew (Timer R Ts R --= 000183 LOGIN CHMAaIrN O1F4 C20U0S3T,ODY03R:E22PORpTm (1n0l) 1 AccouLnotg:in2N9u8m0berS:OLV1A3Y430S0OLEXIS } EsL seE eaaahee ROT | rage 1 Signature: r Sede i m oes nan Date: Big ate e r s _ - 000184 J iDstinointee i10o a =- rwsmensszons fr-- Lm s nt P fioo. jsSooute ne mTEmR aLarneimnsnnnt vame ve7am b.e ew Mae w o"n dhn e rm hoW eu e eaonn eRem 5 EE frTfeeemdd ec ::: : S$3Eg voI memn:o+w poms l== 2moL sfcrSEaoivee ::: " g2rSl fC p Emmu en m = mel: Emel oe sJ Steemnis =I=o on m aTomE weene Tome llLo mm moomm om Mom aoa oo>mn oy fra ie ::" : E SEEm Emm Emsr ITBWoRZ OTI o --ed :: F EENEEA lm ORPG A a BTewats stil) wo or rLe TcE a EPA p ESnmoCiotne BRrT-- . Jp r-- n a15T5on senna. lel 000185 r-- ee ------------------------------ SOLEXIS Mach 12,2003 . EJ5yo0b3ae8FRaRbeeectwsy eDtieoc. . SueCollPAe1s68,01 Decjober iFcEoe03003. 1vouldshe oba brnlcfo peciocin12e4 (PFtOn Ap)he,. Bred 23 treangetsofstaemmpsloefsprto ePpVeDlFiin,set]adto vFsosohpyec]Bcwloyldhafti ittohme conrcaescseio,n lghteetBy hoenesisthoomoeBr1esSt Aco Posieunderpoate aide VIO lw cf ocvk a Scr Hoan Bok WpireecnhsiBtusmdveA.tv1ili 03003 L3Y200- | 2/04 frees Io25 Soe 000186 RESnEARCH SStsattReCeolulghe,DPAiv16801 PoFmasx 184126237121150800 SAMPLE TRANSFER SHEET Protocol Number: NA Exygen Study Number:____ L34300 Cows| ow |. RDeey,qBsy(uhPrienettedhNsaormnte/DaetrT0dic3)/24 [oz `SSaammpplleessrreemmoovveeddffrroomm:: De-- msJC3 BBooxr#t. SShhaelit ---- copsmstnsiosncasoyet Log Toole fl rhels 127 SampleCustioidlDiateaTinme Samples ecivdfom custodian; Samplesmovedto _R{32- i oslatfos 1235 LaboratoryPerfioelIniDuleTiyme Samples moved om Hn Samples rewmed tof _____e Duwn i) g fg Comments: SampleCsualsaItndtoilssdDaties/Tzaime December 19, 20026 000187 BnE S30u5e8cReoselarlchePDargi1v6ee0,1 PhoFnaer:: 881144-.227321-.11053890 ExSppeornSSuldyyPNrotoboecrl.Noi IN1n3At6e2r0n0al Chain of Custody/Fortification SVhieeewt: Sasa TT he sampi les sted blow werened romrepeN atNo. s wes dA TC m 1-- EoXoYmsGEmmNoIoDcsNwkUMsaBET R | |[VOLwaUM0oE(mL)||FORTIaFI0CATI@O|pN| T w w oopsmeowsws T | | wwoo| | .mo || r ww | Dewirg r | eo | | r -- r r rr r r rr r -- PS SY PS ESP 11 r -- 1 r 1 r1 r Cr [o[ man|SmoC misssosutioontnos ||sVooruumeoT Usnemoersspeikiong||TGamGmAeH| -- O r S r rEvS rr AEP Cr 1 | Aswei r mee nd: Tw[e 4/0 vue 03[2hfoz wmidals AMA Toter ons samwepraleneUdsSgEnSNo.3. iets __ YE, Comments: 100, of250mp.sod entivassed olsnpls lrspin