Document NeRo8j1kJKn8y5gxOqx8BjgXE

3M Environmental Laboratory Final Report- Analytical Study Single-Dose Dermal Absorption/ToixnicRiatbybiSttsudy of T-6067, T-6068 and T-6069 +- In-Vivo Study Reference Number: HWI#6329-152 Study Number: AMDT-011095.1 Test Substance: L-13492 (T-6067, T-6068 and T-6069) Name and Address of Sponsor: 3M SCD Division S3t6. 7PGaurlo,vMe NStre5e5t106 Name and Address of Testing Facilit3yM: Environmental Technology & Services . S9t35PBauuls,hMANven5u5e106 AMMetDhTo-dM-N1u-m0b,ers TahnedrmRaevliEsxitornasc:tionofFluoride by Means of a Modified Dohrmann DX2000 Organic Halide Analyzer-Liver AMDT-M-2-0, Fluoride Measurement by Meansof an Orion EA940 Expandable Ton Analyzer AMDT-M-4-0, Extraction of Fluorochemicals from Rabbit Liver AMDT-M-5-0, Analysis of Rabbit Liver Extract for Fluorochemicals Using Electrospray Mass Spectrometry AMDT-M-8-0, Analysis of Fluoride Using the Skalar Segmented Flow Analyzer with Ton Selective Electrode AMDT-M-14-0, Thermal Extraction of Fluoride by Means of a Modified Dohrmann DX2000 Organic Halide Analyzer-Serum Initiation Date: See attached protocol Author: James D. Johnson roved (mes D. Jokngon tudy Direftr u/es/os Completion Date ald coeg i2 Wale L0 osumma0 ry 0000 Aliqtu-ibdutfyolrmaumlmatoinoinuwmassaaltppolfiepderdfelrumoarloloycttaonoraabtbeitisn. thLeivfeorrmsaomfpltreesatweedrfeabarniaclyazneddasa.t a 28 days post dose by combustion for total organic fluorine. The results from treated animals were the same as control values. practical quantitation limit. Serum levels All total organic were also below values were the practical below the quantitation 3 : limitsof the analysis for samples collected at day 1 and 2 after administration of the `mixture or the treated would be unlikely that fabric. From the pharmac any extent ofabsorption okinetic study (HWI#6329-151), could have been detected in this it study. | `This study was designed to provide information as to assess the systemic absorption and toxicity and when applied to relative the skin skin irritancy of rabbits. of L-13492 (T-6067, T-6068 and T-6069) In a pharmacokinetic study (HWI#6329-151), this compound showed little accumulation at 48 hours in liver. The biological half-life determined from serum levels in female rabbits was about 4 hours after an intravenous dose. A rabbit injected with 40 mg/kg died 5 disappearance, there is almost minutes after injection. no chance ofbeing able With to see this the rapid half-life of material after a dermal dose when the first sampling interval is 24 hours for serum and 28 days for lwiivlelr.beHsoowmeveearp,pieftarhaenrceeoifs tahseexmadtiefrfiearlenicne and absorption male rabbits. it is possible that there 3T 0 ESTMAT~ E~ RIALS 3.1 Test, Control, and Reference Substances and Matrices 3.1.1 Analytical Reference Substance: FC-95, lot 161 or 171. They are equivalent, 3s.e1r.u2mAnalytical Reference Matrix: Bovine liver, bovine serum and rabbit serum 3.1.3 Analytical Control Substance: None 3.1.4 Analytical Control Matrix: Bovine liver, bovine serum and rabbit 3.2 Source of Materials: 3M ICP/PCP Division for FC-95, bovine liver from grocery store, bovine serum from Sigma Chemical Company, rabbit serum from AMDT-110394.1 control animals SautoR 2 02550 3.3. Purity and Strength of Reference Substance: Responsibility ofSponsor. 3.4 Stability of Reference Substance: To be determined by Sponsor. 3.5 Storage Conditions for Test Materials: Room temperature for FC-95. For biological samples the storage is -20+10 C. : 3.6 Disposition GLP Regulation offorSptehecitmiemnesp:eriBioodlroegqiuciarletdisfsouresstaundidesflluoidnsgewriltlhabne retained 28 days. per 4.0 EXPERIMENTAL - Overview The tissues analysis for from animals dosed as fluorine compounds. Adtestchreidbiesdcr(eHtWiIo#n6o3f2t9h-e15S2tu)d,ywDeirreecatvoari,laabsleerifeosr of canoamlbyutsictailonteswtasscotuheldmobsetpelrikfeolrymaenda.lyTsihsetsocprreeesneinntg for fluoride in definitive data liver via for absorption if tlihveerp.haOrtmhaecrokaivanieltaibcletetsetst(siwnterraeveenloeucstraodsmpirnaiystmraastsiosnp)ewctarsopsocsoiptyivaendfografsluorine in the ocbhtraoimnaetdowgirtahphcyo/mmbaussstisopnecatnraolmyestirsy.alHonoew,eovnelry,itfhethlievedrefsianimtpilveesrewsouultlsdcboeuladnableyzed wanads adnetyecottahbelreteesvtesnwjouustldusbiengfomretcoenrfrieramdaitniogns.beAlnodw,tihfenporaocrtgiacanlicqufalnutoirtianteioinnclriemaiste of the would method, then further not be performed. analysisofliver for specific fluorinated compounds 5.0 EXPERIMENTAL - METHODS 5.1 AMDT-M-1-0, Dohrmann DX2000 Thermal Organic ExtractionofFluoride Halide Analyzer-Liver by Means of a Modified E5.x2paAnMdDaTbl-eM-Io2n-A0n,alFylzueorride Measurement by Means of an Orion EA940 5.3 AMDT-M-4-0, Extractionof Fluorochemicals from Rabbit Liver E5l.4ecAtrMoDsTp-raMy.-M5a-s0s,SApneacltyrsoimsetorfRyabbit Liver Extract for Fluorochemicals Using BH066Y. 3 O2852 5.5 AMDT-M-8-0, AnalysisofFluoride with Ion Selective Electrode Using the Skalar Segmented Flow Analyzer 5D.o6hArmMaDnTn-MD-X1240-000,OTrhgeanrimcalHaElxitdreacAtnioanlyozfeFrl-uSoerriudme by Means ofa Modified . 6~ .0 DATAANALYSIS ~~ 000 `The data are attached. There appears to `whole liver between the controls and the no 4, difference in 16, 40 mg/kg total organic groups. The fluorine in dose was dwiiftfherreenscpeecbtettowetheenTe-itnhuemrbfearbreidc ctoremaptomuenndt.anIdntahdedictoinotnr,oltsh.erTehaeppveaalrusestoarbeealnlobelow tmheeteprrarcetaidcialngl.imVietroyflqiutatlnetitottaatlioonrgaanndicthfelucoormipnaerwiassonosbsareervreedlaitnivseearnudmbaatse| danodn 2 sdaamypslpionsgt wdaossetoino eliatteh.erTshexe.maTtheerimaletihfopdredsiedntnowtouwlodrkhabveecabueseentchleeatriemdebienftoerrevatlhoef samples were collected. Other data was collected using electrospray mass spectrometry (see appendices). This data, although supportive, in the opinionofthe Study Director is not required to reach the conclusion stated here and therefore is not discussed in detail. 6.1 Circumstances that May Affect the Quality of the Data: The possible problem with this were collected to analysis measure is that dermal there is not absorption a good if it did marker occur. at the times samples No conclusion can be drawn from this data as to the extent of dermal absorption. 1.0 CONCLUSION. In this study, no conclusion can be drawn from this data as to the extentof dermal absorption. 8R .0 MA AINW TEND ANA CE OT F AANDRECORDS 8.1 Raw Data and Data: appropriate specimens, and Raw data, electronic approved protocol, approved data will be maintained in the final report, AMDT archives. enous 4 02652 90 APPENDICES ~~~ 9.1 Protocol and Amendments 0 9.1.1 Protocol and Final Report HWI#6329-152 "Single-Dose Dermal Absorption/Toxicity Study of T-6067, T-6068 and T-6069 in Rabbits" : (Protocol type TP3016.AB for dosing of animals, tissue collection, etc.) 9.1.2 Analytical protocol AMDT-011095.1 9.1.3 Amendment to analytical protocol AMDT-011095.1 9.2 Signed Reports from Individual Scientists: None 9.3 Quality Assurance Unit Statement: See attached 9.4 Key Personnel Involved in the Study: See attached 9.5 Materials and Equipment: See methods 9.6 Solutions, Reagents, and Standards: See methods 9.7 Sample Preparation: See methods 9.8 Quality Control Practices: See methods 9.9 Test Methods: See Protocol AMDT-011095.1 9.10 Instrument Settings: See methods 9.11 Data: See attached. 9.11.1 Summary and raw data; ug F" in whole liver as determined by thermal extraction followed by analysis using Orion ion analyzer. 9m.a1s1s.2sSpeucmtmroamreytrayn.d raw data; analysis ofliver extracts using electrospray [CJ] COR65% e9x.t1r1a.c3tiSounmfmoalrloyweadndbyraawnadlaytsai;s upspinmgFS'kianlasresreugmmaesntdeetdefrlmoiwneadnablyyztehrerwmiatlh ion selective electrode. 