isst0Av03u/2c6/:03 Analysis Summary: `pDua Sget:_1B26idg0na 3BSHV) Dias = Setoxmotonhestys dsverifyf:ol. A. Iwnitiaol Dnate:B. l Givione 7T36 3y 0006 000188 li H 28 g 1 h I il + bt Cn :Y ih Hiieii] 5{HHH i HET EFsk aTd, 4 Hiito & fl Fes id|] [F980 pi Helt iTH1 000189 9 Eli A g 3% LS 8% 3 i hE i : : & of & 3 EE: ght 3 5g i Tog gr RElBEEAZER Bog CEELJeee| e8dd : df i HIP TEICCCECCEN EI | is 3 7 $id . ah HE : 1, [i | Hadi1d] E: | iE :E efi, EEFFEER LETH cE QQ: 3 HEREFEREEEEEEER p8H 3331 3i 1 KILLER & HHiiE: J {4 1 1937315552533 sh 65 000190 [a SF . eesssessiis 2 8 s d2 na2 :Ss . |i :Ee Eoviiiiinnninin |z _0s8888) 128, nesnsd | iE 1$ E 3353350 33 003333 8 | Eoin Berl] omRRRRREnincRRiuiEe i83as| ih EINER RRERERERARREE] | 3 gg Bruni FH oY Femme Pog 8 | |a - 3| $ | i | Cf |: EP 2F3 fHda |g Ha 58382233 88 Bgl paeaceRnRRme 5 foaid 3 : BEEEEEEEEEEEES TBiBt Hyb messierasssssas LC/MS/MS SYSTEM AND OPERATING CONDITIONS `Sponsor Protocol No:NA ExygenStudy No: L34300 Instcument: Micromass Quattro Ultima (LOMS/MS Unit #7) Computer IBM Intellitation M Pro Software: `MWiicnrdoomwasssXPLiPmriotfeeds:siMonaasls:LVyemrxsi4o.n0 5.1: Service Pack I HPLCEquipment: HewHlePttQuPaatckPaurmdp.(HP) Series 1100HP Vacuum Degasser HP Autosamplec HP Column Oven HPLCColumn: G(enJeOsNiEsSCC-H,R5OcMmAxT2O.G1mRAmPHidY.:x4Ppactt(NEo.xyFKgSeI9Dn6:2E7)24) Mobile Phase (A): Mobile Phase (B): 2mM AmmAo cetatneini TypeuIWamter Methanol fe 110? Analyst: EKxayrgenenRiRsehsaearch 3Ph0o5n8eR:e(s8e1a4r)c2h7D2r-i1v0e,39StFatAeXC:ol(l8e1g4e), 2P3A1-115688001 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwriten Peak ID's by: MY idethor 000193 Experiment Report FiSloe:nate: Prived: cBALiymasslynxifCTlhEuuoNrrTosRcdhEaeKymaiMcraaerlncs.hsp2r(7oK,\a2arc0eqn0u9Rdib1s\hp4ef1)o3a.3e9xp Reason Update sovent deioy Thursday, March 27,2003 1430.03 Hue ls | Page 1 | | NaCrmeaetion Time TDhefua2ul7tNEixrpe2r0i0m3en1t4:13:39 | VIenrssiinomnenNtumdbeenrte 10 SoCSDauvrtoeaotnrniatoinDDoe(onlmaaiFnyyi)SeEtrnaarmd2e2 Ca8iM00saossLymcalbraton proCAUDEINGIRCs0325023 SSNooallmvvbeennettrODDefllaFayuTnvectmaopnreV.ralavteur2Eenabled i100 Function 1: MRMof413.00-5365.00, Time 0.0 t 8.00, ES- ToPaynrpaeomdeteer Fe viCmeamssynsdstaulprotacqudbdefatpr Iter Channel Delay (ec) or StE`aSEnprahanTTPi(imDemiae)(a(h)mminD)au(Da) Owls) Caney)a02000Col(eV) Delays) T1560 haan "030 G00 1000 0.05 000194 Mathod Report LMaestthoMdodFiifliee:d: ~ignature: Printed: T:hu\rsdM ay, aMa0rs 0c8h-aa 2p7t,o.L2p0r0o3y\A1C4m Q:U0D9B:x5\0Ra\tex ARBeytaWsCeoEdnNnTeRcsErde\aakyta,eveHnMsPaLrCc(hKmaa2rt6e,hnoRd2i0s0h3a)13:07:14 Thursday, March 27, 2003 14:50:56 HP1100 LC Pump Initial Conditions solavrents cBoy or SFtloopw T(immle/mi(nm)ins) MMaixn PPrreessssuurree ((bvaarr)) OOvveenn TTeemmppeerraattuurreeLReifgtht(+(-)C) P1100 LC Pump Gradient Timetable The gradient Timetable contains 10 Tine 0.00a ssono [2 solo 0c.t0 00 710000 7.50 1f0o0o0 ol 500..00 10000 5s.l5o0 13050 0o.l00 100"a0l0o 0.0 pra 1415700000 s0o.l0o 0000 0600.0 0000 105.00B0300 43050.0 slo entries which axe: o0n.0 00.00 ooloo oooo ooloooo 3 Flow0 (ml/min)0.P3r0e0ssure ooil 00.330000 00[3 00 09..330000 0/400 oolo 00..440000 oooo 0.330000 HP1100 LC pump External Eveat Timetable The Timetable contains 4 entries which are TTnii0mt.ei0a0l ColumoerSwitch oe Conotea.ctl ots ContoFaect? ott 80l.0100 oottte oocnt oonte Conotfact oottee ote Conotafctd ootttt EH P1100 Autosampler Initial Conditions DEDjrreaacwwtSPopSsepicetdeidon(41(/nmm)in) 2200000..020 IStnojpectTiiomneVo(lmuinmee) (41) i15s0l00 TvihaelrmoNsutmabteron 1 ThermostatTemperature (C) 12.0 Page 1 140000 10000 30000 110000 01000 000195 TuneParameters Pag1e FiSlme:atwe: Printed: CAl:\MassLynTxhfulrusodraoychMearmcihca2l7,s.2P0R0O3\1C6Q:U0D1B:\08PFOA Tune.IPR BRyosson 'nCewENtTuRnEeKfiaerens (Karen Risha) Thursday, March 27, 2003 1455717 [Fn Hekate i 8 : 5 i Ea + Bi Se cea HE ae :; Ria N ReE = TDayappeter Scan Source 5) Capillary (kV) CFoannet((V)) HApeexrzt(urve) (V) SDoeusrocaetToemnpTeermapteurraet(urCa) (C) Cone Gas Flow (LH) Desolvation Gas Flow (LHr) An(iaNMily1sRReeesrsooiluuttiioonn ElonniaEnncesrg1y CaE[lNt1i2soRensolution lMHoiMnp2elRneeersrog(l21uytion PPrieasnsuPrreesGsauursg(emsbac) Penning Pressure(mbar) MPrUoXbeConfiguration ER SRSA ss SFtortMiss Settings 3.00 0100 00.00 1a000 131 669 S1$o35t00ings 2Bioo 21I3s0o 272 BEEndMiss Readbacks 294 -11 FSSetass 0100 Readbacks os 95 11403 OFF Standard 000196 go UUNUR ne anisy eas ausesaroiy wre rr a |`QuantiNfSyC3a4li3b0r0at,iointRaepSokrt0326038 SOLVAY,-EXLDAIS 32603, Ansyst Kish ;| Sar AByson FCoPrdoaEcye,NssMiaTnrgeRn2E5(.en25R.o00t70e08)A3M printed: Friday,March 28,2970:109A3M }{ CMeotlhborda:toCna:M2a8sstLaryn0x0fi3uaosroscehtesmicals.PROWethDEVPFOA 032603.mdb 28 Mar 2003 08:18:18 i} { CCooRCrlorbmerpleaaottuionsondnycconpeapaefmr:fesiE:coxi8Pee3nmF.tnaO5lrA7S=60sc3..9"3Aex3r08e40a5.,03203 =0.9861 3 8 : Cemntlpee Gone, Org: Exc, Weighting: 1 Acsrans: Ne "ves Page 1 of 1 Boils ExygenEFReEseaErch,:058 Research rive taT e ColegT e, P-A 16R 801, Data acauakeed an LOVSHSE7 eeon 000197 S`QtuuadnytiNtoy.1SLa3m4p30l0e,RDeaptoarStet0326038 SOLVAY-, ExtDate:03/26/03, Analystk Risha SDantaotsweet: ALC:\WMasFsrUiydmafyu,oMroacrhcehmi2c6,al2s00p3ro\8:00372:60083A8MSOLVAY.qid RByeason PCroEceNssiTngREW(KaarreneRinshsa) Printes:__ Friday, March 28, 2003 8:07:13AM nRDaiitano ,dZESAGEE--SE& Page 10119 EE | CMaeltihboradt:ioCn::W2a8ssMLayrni20f0u3or0o8:c4h5e:m1i9cals.PROMethDBIPFOA 032503,mdb28Mar2003 08:18:18 DNaatmeo::270-3M2a6r0-3280300301 DTeismcer:ip2t1i:o2n3::5X8C031703.0,0 gl Standard | KCeCRErSBToI3E0S04,10S0go.Soanne20) 055 * om 35 ag en 7 as2f aq 38 2 MRMoffcfhairnelie5e. co onfom 5 a. 50 sans aR 20178 70 TR TR 2h 2h 3k mak aE eh - wk ek wh 7h mTEreabein Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMSH? 000198 are `Study No.:L34300, Data Set:0326038 SOLVAY,ExtDate:03/26/03, AnalystK Risha E Bet Ge ob rorsi LAY 1 BRyeason PCrEoNcTesRsEiKngarens (Karen Risha) fBweEoyenmasercOscSosntn ehyevernso =or Description: XC031703-1, 26ng/L Standard sta3gs I. : de oUn RIi"BE mR see se ws T TRT TT 640 6.57 675 IT E. Es 108Ros se ve,a StCele, ,P1801, CntspisnLeCHHdHT 000199 SGutiynNioySL3a4m5p00e,RDoapteerS0326038 SOLVAY,ExLDale0928105, Analyst KRisa Datstet CVassLymsfuoprroolc28h0e38mSOiLcVAaYl.s Signature: printed: AFRBtyeraosno,nMaPrFrrCciohEdcaNe2yTs,5RsMiE2anK0gra0cr3h.e32n80s,7(:2K10a30rA3enM9:R0i7s:h0a8)AM TDNiaamtmeees::220137276a1023780.033003 Description: XC031703:2, 80 ng. Standard PC-rhoinnaT s snes oniza) friao5 n pa ; Wt ta omngys: Ee w L sx 28088 148 79s ' T TTR T Te Th The Sh he ahh e Te rIr RRrTOReeTpR rRomR, i en Research, 3058 Research Dre, tae Colege, PA 16301, Dataaacequiredon LONSMSHT 000200 uUadnytNfoyLS3a4m3p0l0e,RDeaploartSet0326033 SOLVAY,ExtDate 03/26/03,Analyst isha Gsaeset x ACLWMasslyFnreiidauyo,rMoecrhcehmi28c,a2s0p0r3ol9d0372:600838AVSMOLVAY.qid RByeason PCrEoNcTesRsEiWnagrens (Karen Rishe) inlod: Friday, March 28, 2008 :07:13 AM taom:e:270-3M2a6r0-32B0-033004 me: 22:13:54 escription: XC031703-3, 100 ng/L Standard ~ 22063013786-3330.0140S0mmogothS(mMnna.n2xr3d) PaTFOeA Pagedol1s !i ;ii i i 1 ; MRMof 1 cahEmarneeen5l ! | la on gs The hah am ab kaem b--r-- ak1 wk T Sh R ew ek TR Thawmi `Ygen Research, 3058 Research Drive, Sate Collage, PA 16801, Data acquired on LMSMSH? 