9.11.4 Summary and raw data; ppm F" in serum as determined by thermal extraction followed by analysis using Orion ion analyzer. Cum coe 9.1.1 Dose DPreortmoaclolAabsnodrpFitniaoln/RTeopxoirctitHyWSIt#u6d3yo29f-1T-56206"7S,inTgl-e6-068 and T-6069 in Rabbits" dosingofanimals, tissue (cPorlolteoctciooln,tyeptec.T) P-3016.AB for edCeORn656  WSO SN LAIN RS comm on nsor: CTE, St. Paul,LdMinnesota HiE 2\ : Ln a FINAL RepoRT tips Study Title: Single-Dose Dermal Absorption/Toxicity Study of T-6067, T-6068, and T-6069 in Rabbits Author: Steven M. Glaza Studs Completion ate: May 26, 1995 Performing Laboratory: WHa3ad3zi0ls1eotnKo,ninWsWimisascncoonnSssaiiunln,av5aI3rn7dc0.4 aboratory Protect Identification: WI 6329-152 Page 1 of 39 SUMR ALOE ELWS ERY 3301 wnsuan wise manisen wl dirs 3 ry 02656 Page 2 of 39 Wt 6329-152 QUALITY ASSURANCE STATEMENT = This report has been reviewed by the Quality Assurance Unit of Hazleton Wisconsin, Inc., in accordance with the Food and Drug Administration (FDA) Good Laboratory Practice Regulations, 21 CFR 58.35 (b) (6) (7). The following inspections were conducted and findings reported to the Study Director and management. Written status reports of inspections and findings are issued to Hazleton management monthly according to standard operating procedures. From "do __ pase sDiirbaetce tor Masseesent Inspection Dates Reported to Date to 11/28/94 12/08/94 02/20/95 05/24/95 05/25/95 11/28/94 12/08/94 02/22/95 05/24/95 05/25/95 Protocol Review Dose Preparation Data/Report Review Report Rereview Report Rereview 11/28/94 12/08/94 02/22/95 05/24/95 05/25/95 12/10/94 01/10/95 03/10/95 06/10/95 06/10/95 Cecilia M. Danner Representat{ve, Quality Assurance Unit 526-9005 0 Date BhbeEesy Page 3 of 39 HHI 6329-152 STUDY IDENTIFICATION . Single-Dose Dermal Absorption/Toxicity Study of T-6067, T-6068, and T-6069 in Study of Rabbits Test Materials Sponsor Sponsor"s Representative . Study Director Study Location Study Timetable SEtxupdeyrimIennittailati(oInn-lDiaftee) Start Date In-life End Date Experimental Termination Study Completion Date Date 1. T-6067 2. T-6068 3. T-6069 M Toxicology Service 3MMeCdeinctaerl, DeBlpdagr.tme2n2t0-2-02 P.0. Box 33220 St. Paul, MN 55133-3220 John M L. Butenhoff, PhD Toxicology Service Medical Department 3H Center, Bldg. 220-2-02 P.0. Box 33220 S(t6.12)Pau7l3,3-M1N962 55133-3220 Steven M. Glaza Hazleton Wisconsin, P.0. Box 7545 Inc. M(a6d08i)son2,41-WI729253707-7545 Hazleton Building Wisconsin, No. 3 Inc 3802 Packers Madison, WI Avenue 53704 December December 6, 8, 1994 1994 January 5, 1995 May 26, 1995 May 26, 1995 GUEOES C02658 Acute Toxicology SStteuvdeynDiM.recGtloazra Manager SFrtaundcyisCoo(rBduid)natW.orMcDonald PIant-rTiicfeiaSuPpaedrgvhiasmor RReopsoertM. SuBpreirdvgeisor Quality Assurance MSahneargreyr R. W. Petsel Page 4 of 39 KEY PERSONNEL HHL 6329-152 Laboratory Animal Medicine DCiipnldoymaJt.e,CarAyC,LAMDVM Supervisor Anatomical Pathology ATnhaotmoamsicEa.l PaPlamtehro,logPihsDt JDeabcokraSherfL.ortP/irkel NSuepcerrovpissyors, : SAnunpeervMiossohrer Pathology Data OHuL oRe59 Page 5 of 39 CoNTeNTs Quality Assurance Statement KSetyudyPerIsdoennnteilfication ORSbeujgmeumclatarityvoeryComp] iance Test and Control Materials PrToecstedSuyrsetsem ReDissuclutsssion SiRegfnearteunrcee Pathology Report Table : 1 Individual and Mean Body Weights (9) 2 Individual Clinical Signs 3 Individual Derma) Irritation Scores 4 Individual Pathology Comments Appendix A Protocol TP3016.AB HUI 6329-152 Page 2 i3 886 8 109 113 113 15 16 18 20 26 28 29 GhoesR 02550) Page of 39 HHI 6329-152 SUMMARY Tshkiisn sftrurdiytanwcays rabbits. doofneT-6t0o67a,sseTs-s606t8h,e asnydsteTn-i6c069abwshoernptaipopnl/itcoaxitcoitytheandokireelaotfive oTfhethsetudHrya:wa(sNZcW)oSnPdFuctsetdraiunsinfgorteharcehe mtarleeatmaenndttghrroeuep.female acclimated rabbits Group Test Material Do_s(eno/kLae)vel MNaulnebser--of AFneimmpaelss 1 (Con2trol) DisTt-il6l0e6d7water 3 T-6067 40 16 33 3 33 3 545 TT--66006687 T-6059 0 33 v 3 33 3 ba AAddmmiinniisstteerreedd (Fabric). aast aa d1o0s-ecn'vxolu1m0e-cnofpi2e.c0emLo/fkgt.est material orTfheestphebeacctkiravbeobfimtaesta.ecrhiaTrlhaebbaitttretawhteamseincntldiipcsiaptteeedsd fdrreoeemsaeionfleedvhealiirnwtaaacsntd.ada nTishnieingsltaeerreaeddosoefto aopftpheltihcesaktinion dwoarvseesrswcironavgpepreefddorwwiiatthh24S-aahrogauanruzeWexrbpaoapsn?udraaegnedpesErelicaousdrt.eodplwaistth tpaappeertotapperovairdoeundsnao1ccleudsgiesseand oCblsihneoirucvrasaltiaoofnbtsesreranvtdaetsittownioscrewcoeanrtderaoyclomnomdrauttceatrleiidatlyprecaddhmeoicsnkeissatwnredarteaitonc.oanpdpurcAotdxedidimtaidtoaenilsly]y 1,ctlhie2n.ri5ec,safltaenrd rf(aoarnydo2m81i),zdaatyasin.odnatBpuordipyno-sw1eeisfi,eghttbseefrwomerierneattideosenttero(rmDianyceodn2t9r)o.onl DTmahayete-r8iinaioltriaaDladyhdien-r7imsatflroartiirornitation tarhpeepardoDixaniygmwaIatserleyamdai3dn0eg).mbienfuotrSeeusbsteaeqsftuteenrotrbacrnoednaatdrgioenlgsrmemaootfveardliearlm(aDlaaydmi2ir)nriistantadtriaootnnionwDaeyr(sere4mcaodraendded8.ve Bilno-oldifesamipnlietsiatwieorne 4,8, 15, and 22. cI(noDalylaeddc1it),teidoanpf,prroomatxiamtamhateregltiyinnae2l4o-fheoaurnrescvreoipnpossytodfoonstehDea(yaDany3i9m.a2)l.s obnefDoaryes caeeupntpthrraonixifizumegadetdelatyandt2e0rsmaelipnaarotafitoebndloooidfntotwhaesseroiubnnt-a1iiafnnededpchefalrsloeumlaaernadchfnreaaccnrtioimpoalsn.is.ed.AlAlllThseaanmwipmhlaaellssewewroere wlfeirrvoeemr,calollblileaecn,tiemdaalnsa,fapnapenrcdorxoibpmosatyht.eki1dT-nhceenysbxlof1or-docnnsoasnmeepclteimsoanle(osfearndutmheanaendderfmceaemllalluealpapirnliecfaarctahicotingornossui)pt,e livers, Sponsor bile, after dernal application termination of the isint-e1si,fe anphdaskei.dneys were sent froren fo the cozest GHAI Page 7 of 39 HHI 6329-152 Application of T-6067, T-6068, and T-6031 did not result in any test mneactreorpisayl.-reAllaltedanicmhaalnsgesappienarbeoddyclwieniigchtallgyainnoromralmactrhorsocuogphiocut ftihnedinsgtsudya.t The produced control material did not produce any dermal irritation. Test material T-6067 Feactionsvery slight irritation in a fow of the animals at s11 shoes dove plreovdelusced(4,sli1g6,ht and to 4m0odemgr/aktge). erytBhoetmha faanbdricslitgehstt medaetmeariaalnsd,/orT-d60e6s8quaamnadtiTo-n6069, LL00tT CORGHR Page 8 of 39 HUT 6329-152 OBJECTIVE Trheelatoibvjeectsikivne oifrrtihtiasncystuofdytweasst mtaotearsisaelsss wthheen saypsptleimeidc ttooxtihceitys/kainbsoorFptriaopnnioarnd REGULATORY COMPLIANCE TALhdaimbsionriasstttourrdayytiSwoatnsu'dsiceosGn,odoudc21teLdCaFbRoirna58ta.ocrcyo"rAdPT1raanccpterioccweeidtuhRreegtsuhleautsUi.eSod.nsinFofotohdrisNaonndsctluDidrnyuigcsarle in cSpropemovpnilsoiouarsncaewnodrwkis.tthudythedirAencitnoarl, WethlefarsetuAdcytdiRdegunloattiuonnsn.ecessInaritlhye douppilniicoanteofansyhe Identification TEST AND CONTROL MATERIALS The test materials were identified dnd described as follows: dentification Physical Description T1--66006687 WChlieatre,'wecbolocrllotehss liquid T-6069 White web cloth cTohleorcloenstsro]liqmuaitde.rial was distilled water and was described as a clear, Purity and Stability dTtehhteeerScnopniotnnrasotolironmasastseu(rniienascllurwdeeisrnpegonscuionbndiseirldiettryeesdtfortcoontdbeiesttiaomdnaestq)eu.raitaelThfeoprurpiutthryeitypaundrapnodssteassbtiaolbfiitlyitthyis of study. Storage and Retention Tsfharemepelzteeerstofseatnedacthoconmttaerisotnltaaimnnadtecaronittaerlmosplerwaemtrauetreersitaoolfredw-a2s0atCtra+ko1eon0mCatnedmfoprewirla1lt0urybeee.arrseAtaiinrneesdervien a Aancycorudnaunsceed wtietsth in-1ife testing amHacatczeolrreidtaiolnngWwaitssocoHrHneIstiunSrOnPe(.dHMIt)AonySthteraenmdSaapirondnisnoOgrpecraoafntttiernroglcoPmmrapotlceeertdiiusor]ne v(iSOPv)ii je rfientaalinerdepofrotr. other testing and will not be discarded after issuance of ihe SLL 92563 Page 9 of 39 Safety precastions HWI 6329-152 Tahned ptoelsticiaensd control material handling procedures were according to HHI Sos Test Animal TEST Syste Adult albino rabbits of the Hra:(NZW)SPF strain were procured from Kalamazoo, MI, on November 16, 1994 and maintained at the Hazleton HRP, Inc., Wisconsin facility at 3802 Packers Avenue, Madison, Wisconsin. Housing DAufrtienrg reaccecilpitm,atitohne aanndimatlhsrowuegrheoutaccthleimastteuddy,forthea apneirmiaolds owferaet ilenadsitvid7uadalylsy. housed in screen-bottom stainless steel cages in controlled quarters. Environmental `controls for temperature- and humiditythe animal room were set to maintain a temperature of 19 to 23C, a relative humidity 12-hour Tight/12-hour dark lighting cycle. In cases where of 50% 20%, and variations from a these conditions existed, they were documented adverse effect on the study outcome. and considered to have had no Anima) Diet contaminants. Samples of the water are periodically anaivsed by mir there The animals were provided Laboratory Rabbit Diet HF access #5326, to water ad 1ibitum and a PHI Feeds, Inc. The feed measured amount is routinely of analyzed by the manufacturer for nutritional components and environmental were no known contaminants in the feed or water at levels interfered with or affected the results of the study. that would have Selection of Test Animals wpTerhroeegraanpmil.maaclesdThewientrroeandsiotdmueidnzytaitgfiriooenudpsbboyduysainwnimegailgahtsnsturmwabeterirefiaedndedtecbroomdriyrneewsdepioognnhdtinDagryaenad-8ro.mitzagaThteiaonnd wsbeotiduygdhytwediivgdahrtnisoattifoeornxceeoaefcdht+hg2erosauntpiamnadolafsrdeafcdoherviesaaextchiwoengrsreouopfnototfhestemaaectahinstswieecxiaglshletyl.ectsendd tfhonr tthoen the 5% probability level. different gt CcoResq BOLE; Page 10 of 39 HHI 6329-152 Study Qesian } Ainnitnoaltshewefioglhlionwgingfrosntud2y,3g7r7outpos:2,796 g at initiation of treatment were placed Group Test Material Do_s(ena/kLae)vel MNaulmebser of AFneimmsailess 1 (Con2trol) DisTt-il6l0e6d7water 4o 33 3 T-6067 16 3 33 3 645 TT--66006687 T-6069 fr) 33 v 3 33 3 a AAddmmiinniisstteerreedd aast aa material (fabric) d1o0s-ecnvoxlu1m0e-cnofse2c.t0iomnl/kogf. test Justification for Species Selection cHhiositcoericbaelclayu,setohef Ntehew ZleaargleandamWouhnitteofalbbiancokgrroaubnbditihnafsormbeaetniontheonantihmiasl spoefcies. PROCEDURES Preparation of Exposure Area TOohnbetatcihnelipdupaneybdlebnaeirfesoahreedmatdseeksitnup)m',ataeptrhpieraolxfilmaaanpktpselliycoaft2i0eoa%nc,hofrtahtebhebibtatcowtkaalsandcb,oldiypipfesdunrefcfaerceseesaroayfresh(.atior. Taihnreirmiattlaestsitownes,rieteoscrlid(peipfneetdcatcston tsDkhaiaynt)sw8owuelarndedpi2rn9escpletuocdteeadidthfeionrusvieinstouefarlfieazrniiynnggoftlhatesheioanpaspn.ilmiaclast.ionThe sites. Dose Administration AmaTterainailm.alsThreecedaiyvedofatrseiantgmleentadwmaisnisdtersaigtniaotnedofasthDeayres1pective test or control Go(rndoiuespatcihll1. eadnfiwnnaatlie'nrsd)ivbiwodadsuyalwaepipdglohisteed o(en2v.e0tnhlmeyl/dkatgyo) otwhfaesttreecsaattlmcesuniltta.etedatThaenadcroamntetearsouolrfedmatbearsieadl approximately 0.05 nl/cn'. ess Page 11 of 39 HWI 6329-152 LGraotuhpes 2C.ast3. Taintedr&.of Tthhee tGersotupsmat2,eri3a.l av(d1-6&06s7m)imewtass a(odrministeerredounndiialulted respectively) using the average bulk density of 1.04 g/mL to determine the dose volume for each dose level. An individual dose of the test material wtarseatcnaelnctu.lateTdhe foarreseacohf eaxnpimoaslurebasfeodr otnhe i4t,s b16o,dyanwdeig4h0tngo/nkgthdeosdeay loefvels Tanged From 0.001% 00k m/e was 9, 9, and 16 cm',respectively. The approximate rate of application Grreosuppescti5veandtes6.t sTihtee atsesta m1a0t-ecrmiaxl 10(-Tc-m606s8ectoironT-6o0f69m)atewraisalapptlhiatedwatso the moistened with distilled water. Each area of application was covered with a 10-cn x 10-cn gauze bandage secured with paper tape around all edges and overwrapped with Saran Wrap and rEelsatsrtaoipnlasthte taanpiemaltso dpurroivnigde tahne o2c4c-lhuosuirveexpdorseusrsiengp.erioCdo.llars were used to Approximately 24 hours after test or control material application, the restraining collars and bandages wert removed and the residual test material was removed with tap water and disposable paper towels. Reason ft oute of Administr: The derma route 15 a potential route of exposure in humans. Observations of Animals Clinical observations were conducted predose and at approximately 1, 2.5, and 4 hours after test or control material administration. Additional 1 inical observations and twice a day mortality checks (morning and afternoon) were conducted daily thereafter for 28 days. 5Body weights were determined for randomization purposes on Day -8 or Day -7, before test material administration (Day 1), and at in-life termination (Day Pinte after bandege vamoval (day 3) and on Bares went The initial dermal irritation reading yas made before test or control material raedamdiinnigs)t.ratiSounbseaqcuceonrtdinrgeadtiongtsheoDfradiezren'alteicrhrniitqauteion(rewceorredemdadaes atphperoDxaiyma1tely 30 cozssl Page 12 of 39 SBalmopodlesCaompllleescti(oanpsproximately 4 nL) were collected fron a marginal eHaIr v6e3i2n9-o1f52 . all animals before experimental initiation blood was conducted 24-hours postdose (Day (Day 1). 2), and Subsequent collection of on Days 4, 8, 15, and 22. In addition, was obtained at the time of necropsy from the posterior vena on Day 29, approximately 20 mL of cava of each animal. All samples blood were centrifuged and separated into serum were then stored in a freezer set to and cellular fractions. These samples maintain a temperature of -20C 10C until shipped to the Sponsor. Pathology At termination of the experimental phase (Day 29), animals were anesthetized with sodium pentobarbital, bled via the posterior vena cava, exsanguinated, and necropsied in random order. The sites of test and control material application were washed with lukewarm tap water before the necropsy procedure. All any animals were subjected to an abnormalities were recorded. abbreviated gross The whole liver, necropsy bile, an examination approximate and I-cm x 1-cm section of the dermal application site from all animals, and both kidneys pflraocmedtheon first dry icmea,l e thaennd pfleamcaelde iinn eaacfhreegzreorupswetereto cmoalilnetcatiend aandteimmpmeeradtiuarteelyof 20C 10C." After necropsy, the animals were discarded. Shipment of Blood. Bile. and Tissues After experimental termination, the blood samples (serum and cellular ffrroazcetnion(so)n, drlyiveircse,) btiolet,he dSerpmoanlsorapp(lJiacmaestioD.n Jsoihtnesso,n,and3MkiE.dEn.eys& wPe.Cr.e, seBnldtg. 2-3-09, 935 Bush for the retention Avenue, St. Paul, MN, 55106). The Sponsor is responsible and disposition of the samples. HNI does not accept any responsibility for the analysis nor are these results presented of in the tissue samples this report. collected in this study Statistical Analyses No statistical analyses were required by the protocol. 0cation of Raw Data, Records, and Fina) Report Trheetairnaewd daitna,therecaorrcdhsi,vesandofanFHIoriigninaaclcorsdiagnnceed wciocphy HoHfI thSeOP.final report will be cozesy Page 13 of 39 Body Weights RESULTS HHI 6329-152 ; wIenidgihvtidugaalinsandfrommeanDaybod1ytwoeiDsahyts29.are in Table 1. ATl animals exhibited body Clinical Observations tIhnrdoiuvgihdouuatl. cthleinisctauldy.signs are in Table 2. A1l animals appeared normal Dermal Irritation rpIernaodcdituviicodenudaslnoinddeerormnmaeallaniirinrrairltitaatttirioeonant.esdcoa"rTteesst4 ammrgae/tkeigrn,iaTlainbTle-t6wo03.67aniTpmhraeoldsuccoentdtrreoasltTeiqgmhattatereiraylthema dT1e6-s6qn0ug6/a8kmgaa,tnidoanTnd-6r0ei6an9c,ttiwoopnrsoa.dnuicmaeldssltirgehattedtoamtod4e0ramtge/kge.rythBeomtah afnadbrisc1igthetstedmeamtaeriaanlds, Patholoay TIensdiiovnidsuaolbsearnvimeadl inpaatnhyoloogfythceommaeninmtaslsa.re presented in Table 4. Page 15 contains a pathology report by the study pathologist. There were no DISCUSSION TTah-de6m0i6na8ic,sutteearnedsdysTat-s6e0m6ia9c swiaenbrgseloerepdvteairlonunaa/ltteodxaipcpilinitcmyaatlaienodna.nrdelAafptepimlvaeilceastakiilonbninioorfrriattbhaebnictytsheosfweheTn-6067, dmfeairtnmedarilinagsl`sirardtiitdnaetcnirooontpswryae.ssulotAbTsleirnvaenadinmyaalsesffaeacrptepsseualrotnedbofondorytmhaewleiagpthphtlriocugagatihinoountorothfmeatchrseotsudccyoo.nptircoN]o m1-a6t0e6r7i,al,andversyligshltightto T-6068 or 1-6063. miordreirtaatteionirwraistatsieoenn wians a sefeenw oinf tthhee aanniimmaallss ttrreesatteedd wwiitthh SIGNATURE SSttuedvyenDiW.recGtloazra Acute Toxicology Date Seq CTs Page 14 of 39 HHI 6329-152 REFERENCE I. Draize, J. H., "Acute Derma) Toxicity (Single Exposure)," In: Appraisal : oTofxitchietyS,afAestsyocoifatCihoenmicofalsFooidn (1959). FaonoddsD,rugDrOufgfsicainadlsCoosfmettihecsU.