000201 rere pepe------------------ `SQauayntiNto.y1 3Sa4m5p0l0e,RDeaptoartSet0326035 SOLVAY, ExtDste:03126103, Analyst KRisha DoSataswewt e CAUiWasslFyrnirdiauy.orMochaemricl2ce0p0rh3o9l002372.650083A8,MSOLVAY qd : printed:___ BRFryeiadasyo,nMaCPrrcEohNcTe2sR6sE,iWn2ag0r0e3ns97(:K1a3rAeMn Risha) NDaatmee::270-3M2a6r0-3280:033005 TDiesmcer:ip2t2i:o3n0::4X3C031703-4, 250 nglL Standard PcSsFozO6r0Ai38a:,3085aSnmooklSiannd2ar)d o PiTroioes Page5 oi 19 !: Rot carsoasmiissain.d | ' Lo Tee Te he ik 4k 4k seE sk 8% |E8%Tr 7% TThe 800in Exygen Research, 3058 Research Drv, Sate College, PA 16801, Data acquired on LOMSMSHT 000202 GCQuaentySaLm3p5l0e,RaDpiorStoL0326098 SOLVAY, EXLORG032603, Anabyst sha DBotaseot RCay:WassLyndfroenr2c5c2h0e03mi0a7.l0p8ArSM0O3L2V6A0Y3iBd Prtod._ BRFyasosodn aP(CrEoyNs2Ts5aRe,E5s\M0gK0a3raen7rs.(1Kc9aArehnMRisha) TNDiaammteee::2702.24067051332810.033008 Deiplon XCO31703.5,508nl. Standard SpCprsaonE ncS SrooE nnzy (abiron TTT mea |i i] i | wert creistye:s " . ETT TI TI1 E TTR TR TTR he ke a apTee rm Exygen Research, 3058 Research Die tte Colege, PA 1880, Data sid on LCMSNSHT 000203 a QuantiNtey S3a4m3p0l0e,RDepaorSteL0326038 SOLVAY,ExtDate 03126103,Analyst Rishe PageTol1s DSatwaseet CABiyMassLyFmrdifClduaoEyrMoNchToerRrriEca(Klc2ea0.er0pher9ronlRe200i73ns2.sh60s0a83)A,8 MSOLVAY.qd Ported: RFreiadsayo.nMaPrrcohce2s8s,i2n0g03 3:07:19AM `DNaatem:e:270-3M2a6r0-3280-033007 TDiesmcer:i2p3t:io0n4::1X7CO3703-6, 1000ng Standard SPTEsF2OAeA0T30,3000m0 9o8sSc)ars = fesiirsotas nko enlsaimzeeln5: i ol Tyr nar I I I EEE creEpSema Exygon Research, 3055 Research Dive, Stale College, PA 18801, Data acquired an LCMSHSET 000204 santify Sample Report - dy No.1.34300, Data Set:0326038 SOLVAY,ExtDate:03/26/03, Analyst Risha Page 8 of 19 ! oBn i ws ! sy il "rw 51077 148 [| 190 2 43 401 ! Here | iy ol | 1en Research, 3058 Research Drive, State College, PA 16801, Data acquiredon LCMSMS#7 000205 ii iS tu No 3430R 0, Data Set0325038 SOLVAY, ExtDate 03/26/03, Anala yst Risha man || dJogtraset.ce ALCMasslFyrneViyo,rMochaemicral2sc0p0r3oh$0032726.003888ASMOLVAY qd By CENTREW(KaarreneRinshsa) : ; vinted: FRreiadsayo,nMaPrrcohce2s8,si2n0g03 907:19 AM |! altaem:e:270-3M2a6r0-3280-033009 i i J"eIsmcer:i2p3t:i3o7n::401105020 Control [i 3F126o0600n3280.C3o0n0o9rStn 26) - 1 . olf 19J0im gon 2Maza310 le RNG d2a3sm5e0leneg3s0.s | spa ass 538 aes pee oss 700 218 re 17o4 " TR TR he ak ve Rak i Sk Sk em ak 7h 14remay in +y9en Research, 3058 Research Dive, State College, PA 