-s.D,ermppa.) 54-56 Page 15 of 39 HN 6329-152 PATHOLOGY REPORT . There were six rabbits (three males levels euthanized and necropsied at and the three females) termination of each from six dose the study. The test h material, dose level, day of animal are in the Individual death, and gross observations recorded for each Pathology Comments that follow this report. discarded. At necropsy, there were no visible lesions in any of the animals. bile, an approximate 1-cm x l-cm section of the dermal application The liver, site from all animals, and both kidneys from collected, frozen, and sent to the one male Sponsor. and one female in each group After necropsy, the animals were were P AAo C ze-- Pathologist (6329-152. 1hm) 020895 meReZ5 SHOU coz670 Page 16 of 39 HW1 6329-152 Table 1 vate Individual and Mean Body Weights (9) Fenale fi lpriimearl Radanecdoenomn- bay TT Mmienarl bRoamandesomn- bay % Group1 (Control) - Distilled water (0 mafia F52725 F52711 F52719 Mean 2,699 2,592 2,456 2,582 2,79 2,726 2,494 3,135 3,085 2,671 52721 F52806 Fs2727 2,463 2,524 2,639 2,672 2,964 2,542 Grown 2 - T-6067 (8 mask 2,651 2,621 2,13 2,664 2,963 3,086 3,103 3,051 F52718 F52723 F52713 Mean 2,380 2,482 2,602 2,488 2,450 2,778 2,521 2,795 3,181 2,980 F52715 F52809 F52738 2,363 2,498 2,489 2,585 2,985 2,450 Grows 3 + T6067 (16 naska 2,317 2,511 2,619 2,502 2,752 2,909 2,946 2,869 F52737 F52801 F52724 Mean 2,631 2,611 2,634 2,625 2,634 2,699 2,616 2,878 3,113 2,933 F52733 F52788 52720 2,543 2,575% 2,560 2,650 2,975 2,559 Group = T6087 (40 nasi 2,629 2,429 2,627 2,562 3,017 2,994 3,028 3,013 F52802 F52730 F52731 Mean 2,543 2,408 2,339 2,430 2,785 2,520 2,489 2,598 3,088 2,766 2,715 2,856 52714 F52734 Fs2774 2,523 2,557 2,364% 2,481 2,578 2,660 2,556 2,598 2,893 2,839 2,930 2,887 * Day -7 body weight omecnoed Page 17 of 33 HHI 6329-152 IndividualTabalned 1Me(aCnonBtoidnyueWde)ights (g) Tandoanle Tandonf:emale :3 Mer Animal DavE ization TDaIy E Anmiemmael baization Day z= Group 5 - T-6068 (10 cn x 10 cn Section F52729 F52803 Fs2712 2,431 2,442 2,631 2,545 2,59 2,645 2,893 2,920 2,886 F52716 F52787 Fs52728 2,652 2,494% 2,495 2,118 2,544 2,619 3,21 3,017 3,009 Mean 2,501 2,595 2,900 2,547 2,647 3,079 Group 6 - T-6069 (10 cn x 10 cn section F52736 F52717 F52735 2,681 2,405 2,570 2,745 2,538 2,606 2,99 3,025 2,875 F52739 F52732 F52726 2,442 2,417 2,591 2,480 2,525 2,768 2,957 2,930 3,110 Mean 2,552 2,630 2,965 2,503 2,591 2,999 * Day -7 body weight eCe0:267 Page 18 of 39 HHI 6329-152 IndividualTabClleini2cal Signs s 1 Se me oman B00 rls Male Female Group 1 (Control) - Distilled Water (0 ma/kq F52725 Appeared normal / v F52711 Appeared normal v v F52719 Appeared normal / v F52721 Appeared normal v v F52806 Appeared normal v v F52727 Appeared normal / v Group 2 -"T-6067 (4 ma/kq . Male F52718 Appeared normal v / F52723 Appeared normal v v F52713 Appeared normal v / Female F52715 Appeared normal / v F52809 Appeared normal v v F52738 Appeared normal v v Group 3 - T-6067 (16 ma/kg Male F52737 Appeared normal / v F52801 Appeared normal v v F52724 Appeared normal / v Female F52733 Appeared normal / / F52788 Appeared normal v / F52720 Appeared normal v v / Condition existed. ovovEy 02678 Page 19 of 39 HHI 6329-152 ndtosaual Content"elgns : Se hm wear 04 rel Group 4 - T-6067 (40 mg, L) Male F52802 Appeared normal v 7 F52730 Appeared normal 7 7 F52731 Appeared normal v/ Jv Female F52714 Appeared normal v 2 F52734 Appeared normal 7 7 F52774 Group 5 A= pTp-e6a0r6e8d-(n1o0rmacln x 10 cnJSection 7 Male F52729 Appeared normal 7 vs F52803 Appeared normal / 7 F52712 Appeared normal J 7 Female F52716 Appeared normal Jv 2 F52787 Appeared normal 7 7 Fs2728 Appeared normal Group 6 1-609 (10 cn x 10 cn2Section 7 Male F52736 Appeared normal v/ 7 F52717 Appeared normal v/ 7 Female F738 F52735 Appeared normal Aopesred normal 7 4 Forse Appeared normal 4 F226 Appeared normal 7 Condition existed. J ' ' . "ren. cozsg Page 20 of 39 Table 3 Individual Dermal Irritation Scores HWI 6329-152 . 3 Group 1 (Control) - Distilled Water (0 mg/kg) Dermal Reaction --tSatudylDayes I248 _emStut dy Ge ay s I 2% Animal No. Fs2725 Aninal No. Fs27 AEtErodyentnihsaema [Joo 000 000 000 Fissuring Desquamation Coriaceousness 0 0 0 0 o0 o0 00 o0o o00 0o0 0 0 o0 o0 0g0o [J4 00 0 0 0 Erythema EDAdteeosmnqaiuaanation FCoirsisaucreionugsness Erythema EAdteomnata Fissuring Desquamation Coriaceousness Animal No. F527] Animal No. F52806 0 0 0 0 0 000 000 000 0 0 0 0 0900 o00 gg0oo 0 0 00 00 o 0 o o0 0go J0 Anima No. 52719 9000 0 00 00 00 0 0 0 0 0 00 00 o0o Aninal Mo. F577 0 90 go 900 o0 o0 0 0 0 0 [ 00 o0 g0o J0 7% * Page 21 of 39 Table 3 (Continued) I 6329-152 Group Individual 2 - T6067 (4 mark) Dermal Irritation Scores 4 Sbaotesh StoFensltesy Dermal Reaction ITf.nina2 l vo._4 rs27188 1fniea2 l o._a rs273 15 Erythens 000 01oo Edema Atonia 0 0 0 0 0 0 0 0 0 0 [J 0 0 0 0 0 DeCosrqiuaacmeaotuisonness 00 00 00 o 0 o0 05 00 00 Fissuring 0 0 0 [1 0 0 0 0 nim) to. es2r23 fnima to. pszan Erythema cortaceousness Edema Atonia Desquamation Fissuring 0 0 0 0 0 I] [J 0 0 0 0 0 [ 0 0 8 0 0 0 0 I [3 0 0 5 5 J 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 [ 0 0 nie to, gsz713 minal to_rs2738 KJ Eoryntihaema DecFsoirqrtuaaicmneaogtuisonness oo0 ooo0 a00 o00o 0o0 o500 000 0 oo 0o5 o50 000 0002 508050 0oSsO0 GOcOoNz6S76 Page 22 of 39 HAL 6329-152 Group 3 - T-6067 (16 ng/kg) Table 3 (Continued) Individual Dermal Irritation Scores s Dermal Reaction EEdreymthaena Atonia FDCeiossrqsluuaarcmieanotguisonness StuMdaylesDav IT 2 4 & Animal No, 52737 o 01 00 00 0 0 0 0 00 000 000 oo0o StFuedmyalebsay I24 Anima) No. F52733 00 oo aoo 00 0 0 0 0 000 o00 go0o oo[oJ Animal No. 5280 Animal No. F52788 Erythema ADEetdsaeqnmauiaanation FCiosrsiuarcienogusness 0 0 0 0 0 000 000 000 0 00 00 00 0 0 0 [ 000 0o0 000 o00o 00 o0 00 00 Animal No. F5272 Aninal No. 52720 EEAdrtyeatnnhsieama CDoersiqaucaenoautsinoenss Fissuring 0 001 0 000 0 000 [J00 oo 0o00 o00 o o00o 0 00 00 0o 00 0oo o0 o VHOaRY. coe Page 23 of 39 HI 6329-152 Table 3 (Continued) Individual Dermal Irritation Scores Group 4 - T-6067 (40 mak) : UermalReaction Erythema AEtdoenmiaa DCeosrqiuaacmeaotuisonness Fissuring TT StMuadlyesDay 24 Amina) No. 52802 1 00 0 00 00 00 00 00 00 00 0 J 0 J I aStFuedmyald eGsay E Anina) No. Fs2710 09o []0 00 o0 0 00 0o 0go o0o 0 0 0 0 Erythema Edema ADteosnqiuaanation CFoirsisaucreionugsness Aninal No. 52730 0 0 0 0 0 0 [ 0 0 00 00 o0o 0 00 00 [Jo Anima No. 52736 0 0 0 0 0 0 0 [J 00 00 0o gq0 00 0o 00 0 AtEEodreynmtiahaema DeCosrqiuaacmeaotuisonness Fissuring Anima) No. 5273 0 000 000 000 00 00 00 00 0 0 0 [J Animal Mo. F52770 000 0o1 o00 0 00 00 o0g [J 0 0 0 0 TTR 02578 Page 24 of 39 HI 6329-152 Table 3 (Continued) Individual Dermal Irritation Scores : Group 5 - T-6068 (10 cm x 10 cm Section) Dermal Reaction Erythema Edema Atonia Desquamation Fissuring Coriaceousness TT 2--rMarle4srr-- 8 Aninal No. 52729 0 1 1 1 0 00 00 00 0 I 0 1 0 00 [0 00 I A StFuedmyalebsaE y Aninal No. 52716 0 0 0 0 00 o0 o0 [4 0 0 0 0 00 0o o0 04 Animal No. 52803 Ania) No. 52787 Erythema AEtdoenmiaa Desquamation Coriaceousness Fissuring 0 9 0 0 1 0 0 0 0 0 I 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 9 0 1 1 0 0 0 0 0 0 [3 0 0 0 0 0 0 0 0 [J 0 EErdyetnhaens AtDCoeorsniqiauacaenoautsinoenss Fissuring Animal No. o 01 00 000 0 0 F52712 01 00 000 [Jo0 0 0 Animal No. 00 o1 00oo 0o0 0 0 F52728 o2 0o0 0 0 0 Gi, cozepg Page 25 of 39 HH 632-152 Table 3 (Continued) Individual Dermal Irritation Scores 4 Group 6 - T-6069 (10 cm x 10 cm Section) Dermal Reaction AtEEodrenymttahaema DeCosrqiuaacmeaotuisonness Fissuring StuMdaylesDav 1248 Animal No. F52736 St Fema],oas r I24& fnima) No, P2730 0 001 002 o 01 o00 011 o21 o31o 00 00 00 01 00 00 0o 1 0 0 [1 0 0 [J 0 0 Erythema AEtdoenmata Desquamation CFoirsisaucreionugsness Animal No. F52717 Animal No, F52732 0 1 1 0 0 0 0 0 0 0 oo oo 0 0 0 0 0 0 0 0 95 0 0 0 0 0 0 0 1 1 0 0 1 1 0 0 0 0 0 0 0 0 0 Erythema Edema Atonia DFCeoisrsqisuauacrmeiaontugsinoenss Animal No. F52735 0 1 2 1 0 1 1 0 0 0 0 0 0 00 00 o0 0 0 0 1 Animal No. 0 1 0 0 0 0 090 000 F52726 2 1 1 0 0 0 ag0oo o41b Ld COR6S0 Page 26 of 39 Table Individual Pathology Comments AMnaimmbaelr Sex DS ied TM est D: F Necropsy Observation Group1 (Control) - Distilled Water (0 ng/ke eos ow. 2 Wo visible lesions. F52711 " - 29 No visible lesions. saa F52719 M - fo - 29 No visible lesions. 2 Mo visible Tesions F52806 F - 29 No visible lesions. F52727 F - 29 No visible lesions. Group 2 = T-6087 (8 na/ka F52718 M - 29 No visible lesions. F52723 M - 29 No visible lesions. F52713 M - ans fo 29 No visible lesions. 2 No visible lesions. F52809 F - 29 No visible lesions. F52738 F - 29 No visible lesions. Group 3 - T-6087 (16 navi F52737 M - 29 No visible lesions F52801 M - 29 No visible lesions. F52724 M - 29 No visible lesions. F52733 F - 29 No visible lesions. af 52788 F - 29 No visible lesions. 2 No visible lesions - Not applicable. HWI 6329-152 3 . TOcNoE26S5 Page 27 of 39 HWI 6329-152 Individual Fatnetony Comments : AMneimmbae)r Sex Died JestSacDraiyficed Necropsy Observation Group 4 - T-6067 (40 ma/ka F52802 M - F730 ow - 29 No visible lesions. 2 No visible lesions. F52731 M - 29 No visible lesions. F52714 F - 29 No visible lesions. F52734 F - 29 No visible lesions. F52774 F - 29 No visible lesions. Group 5 - T-6068-(10 cn x 10 cn Section F52729 M - 29 No visible lesions. F52803 M - 29 No visible lesions. Fs2712 M - 29 No visible lesions. F52716 F - 29 No visible lesions. Fs2787 F - 29 No visible lesions. F52728 - 29 No visible lesions. F52736 M - F52717 M - Fs273s om . F52739 F + F52732 F - fare oF . - Not. applicable. 29 No visible lesions. 29 No visible lesions. 2 Wo visible lesions. 29 No visible lesions. 29 No visible lesions. 29 No visible lesions. oHeeEr' oz652 Page 28 of 39 APPENDIX A Protocol TP3016.A8 HHT 6329-152 CTI Co263%  WISCONSIN Page 29 of 39 Sponsor: st. paul,TMHimesota PROTOCOL TP3016.A8 Study Title: SingleT-SD6o06s7e, DeTr6m0a8l8A,bs`oanrdpt1i.6o0n69T.oxiinciRtaybbiSttsudy of `Date: December 5, 1954 Perforaing Laboratory: MHa3ad3zi0ls1eotnoK,ninWsWimisascncoonnBssoiiunnl,ev$aI3rn7dc0.4 aboratory Project Identification: WI 6329-152 ) : cozesp Page 30 of 39 } TP3016.A8 Page 2 STUDY IDENTIFICATION ; SingleT--6D0o6s7e, DeTr-m6a0l68,AbsanodrpTt-i6o0n6/9ToxiniciRatbybiSttsudy of HI No. 6329-152 Test Materials 210. TT--66006678 30 T6089 Sponsor Tnoxicology Services S2t0.-2P6a-u0l,2 3MNH C5e5n1t4e4r Sponsors Representative BEJon L. Butenhof, pho ) T2o0x-i2c6o-l0o2gy3MSeCrevincteesr St. Paul, WN 55144 (62) 733-1962, Study Director SHtaezvleentonM.WiGslcaoznasin, Inc. MPa.0d.isoBno,x W7I54553707-7545 (608) 241-7292 Study Location HBauzilledtionng NWoi.sco3nsin, Inc. 3Ma8d0i2soPna,ckWeIrs A5v3e7n0u4e PrEoxppoesreidmeSnttuadly STtiamrettaDbaltee Experinental Ternination Date JDaencueanrbeyr5,8, 19199394 Draft Report Date February 16, 1995 ) CoR63s oTOeSY Page 31 of 39 i TP3016.48 1. sStiundgyle-Dose Dermal Absorption/Toxicity Study in Rabbits Page 3 : 2. Tpfourrrpiatosassneecsys otfhetessytstmenaitceriaablssorwpthieonnapapndlietdoxitoc.itthyearnudinreultatiivcey tskIin 3. SLTehaaibusolraaStttoourrdyyyCPwoirmlaphcltiibaceneRcceeongduulcatteidonisn SatcacnodradnaenscyeGuwsitsoht trhces.following Good {1 Conduct as 2 Honregulated Study ['(] X] 4201 CCFFRR 51860 (F(DAP)A-F17Ra) [] 40 CFR 792 (EPA-TSCA) {[1] 155(81N)oh3s0an(FNion.al)385(0OEC(Do)mpanese MAFF) [1 Notification No. 313 (Japanese MOHW) wdAWoieIrrlkef.captrroeorc,Aecdtu`trheResegsutilunadtytihodinosss:sprontoIotncoutlhmeeacorkepsisniainroincloymopfdluiiphae)n.ctesespwtaeimtchoornytmhamedeAsniigtacsy)] ) 4. QualityAssurance The the Qpuraoltoictoyl,AsssutruadnycecoUnndiutct,in aandccotrhdeanfcienalwitrhepoHratzlweitloln be audited Wisconsin by 5. (HW1) Standard Operating Test Materials Procedures (SOPs) and policies. A. l21dentGTiefEeicsation 5 Te 8 P1hy1sicaal 2. (To beDedsoccruimpetnitoend be documented iinn tthhee rroawn ddaattea)) 5 (To ba documented in the raw dara) C. Purity and Stabivity TdheeteSrpionnastoironasssu(miensclurdeisnpgonsuinbdielrittyastfosronpdurrtitaynean)d stability Tesh Page 32 of 39 | 0. SRotoonragteemperature TPa9g3e0146.8 : . RemRaestseeerrrivvaeelSssuamWmpipllllees(sb)e otafkeenachforbattchhis/losttudoyf. test and control HfT1H0ohIreyei1ta0ner'ssyateafafronrsrdeedpzcieeosrnrptorHsosAelIittiSmtoOaonPt.emraiinianTlahteacicrnoSerpsdoeaanrnsvtcoeerempswweaiirmltaplhtluersbteehewicolofslnptp-arb5cee0tp-ersditasotraryofectdeorat regulatory Good Laboratory Practices. F. ARneytenutnuisoend completion toefstthematienr-i1ailfse wpihlalse beofrtehteurnsetuddyt.o the Sponsor after G. SAsaferteyquiprreedcaubytiHoHnIs SOPs and policies 6. Control Material . \ A. IDidsetnitlilfeidcawtaitoenr 8. PhCylesairc,alcDoleosrclreispstiToinquid C. TcPhoensuipduerarrinetddyiStatonadtbbiesltyiaatdbyeiqluiattyeofforthitshemapnuurfpoascetsureodf mtahtiserisatludyi.s 0. StRooornagteeCmpoenrdaittuiroens E. RSeeseerSveecStaiomnpl5e.s. Reserve Samples f. AaRnneydt:enwritelimloaninnoitngbecondtirsoclardmeadteraifatlermaiyssbueancuesedoffotrheotfhienra treesptoirnkg. 6. SaAsferteyqupirreecdaubtyioHnHIs SOPs and policies J Cozssy VOY Page 33 of 39 . 7. Experiments]Desian A. Aina TPa0g3e0165.48 ; (1) sRpaecbiies (2) HiSrtar:ai(oNIsMs)oSuPrFc/eHRP, Inc. ) Afodearat Initiation (4) M2e0ta0ht3.at0 Ikngitiation (5) Number and Sex 18 males and 18 females (6) IInddeinvtiidfuiaclatniuonmbered ear tag (7) Husbandry ) (2) HI(ohnuedsaivivynigdugaalulgye,} in screen-botton stainless steel cages (b) FA(oPHmoIedasFueerdesd, arIonuc.n)t. the manufacturer f ofThLeabofrooadtor1y3 ornutri tional RraobubtiitnelDyietanaHlFys#e5d32 components any 6s y environmental contaminants. ( ater wAadteTribairteunanfarloymzeadn bayutHoMmIatifcor sytosttaelm. disSsaomjpvleeds osofl tdhee, ohfroagrradnnSoeesplshe,ocstgeahdnadteelSsep,neecnaitnfsdi,edchhlmeoiarcvirynoabntieoeldaogthiycdarlocacrobnotnesn.t and (@) CTthhoaentrteawmoaiurnleadntnosinktneorwfnerecownittahnintahnitssstiundyt.he food or water (e) EEsenntvviirtrooonmmmeaennitntatlainconatrtoelmsperfaotrurteheofani1m9alC trooom23w0i.ll abe ) rVeilgahtti/v1e2-hhouumriddiatrykocfyc5l0e%.+20%, and a 12-hour mac) COR55g Page 34 of 39 * T3016. Page 6 (f) AAtcclTiemasattio7ndays ; (8) SnaBoeadlseeeaqncduitamitoaoenlnnhueoinsafbletoTrhbevstioaofnudAsenlxibytmordaayplosoawrneiimghaehaltlstahcic1oi1srdipbenlgacpeutdrochoHnaVIsetdeSsOtPv.sa.thaArn t dasantyirsmaatliosffiewsditluldbyodbyeInwpiteliiaagctheitdonri.anntodomsitzuadtyiognroupprsogruasminwgisahin os nine (9) HisJtusotriifciaclatliyo,n the aninal of cfthhoeoricNSeepwebceiZceeasauTsaSenedloefcWhtiittoheen Jaalrbgienoamroaubnbtitofhas been background information on this species. 