16801, Data acquired on LCMSMS#7 000206 SQuayriNfey S3a7m5p0le0TDopaoarSto0325038 SOLVAY,EDe026/03,Anast Risha DSattaasuerte, Printed CBiylMassLFynrxaCfyluE.orNMaacTheenRmi2Ec6a,(Kl2ks0.aa8pr3rreon9\oR00i3n7s2h06se08)3A8 SOLVAY gid. RFeraesyo.nMarPcrhov2e5s,ai2n0g03 97:18 AM TNDiaamtmeee:::227053:M62a46r:02z36o89010 Sescrpton; 0106020 Spk A, 50 nglL >SShF2oar3010 Sine) prionn fo 0 Fags 10018 i}i iI!i| I [EdmT eesms x "8 ou rr nar A aA TE CETTTR iR ake ake ake ak aw iE ER ek eh eh 7% TE ab . i| genReseach, 3058Research Dive, StasColege, PA 16501, DatsaconLiOMSMdSHT 000207 `QSutaundtyiNfoy.SLa34m5p0l0e,RDeaptoarStet0326038 SOLVAY,ExtDate:03/28103, Analyst Risha SDiagtnaasteurte: Printed: ABCLiyWasslymFCriEifdNuaTyo,RrEoMcKaharecrmhoin2c6sa,l(2sK0ap0rr3eonl90:i03s72h:6a008)38AMSOLVAY.cld FRreiadasyo,nMaPrrcohc2e8s,si2n0g03 8:07:19AM DNaatmee::280-3M2a6r0-3280-033011 DTeismcer:ip0t0i:o1n1::102106020 Spk B, 500 ngiL PS0i3Ot2e6oA0s3o83s0p1e1, Ssmocotnnbinzz) pSroen poy Ed FPagetiors ;| i! i ; enoMeu1l5m07te60s0s0.8 TTR TTR E| R TER TR Tk ak Wk em ek Ge 700 750 abi Exygen Research, 3058 Research Drive, Sate College, PA 16801, Data acauired on LCMSHS#7 000208 WJSQuEanStnifyESample -- eEReportcm eryinhdsi =iof-- nnEr ensnis,for 2... cob g -- s =T B=unEEor 52 1 1 Page 120f 19 HwEy 000209 QuSatundtyifNyo.SLa3m4p30l0e,RDeaptoartSet:0326038 SOLVAY,ExtDate:0326/03, AnalystK Risha SDaotnassteutr:e: Printed: ACLiMisssLFryindfalyo,rMoachrecmhi2c8a,l2s0p0r3ol9.00372.50083A8MSOLVAY.qld RByeason _CPErNocTeRssEiKhagrens (Keren Rishe) Friday, March 28, 2003 9.07:19AM DaNtaeme::280-3M2a6r0-3280-033013 TDiemsecr:i0p0t:i4o4n::4L734300-1 Rep, DF=100 0PR 3F2O60A3e 83013SSrohan 20) we To aan TTRT aemoris peels. rie Th 1k TE 2h 2% 360 3% AB 4% sl oo sL m 600 6s 780 750 | 40 Exygen Research, 2058 Research Dive, State Colege, PA 16801, Data acquiroend LCMSWIS#7 000210 `Guaniify SLam5p2le0RDepmorSt 250 SOLVEAxY, tetazeos, Aras DSaoasmate fGe aFsaytarr 2o00pn8rGS0Zo7S0083mSOLiVAYc44 inet: BFBydraasa(BeCrEeN3Tc5R,oE2Kn0ar0e8ns97(K1ar9en0Risha) oaem:Zata52)6ar0e2308038014 Despin:XCASYTOS.1, 25ng Standard S rSio"aataE n sE m. e fio)n "Page tol 19 rs tJpegEe pr os RS B 2 O L. SEE 63A 16.44 88A 1 ET E e T TRE TR TR Sorgen Ress, 205 Research re,SseClg, PA1851, Ds acqred on LOSS 000211 I --TE vay a J `Quantitfy San mple R2eportSucs2003 souvay, eat nz space SDhantaatsuerte: ABCLy:asCFsriEdtayNy, MTnarRdchEi26Ku,(G2oar0p0ertr5neo\e$R003i7cn2.n60hsa083)Ae8NSmOLiVcAYlisd