8. DoAsdmeinistration (1) Test Grows Grow Test Materia){Dosemo/lkeav)el MNalues mofbAEneiemmsairless ) 1 (Control) Distilled water or 3 3 32 T1-.66006677 164 33 33 545 T-T16-60600666897 -4-0 333 333 **+ TToo bbee aaddnmiinniisstteerreedd material (fabric) aast aa d1o0s.e0-cvaoluxne10o.f0-c2h.0paislc/ekgof test (2) OPinfr'etnpheaecreasdtsaiaoyrnyboeff(otorEexopbtotesasuitrnemaAutrneebralieanlishaepdplisckaitn)i,on,thetheflbanakcsk aonFd, celaicphperra.bbitThewilslhavbeed calriepapedwilflreeconosftihtauitre waiptphroaxniemlaetcetlryic O2I(f0ir%nrttihatoecafttiatonhsinekm,iantl)oso.rtawlidlelfTbehocebdteysanisitnumhsraapflteasccwtewoeiudallrledfao.bprereiccTnllhtuieepdrpefteerdretiahentusgmeunnslteeeessdioieoftdnesa,sny throughout the study 2 SrC0iz,6gq Page 35 of 39 3Pa0g1e67.88 (3) WDArIeoITssLpeeacAnbteiddimmvaieelnssistiwtegisrnltaaltteiodrornec3c5oeniDtvraeoyla1.msaitneTgrhlieealra.edsnpieTnchitesitvdreaaytdiooosnfetofrertrheeent : 9Taah1nnetiiommaaGllrt'sohsuepinbaro1,edGayr2ouwo,pef3si,gehx1tap,no2dSj,uurs4et3,mabitneiefnroadirae4tlhswiaind1wmi1iatnn)dibesturnbaiatfsioeornnmsea1sansdtehsreca'rpreoandt mu3{onGidr1iso0ltu.upe0tsn-eecddn1.-'6xw)it"1hwT0hi.eld0li-Gscrtnboeiulpplcieoe5dceawnaodtfert.mheaterTerhseipaelacsrteiawvbieelo.lfsatobeprestp.tilessaieieptclieiriesodas]as bandage secured with papveerredfawpeitharoaun1d0-3c1n1 xed1g0ecsnaccyoure pcorovolevlriawdrreeadppanedduroiwcnicgtlhustihSevaera2nd4r-ehWsorsauiprngs.panpdiTchEeal.tarisaotnnogpilpatesatrawi.tlahpepeto (4) BThuhemeaasnodsne.rmfaolr Rroouuttee o1f5 aAdpaottneinsttiraaltiornoute of exposure in ) (5) AatRhppeeppmlroivorcaxelasiotimidafuotanellTyetshttee2s4Mtbahatmoneaudrtraiesgarelisaaflatnewdrilctloelsltbaerosrremcwioolnvlterdobleusimrnaegtreorevieadl and an appropriate solvent, If necessary. se or C. ObservoaftAniimoalns (1) CaaFldpoinprnirinoccixlasiiltmnraiactOateblilsoyenrsvi1,agantnsid2.o5nbf,seofraonrcdelin&tiecshatolurosrSicgaonfnstterraonldtemsmtoartmtearatileairltiyasat dsaaitidromneiTscen,tiiessdttanrbda2y8titdoetahniyecse{.s0tdauaydOiybl1sy)deir(`rvaanea.dctm.tidooanriaslndynaptyhoembr)yeaaffxtovreermnodfuvosrilaofaiictn)yteSolr (2) dDBReaeryfnoare IlereToiaa erfdsritiDntegd aortrmi(aocAlnoi tntItrarrecroahnildmtieannmtgtagtiewo1ri)nl.ilalAbdeaddimmtaiidnoeinssta]nrdadtirooepnceoyrtdheed inniitiiah]e aIfionfrrdtrieivretiaadctbuhiaaonlnadnaigdrmeeearalmdraeilmnogvsiarlwriilt(laDtaiyboen2n)ardeaecnodradopsnprwoSixtliu)mdyabtaeDlayaysei1n04temmrincneuyts-es (3) Body weights ) Jo1nuasatDya)ybe2f9o,reantdestat orunscconhterdoulledmatdeeraitahl (wahpepnlicsuartviiovnal(Deaxyco1n),ds FCO0O2T69 Page 36 of 39 TFirgeo'se. (4) sampleCollections t (a) EBreefqorueenciynitiation (0ay 1), spproxisately 24 hours Speopsetr-idmoesneta(lDayter2)m,inaDtayison4,(o8y, 1155), 22, and at (5) Nbuinber of animals () MB2fl,ero7tao3hnd,o.'dt5h<,eaonfa1pa8lC.reogslil%nae(nscds]tp2ip8osr:naarxtMvmoespitrneolxyoife4setm1eLit)nyerwi2lbelarpLbeonntcpoblullroeocedtred (ictial "volume to bs documented Inthe rou saat aint CbnSSeoaainmctpromrlibeftfsiaucisgenwaeiedcd1dr,]aitffiabrectonehmddeSttthothierineendespeonposooafttrreairnrtbieeoo.ocnnrrdasepveveecaeynopnan.ed(r;nDcaeaidtyvouancc3eeo0lfo)friunepdaaTcrhheen \ CFF2irr0apacectCrtitiono+nen1sns0.taCwsl.itloltrTeehbrdeemiinsnsaeetnpa'itaorfnafr,traeoedtseennsertsueesr.thstenodmSsapeioctneissoairlearrte Samples will be shipped to: JWSlaamEge:sE03.-3a6Jr7o6he5nson $SE35P0au5l, FWyienueSs108 Janes 0. Jonson or alternate will be notified by ttheelepShaomnmeieat (612) 778-5294 prior to the shipment of 0. Patholoay (1) UnAROnsrycihbaeundniumgladecdoSnddyaiicntrgiiofndiucrieiTns]ganbhdeeDesSuabtliheyscteodr ssoa.crunifaipcehdeeriinataed tgPahernecoeossrsmtdaherendgte:iicnzraeoldpnstywcaiaatrelhxsvaemsiiionnnd)a.iatuioobnlpreednabtnuovdnbidaaarlblctihotenaadblinetorinr(o,monafaslawivitiaiin}sejsecbcwnotisiloln be in cSxrsiaenagrudienda:ted: After fecrapsy, the animals rai ) SHOR 02697 Page 37 of 39 TPaeg3e0'1s6.4 () ASsEucrhveTidevirinmneigdnatasinaoicnmrailcosifceWtIhTe) exbep.erainmeesntthaeltizpehdasewit(h0aySos29i)s,h : bbpSaeeleoenbndrtreeoeccbvvroaiiorrsapdbtseieitdtdeh:adel.grvaei(snnvsairanacenaivcdnaorj,niepcoeetryxidsoeanenrxgaiumaniinndntaahttaeeil]domn,a.srbg3rinondTrahelesaulssepaaerirceetevseredsiwniw)1i,i]l]an (@) Simple collection wnSTehhicpe)rroospxbisietynesaStpaersoohfce1ed-tdceuawsritetx.han1dT-Tcuhmkceoonwswteahrcrootnllieotnmop|aotIaFevretrite:ahrle bdipaetepreiph.olari)acnatotiotnhe aFrpopnlictahteiofnirsstitemifcromandallfeanniilmealnse,croapnsdiebgothikn'idsoncekys Agffrrtoeeuerpzerwnielcslreotpbsetyo,cmoaltilhenetcataienndimaaalnsdteWmiipmTemTreadtbieuartede1lcyocfaprl3da0ecde.d 4i1n0aC. The issues. (1iver, bile, dorsal application site, wSkpiiodnnesyobser)aSwhfiitlpelpredbeextpoesreintmtheenftprseo]rzseontneromnTi1ndsartteyidoinc1.e3 SteoTchtetihoesnamples ) F7.eCt.e(n4t)i.o(nc)a.nd dThiespoSspiotnisoonr oifs trheespsoanmspilbelse. for the E. StNaot'SitsattiicstailcAanlalaynsaelysses are required. 6 Report A final report including those items listed below will be submitted. DDDPareetossecccserrdiiouppfrtteiiseooxnnpeoorffinttehhneetattleessttinaSintydisattecimoonntroalnd matteerrmiianlatsion DTGTraeaobsbsucuslrlaiatpptitaioiotnonhnolooofofgfymmeoaarnFntyianbldtoiiodtnxyygicsw/deaaeirtfgeafhsetscbstypsa/bsdtyeehxresmleaaaxnlcdyadnisdoresrpdeiootrsalseteiveoelnvel J) ToC0T690, Page 38 of 39 ' PTaPg3e0161.0A8 9. OfrLaioccgiailtniiatolantedoaftaauR,daiwtoirDnatgcao,ptiheeRsecsottruhddesyr.edofu3,rnidnwgiFlinliatlsbepRraeovpgaorrreltsasbleandatbeWfAIoreto : aralecltcaeiponrteiadgnicneianlotfhpeatpheearrcfhdiinaatvlae,s roeifpnocrHltHu.Idinagchceotnrhdoistnehge itftoienmaH)H1IirstSeoeppdo.rtbelioswcwoimlplletbeed, PDroosteocporlepaarnadtipornotorceoclordasmendments InB-oTdiyfeweriegchotrdss DObosseervaadtmiionnisstration ASnaamtpolneiccaolllepcattihoonlogryecorredcsords SSthuidpypicnogrrreescpoornddsence Final report (original signed copy) Tnohte. bfeolalrocwhiinvgedsuwpiptohrtithneg rsetcuodrydsdatwai.ll be retained at Hl but will ) AWnaitmearlanraelcyesipits/arceccloirndastion records ARneifmrai)gerraotoomrtaenmdperfarteuerzeerantdempheurmaitduirtay rreaccoorrddss Instrument calibration and maintenance records oUoows 02693 Page 39 of 39 : TPaPg3e01161.8 PROTOCOL APPROVAL oSphonnsTa_rPusthReeenphnroe?sfe,ntRaPthiiovte sudlaf 3H SSteuvdeynDiW.recTthoarza Acute Toxicolosy . Hazleton Wisconsin, Inc. Tefssen. tstive Quality Assurance RTE Hazleton Wisconsin, Inc. (6329-152.protdskl) w1e2-12-44 ote lo AY mate safe fod ouCe0e6es94 9.1.2 Analytical protocol AMDT-011095.1 BHOBTE Co269 3M Environmental Laboratory Protocol - Analytical Study Single-Dose Dermal Absorption/Toxicity Study in Rabbits of T-6067, T-6068 and T-6069 : In-Vivo Study Reference Number: HWI#6329-152 Study Number: Test Substance: AMDT-011095.1 L-13492 (T-6067, T-6068 and T-6069) Name and Address of Sponsor: 3M SCD Division 367 Grove Street St. Paul, MN 55106 Name and Address of Testing Facility: 3M Environmental Technology and Services 935 Bush Avenue St. Paul, MN 55106 Proposed Proposed Initiation Date: July 25, 1995 Completion Date: August 25, 1995 Method Numbers and Revisions: AMDT-M-1-0, DTohehrrmmaalnnExtDrXa2ct0i0o0n oOfrgFalnuoircidHealbiydeMAenaanlsyzoefr-aLMiovdeirfied AMDT-M-2-0, Fluoride Measurement Ion Analyzer by Meansof an Orion EA940 Expandable AMDT-M~4-0, AMDT-M-5-0, AExntarlaycstiisonofoRfaFblbuiotroLcihveemriEcxatlrsacftrfoomr Rabbit Liver Fluorochemicals Using AMDT-M-8-0, Electrospray Mass Spectrometry Analysis of Fluoride Using the Skalar Segmented Flow Analyzer AMDT-M-14-0, with Ton Thermal Selective Electrode ExtractionofFluoride by Meansof a Modified Dohrmann DX2000 Organic Halide Analyzer-Serum Author: James D. Johnson rovedBY: ames D. Johrison Study Difector Ais Date Plo 2 Bball fbf John Butenhoff, PhD Date Sponsor Representative 1 "H0O2T6S96 10PURPOSE 000 `This study is designed to provide information as to whether L-13492 (T-6067, T-6068 and T-6069) is dermally absorbed. The analytical aspectofthis study is to determine total organic fluorine in the tissue and serum of rabbits at various times post dose dermal application of L-13492. : 2.0 TEST MATERIALS 2.1 Test, Control, and Reference Substances and Matrices 2.1.1 Analytical Reference Substance: FC-95, lot 161 or 171. They are equivalent. 2.1.2 Analytical Reference Matrix: Bovine liver and bovine serum 2.1.3 Analytical Control Substance: None 2.1.4 Analytical Control Matrix: Bovine liver and bovine serum 2.2 Source of Materials: 3M ICP/PCP Division (2.1.1), Grocery store (2.1.2, 2.1.4 liver), Sigma Chemical Company (2.1.2, 2.1.4 serum) 2.3 Number of Test and Control Samples: Tissues and fluids from 30 test animals and 6 control animals. Tissues and fluids include liver, kidney, serum, cellular fraction, dermal application site and bile. Analysis of these tissues will be at the discretion of the Study Director. 2.4 IdentificationofTest and Control Samples: The samples are identified using the HWI animal identification number which consists ofa letter and five digit number, plus the tissue identity and day identity (serum). 2.5 Purity and Strength of Reference Substance: To be determined by Sponsor. 2.6 Stability of Reference Substance: To be determined by Sponsor. 2.7 Storage Conditions for Test Materials: Room temperature (2.1.1), 20 + 10C (2.1.2, 2.1.4). Test and Control samples will be received according to AMDT--10-0. 2.8 Disposition of Specimens: Biological tissues and fluids will be retained per GLP Regulation for the time period required for studies longer than 28 days. 2.9 Safety Precautions: Refer to appropriate MSDS. Wear appropriate laboratory attire. Use caution when handling knives for cutting the samples. 2 OCHORMES9F 3.0 EXPERIMENTAL - Overview `The tissues from animals dosed as described (HWI#6329-152), are available for analysis for fluorine compounds. At the discretionof the Study Director, a series of analytical tests can (See Methods--next be performed. Section) is the The appr screening for fl opriate analysis utooripdreesiennltivdeerfivniiaticvoemdbautsatifoorn : fluorine in the liver. When sufficient data Not allofthe tissues and has been collected to meet fluid samples the objectives will be analyzed. of the study in the opinion of the Study Director, analysis will cease. 4.0 EXPERIMENTAL - Methods 4.1 Liver and Serum screening methods: (attached) D4.o1h.1rmAaMnDnT-DXM2-010-00,OrTghaenrimcalHaElxitdreacAtniaolnyozfeFrl-uLoivreirde by Means ofa Modified 4.1.2 AMDT-M-2-0, Fluoride Measurement by Meansofan Orion EA940 Expandable Ion Analyzer 4.1.3 AMDT-M-4-0, Extraction of Fluorochemicals from Rabbit Liver u4.s1i.n4g AElMeDcTtr-oMs-pr5a-y0M,asAsnaSlpyescitsroofmeRtarbybit Liver Extract for Fluorochemicals 4.1.5 AMDT-M-8-0, AnalysisofFluoride Using the Skalar Segmented Flow Analyzer with Ion Selective Electrode 4.1.6 AMDT-M-14-0, Thermal ExtractionofFluoride by Means of a Modified Dohrmann DX2000 Organic Halide Analyzer-Serum 5.0 DATA ANALYSIS ss 5.1 Data Reporting: fluoride per tissue or Data fluid, will or as bFeC-re1p4o3rt(eedleacstarocsopnrcaeynmtarastsiosnpe(cwteriogmhett/rwye)igphetr)unoift of tissue or fluid. Statistics used, at the discretionof the Study Director, may sitnacnlduaderdredgerveisastiioonnsaonfalycsoinsceonftrsaetriuomnscofnocrednitfrfaetrienotnsdowsitehgtrioumpesa.nIdfnaevceerasgseasryan(din the opinion applied of the Study to determine Director), statistical simple statistical difference. tests such as Student's t test may be 3 Breog 6D .0 MAA INTT ENAA NCEA OF RN AW DRECORDS 6.1 Raw approved Data and Records: Raw data, final report, and electronic data approved protocol, will be maintained appropriate specimens, in the AMDT archives. 7.1 AMDT-$-10-0, Sample Tracking System 80ATTACHMENTS ~~~ 8.1 AMDT-M-1-0, Thermal Extractionof Fluoride by Means ofaModified Dohrmann DX2000 Organic Halide Analyzer-Liver 8.2 AMDT-M-2-0, Fluoride Measurement by Means of an Orion EA940 Expandable Ion Analyzer 8.3 AMDT-M-4-0, Extraction of Fluorochemicals from Rabbit Liver 8.4 AMDT-M-5-0, Analysis of Rabbit Electrospray Mass Spectrometry Liver Extract for FluorochemicalsUsing 8.5 AMDT-M-8-0, Analysis of Fluoride Using the Skalar Segmented Flow Analyzer with Ion Selective Electrode 8D.o6hArMmaDnTn-MD-X1240-000,OTrhgeanrimcalHaElxitdraecAtnioanlyozfeFrl-uSoerriudme by Means ofa Modified ` G0c86oF=L6.-9q 3M Environmental Laboratory Method ; `Thermal Extraction ofOFrlguaonriicdeHablyidMeeaAnnasloyza ferM-oLdiivfeired Dohrmann DX2000 Method Identification Number: AMDT-M-1 Revision Number: 0 Adoption Date: /o- $-1C Revision Date: None -_-- Author: Rich Youngblom Approved by: hi iroup Lead { Lithazie Quality Assurance fofs/7< Date f0o-g45 Date Software: MS Word 5.1a Affected Documents: AMDT-M-2 Fluoride Measurement by Means ofan Orion EA940 Expandable lon Analyzer AMDT-EP-3 Organic RHoaultiidneeAnMaaliynzteernance oaf Modified Dohrmann DX2000 1 Trees coz700 1.0 SCOPE, APPLICABLE `OM P NDS, AND MATR! CES 13 Matrices: Biotogeal tissues, parscutaly ve, f1l.1uoSricdoepef:roTmhivsarmieoutshomadtriiscfeosr. thTehoepefrlautoiroidneoifatyDpoicharllmyacnonllDecXt2e0d 0in0TwIhSeAnBitsiosluutsieodn tfoorexatnraalcytsis `1w.i2thApapnliiocnasbelleecCtoivmepeoleucntrdosde:. Fluorochemicals or other fluorinated compounds + 2.0 KEYWORDS D2.X12F0l0u0or,idfel,uofrlouocrhienmei,ceaxltsr.action, pyrolysis, ionization, ion selective electrode, Dohrmann, halide, 3.0 PRECAUTIONS condom, 3.1 Glassware and exhaust gases can be extremely hot. 33..32 3.4 PGrleassssuwrairzeedisgafsreagsi,lep,robpreorkecnomgplrasesssmeadygcaasuhsaeinndjluirnigesp.ractices required. Solvent based samples may flash, may need to allow them todry down before starting run. 3.5 Potential biohazards due to the biological matrices. Use appropriate personal protective 4.0 SUPPLIES AND MATERIALS STM water 4.1 4.2 Compressed Compressed Oxygen, Helium, Hydrocarbon free, High Purity Grade, regulated regulated to to 30 45 PSL. PSL. 4.3 Quartz glass sample boat with TeflonTM tubing, Dohrmann 890-097 or equivalent. 44..54 QOruiaonnz9g4l0a9ss99coTmobtualstIioonnictSubter,enRgetlhiaAndcjeusGtlamsesntGB-u9f4f0e5r-(0T1I2SoAr.Beq11u)iovarleenqtu.ivalent. 4.6 Sample collection vials, HDPE. 4.8 Polystyrene pipettes. 44..910AcHtaimvialtteodnCShyarrcionagleo, rE.eqMueivraclken2t0.05 or equivalent. 4.11 Miscellaneous laboratory glassware s EQUIPMEN 55..12 IRoBsMemcoomupnattiDbolher3m8a6nnorD4X8260c0o0mpOurtgera.nic Halide Analyzer, modified for fluoride extraction. 55..43 EDxXc2e0l 0S0prseoafdtswhaereet,, vveerrssiioonn 51.0.0o0,rmogrdeiaftieerd for fluoride extraction. 6.4 INTERFERENCES m6.a1ySvaamrpylfeiosimzemaitsrliixmittoedmtao tapproximately 150 mg, depending on sample moisture content. This 2 coziof 1.0 SAMPLE HANDLING s7a.1mpSlae.mplUesseafroerncoetpsoorbeprhoabnedlteodtrwaintshfebrartiesshuaensd.s. Fluoride may leach from the skin to the c`7ml:ee2taShnaansmocpalll,peoesrlofmaenltdihvcaeunrtoatlri-enwgcaubtotearrfdsr.oolmuTtfhireoonzceauntfttlirinvgeearbcoahanrdldipvaelrnaidcsesdccuaitlnpaeltasrheoduladndbelacbleelaendewdewiigthh bwoaatte,r,Use a : : RATION AND STANDAR| ION. 8.1 Preparationof Calibration Standards R8e1f.e1rTthoeprsottaoncdoalrdfsorrtehqautirpreodjefcotr. each project will ned be appropriate for tht individual project 881..5110..32mFgToy)praircnaadblbwliyetil5gi0hv-e5rit0si0tnupdaipelsma,bFeulCse-edb9ea5enidfnltimavereterdhaawnseoitlhgehstmbaaotnardti.axr.dsCaurteauspeide.ce of frozenbeefliver (100- 8.2 Calibration - Overview cTuhrevenoisrmraelquciarleidbrtahteiponroicsetdhuereflluiosrtieddebceulrovwe i(sAuMsDedT.-M-2). However,ifan optional spiked liver 88a..n22d.21coTAympbicucasaltlilibynr,agttithohrneeecmururesvpielincfgaottrehtsehoesfaDemXaec2h0me0st0thaonisddasgreadnneadrnadmtaeftdirvibexyctosynpcpieeknaitsnrgatthsieaomnspsaolmefpslsewtsiatnthdoakbrednsotewwsintlelds.tbaendards 8Rs.ep2ic.ko3evde.SrteadndFa(rudgc)uornvethweilyl-abxeisp.lotGteenderaastMeaasrsegSrpeiskseidonFc(uurgv)eoanndthcealxc-ualxaitseatnhde SeqtuaantdiaorndfMoarstshe line a8:n2d.4thMe ars2sv aSlpuie.ked F (ug) "FC-95 is 6=0.