Printed: FiRkedsasyo,nM_aPrcrhoc2e6s,t2i0g03 3:07:19an | DamDetnsece:risp2to8i.ronai:rs2X0G003317012, 50 ng. Standard EParnoiansors 20) ron - i ---- " Page 15 or 75 - Mot chums. alanis 2 rsr TEe T m TR STARnannak 1 a . ose Vogo A1h7ao ah RRTOR ER TTR Xygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000212 SQStuiuaS dnytiNtoy:SL3a4m3p0l0e,RDeap-- toartSet0325038 S-- OLVAY,ExtDale 0-- 3/2603, Analyst-- Risha -- Fae 180115 DSiaotnaasleutr:e: ACBLy:tfasCFsEiLdNyaTymR,rEMtWaharrocerhno2sc8(,hK2e0am0ri3ec5n.aR0ii7ssh0pa8)rAoSMlO0L3V2A5Y0q3l8d Printed: FRreialdasyo,nMearPcrohnc2e6s,sd i2n0g09w 9:07:1s 9AM TDNaiatrmee:::20801.:33a24r6:0520308033016 Description: XCO31703-3, 100ng.Standard PScrsEosRAS3,otsosmmeonnSgienr2a) - frionn Mot cpharme: 5 Jr J | [2 1 booTres ae ak ae ak ak eke ke TER oerR Po, TER TTr R TRt min a rn scm, venience 000213 | A ue SEN Quantify 0 SampleShReport a asnso sovvar exomessas oar TE rn ---------- Signature: Pinte AFB8toroyn,viSCFrriEdhagIyo,TiMaaEirenchn0287,c:2100a0309r:07s:08 AM DaDPeirsc:rip2ti3onXerCsUS12750tgi3S.ta4nda,rd 1 s TPironans soning "Tw = reining Page 17 of 19 hagawrcBa a 1 1 Lr : TT TE TT a r TE e Exygen Research, 3058 Research Driv, State College, PA 16601, Data acquired on LCMSMSHT 000214 | QStuuadnytiNfoy:LS3a4m3p0l0e,RDeaptoarStet0325038 SOLVAY,ExtDate:0312603, Analy--st isha DSantaatsuerte: AGBL:yMasslyFrnCiediEahyu,NoMrTaorcRchehEm2i6cK,(a2Ksa0apr0rre9onle9R0.i30ns27.h60s0a3)A8 SOLVAY.qd Printed: FRreiadasyo,nMarPcrohc2e6ss,i2n0g03 507-19AM DaNtaem:e2:60-3M2a6r0-3280-033018 TDiemscer:ip0t2i:o0n8::2X6CO31703-6, 500 nglL. Standard XP0-C2Fa6Oa0IA3T8G.33,1820S0nmgoo.nSgainn20d) Frion Ed "Page 180 18 MRM h2laSinaeeeosn.s wee TRIS ak ak aR he eee TT TTR | `gen Research, 3058 Research Drive, State College, PA 18801, Data acquired on LCMSMS#7 | i 1 000215 | SGGtuvuadnytiN-- toy-SSLaa3m4mp3lp00e,R-- eDaptoLaUr. tS4eY0F-- 3A2A603H8ASVOEL-- SVIAVYL,YExtDa-- te 03280h3-- i,dAnsyst-- Risa -- TT -- ---- --Pa-- g-- e Tao-- s SDaatausette. : ABCy:WaFCsrEiNdsaTyR.lEMWayracrmhon2f6s,o(3K0rpa0ro8elon0S073cRB2i5hs0)3eA5nSOiLVcAYagsia Printed: RFreiadasyo.nMaa rPcrohce28s,si2n0g03 37:19An NTaDiamtmeee:::2008243:022a55r:0132580.033019 Description: XCO39703., 1000 nglL Standard pA3ir2i1o0na3e03,18oSkomSsa) frionn Meters raRmsoss. EA Sani "| ECE IEI i : ra ores a PSR in 9en Research, 3058 Research Die, Sst College, PA 16301, Data acquired on LOMSMSHT 000216