(0A4m%ouFntthesrpeifkoerde i0n.6m0L0)4 x is (tChoenfca.cotofr ustsaenddtaordcoinnvperptm)FCx-9(50.t6o00F4)* 82.5 Standard Mass Recovered F (ug) = (TISAB volume in mL) x (Orion reading in ppm) 83 Calibration - Procedure 8833..11.1StRaurtn 2Upor more be used if the previous sCalmepalneCsyccolnetsaiwnheednhisgthatcionngceinntsrtartuimoennsot fcafclhuodraiyd.e More clean cycles may 888333...222..21BlPFaronerpkrasarbebistasmtpuldieesu,siunsgetbheecsalmiveermaesththoedsmaatnridx.typPeroefpamraetartixleaasstt3hesatemsptlseasmopfleb.eef liver a(8n31a.0l20y.-z3e1sP5au0mtmpsglae)mpaflcocerobirlndainDknosgh.trommaentnhobodatA. MDCoTm-bMu-s2t efaorchthseaimopnlesealsecdteisvcereilbeecdtriondseeacntailoyns9i.0sand 3 OH00E4 COZ70 Jb8u.e3df.og2re.em4epnrFtoocroefreadtibhenbgiopwseitrtuadhiteotshr,ettchhaeelirmbereaatdteiionrng.riesaBsdtuianmbglesfoawrmiptalhbelrseasnnpkteclstatmthopilsheilsistmohirotiucilasdlrrebeaeacdh0ie.dn0,g3sop(fppurmenvodiroilunoswt4he8er hours). b8.e3f.o2r.e5prFoocreendoni-nrgawbbiitth stthuediceasl,ibrtahteiobnl.ank readings should reach a predetermined ion concentration c8.o3m.b2u.s6tiIotnm.ay be necessary to mix approximately 50 mgof charcoal with the sample to aid l88a33b..e33l.e1dStwWeaeinigdghahrbdooautCtsu.art vFleeoarstra1b5bimtatsrtiudxiessa,mpwleeisgh(51s0t0a-n1d5a0rdmsgwbietehf3lirvepelricsaatmepsleesa.ch)Reincotrardedweaingdhs in 8st3u3d.y2dataP.lacSetowreeitghheemdabtereifxlsiavmeprlseasmopnledriny Dicoeohrrimcaennpascakmsplteo kbeoeapt them frozen until used o`8qr.u3ai.nn3t.ti3hteyoSbtfeaterhtfewivisettrh.antdhaerldoowensotrsitnantdhaermdatcroinxc.entFroatriroanb.bitUsstiudnieg2s,Haumseil4tounLsoyfsritnagned,aerjedctaandfeijxeecdt it on m8a3y3b4e uAsteldeaasttt3herdepilsiccraetteisonshofotuhlde banealuyssetd, for the lowest standard concentration; more replicates r88e3.p3.l.3i3.c.a65teRsC,uornmubnaullasnt1o5tthhseetrasnsadaammrppdlsle.eIafsfordoetnshectrriesbpteladindciaanrtdes.eisctIsiniodgninci9fa.it3ceaainnntdldyaatdnaiaftlfhyearzteenttahecfcnrooermwditrnhegeplotiotchaAetMreDtrTewp-olMa-ce2s,the old replicate and that the new replicate will be used to calculate the regression curve. l8e.a3s.t3.07.95W,hceonnsaullltswtiatnhdasrudpserhvaivsoer.been run, calculate the r2. r2 must be at least 0.95. If it is not at c8h.3a.n3g.e8d.ANneeww ssttaannddaarrdd ccuurrvvee mshaoyuladlsboebreurnuwnhaettnhetdhiesccormebtiuosntoifonthteubaenaolrysst.ample matrix is 8.4 Storage Conditions for Standards T8y.4p.i1caSltloyr,asgteanrdeaqrudisreamreensttsorfeodr sattarnodoamrdsteamrpeerdaetpuernedeinntploansttihcesicnrdeiwvitdoupalbostttlaensd.ards used. 8.4.2 New FC-95 standards should be prepared at least once a month. 9.0 PROCEDURES 99..11.1TyCpoimcbaulsOtpieornattuibnegtCeomnpedriattiuornes:= 950C. 99..11.32 VOaxpyogreiznatainodnH/Derlyiiunmgftliomwe == 52040ccs/emcionntdes. 9.1.4 Bake time = 300 seconds. 99.22.1StIaftrhteUpprPorgorcaemduisrneo:t started, start the EOX program on the PC. 99..22..32 POuptetnhethfeumSaYcSeTmoEdMulSeEaTnUdPthweicnedllowi.n the READY mode. 9.2.4 Close the SYSTEM SETUP window. 4 Ra C0708 9.2.5 When the oven has reached the found in the CELL CHECK menu. READY temperature, run the CLEAN BOAT program 9.2.6 See AMDT-EP-3 for details of the Dohrmann sofware. 99:.33.1SaOmppelnetEhxetSraAcMtiPoLnEPrHoAceTdCurHe:and place the sample mix approximately 50 mgof charcoal with the sample to in the BOAT. aid combustion. It may be If this is necessary to done, charcoal should also be mixed in while establishing the baseline and when generating the standard curve. 1 9.3.2 Close SAMPLE HATCH. 9.3.3 Add appropriate volume labeled sample collection vial. of TISAB Typically solution or 1:1 TISAB:Milli-QTM water mixture to a 0.6 mL to 15 mL are used. For rabbit studies, use 1.0 or 2.0mL of 1:1 TISAB:Milli-QTMwatermixture. i9n.c3h.e4s.PlGaacesetsherevliaelasseod tdhuartitnhgetpiyproolfystihse mCuOstMBbuUbSblTeItOhrNouTgUhBtEhe iTsIiSnAtBh.e TISAB atleast 0.25 9.3.5 Run the EOX-SOLIDS program found in the RUN menu. 9.3.6 93.7 IWfhuendniltuhteeEd OTXISpArBogwraasm is finished, re used tocollect mov the e s the collection ample, add an vial from the equal volume combustion t of Milli-QTM ube. wat er to the TISAB to make 1:1 TISAB:Milli-QTM. 9.3.8 Rinse the end of the combustion tube with Milli-QTM water and wipe with a KIMWIPE to 9r3e.m9ovOepaenny tThIeSsAaBmprleemhaaitncihnganodn the tube. remove any remaining ash from the boat. Ash can be removed with a cotion tipped applicator or vacuumed out. It may be necessary to scrap particlesoff the. bottom witah spatula or other similar device. A dropofMilli-QTM water may be added to the boat to aid in the Clean Cycle. 9.3.10 Close the hatch. - 9.3.11 Run the CLEAN BOAT program. 9.3.12 Sample is ready for analysis by ion selective electrode (AMDT-M-2). 9.4 Sample Calculations (Slope) 9.4.1 94.2 Use the Sample sMtaasndsarRdeccouvreveretdo calculate F (ug) = the sample (TISAB vol value. in mL) x (Orion readinginppm-intercepr) 10.0 VALIDATION 10.1 Quality Control a1n0a.l1y.s1isDaiislsytaSrttaerdtbUypanCahlyezcikngSQamCplseasm:pleOsn.ceTthhee QstCansdaamrpdlceusrvaereistoesbteabtlhieshseadm,eeasachthdeayloowfest dcoonnceenitnrtartiipolincastpeikuenldesssamtphleefsirustsetdwotoregpelniecraattese the are swtiatnhidnar2d0cu%rovfet. heEascthancdoanrcdencturravtei,otnhmenusatbtheird replicate is not necessary. 103 Other Validation Parameters: NA 10.2 Precision and Accuracy: See method development analysis and sample analysis in `Fmlautorriicdese aNnodtedbifofoekrsen2t,3r,efaenrden5c. e cProemcpiosuinodnsa.nd accuracy varies when analyzing samplesofdifferent 5 cPoHzO7OoEfE 1.0 DATA ANALYSIS ILI Calculations 1H1L.L1L.L2 TFoorctahlecusltaatnedtahred fcluurovrei,deusceonrtergarcetsisoinoninatnhaelyssaimspilne,Exsceeel,mevterhsoidonAM5.0 DoTr-Mgr.e2at.er. : 11.2 Analyzing the Data la1er1se.s2w.ti1htahn1i2n5m20u0%so%tfotbfeheeaatcalhveaeosrttahg0e.ero95afntodhrotgshreeeaottuewtrol..ie"rOAuintslygireseruastc"ehrmotauhtylainbeer2se0xs0hc%oluuolfddetbdheie faptvoewirnotaegodefootuhftetithhnorseteeh.etrdewaptlaoircaanteds noted in the Final Report along with the reason it was considered an outlier 12.0 ATTACHMENTS None 13~ .0 REFERENCES ~~ 31439.,1 RreovsiesimoonuBn,tDDeochermmbaenrn1D9X932)000 Organic3 Halide Analyzer Operator's Manual (Manual 915A1n3a.2lyzAeMrDT-M-2 Fluoride Measurement by Means of an Orion EA940 Expandable lon A1n3.a3lyAzMerDT-EP-3 Routine Maintenance ofa Modified Dohrmann DX2000 Organic Halide 4.0 REVISIONS Revision Number Reafosr Choannge Revision Dae 6 7 Cc 02708 3M Environmental Laboratory Method 3 Fluoride Measurement by MeaAnnsaloyfzaenr Orion EA940 Expandable Ton Method Identification Number: AMDT-M-2 Revision Number: 0 Adoption Date: [0-475 Revision Date: None ------ tm ------------------ Author: Rich Youngblom Approved By: fone Gi Leader 15/0s Date Le SLR AL Quality Assurance fo-471 Date Software: MS Word 5.1a Affected Documents: AMDT-M-1 Thermal Extraction of Fluoride by Means ofaModified Dohrmann DX2000 Organic Halide Analyzer 1 #00055 coz706 10SCOPE.APPLICABLECOMPOUNDS, ANDMATRICES TLoIn SAnCaOlyPzEer:. This method is for the calibration and operationof an Orion EA940 Expandable 1.2 APPLICABLE COMPOUNDS: Fluoride. P1.H3 OAPFP6L.0. ICABLE MATRICES: Liquid samples in an appropriate buffer solution, Preferred 2.0 KEYWORDS 2.1 Fluoride, fluorine, ion selective electrode 3.0 PRECAUTIONS 3.1 No hazards idenified with this method. 4.0 SUPPLIES AND MATERIALS 44..12 OOrriioonn 9Mo4d0e9l999T0o0t0a0l1TeolneicctSrtodreenfgitlhlinAgdsjoulsuttmieonnt(ABguCflf)eroIrTe(qTuIivSaAlBeInIt.) or equivalent 4.3 4.4 MOirliloin-9QM4TM09w0a7ter10o0r peqpumivfallueonrtide standardo. requivalent, 44..65 MLaagbnetitsiscuess.ir bars. 44..87 SPlaamsptilce1c0o0llmecLtiovnolvuiamlest.ric flasks 44..910PoMliysscteylrleanneeopiupsetltaesb.oratory glassware. 5.0 EQUIPMENT 55..21 OOrriioonn MMooddeell 9E6A0994000 ESxolpiadndSatabtleeCloomnbiAnnaatliyoznerFolruoerqiudievaelleencttrode or equivalent. 55..43 MIaBgMnectoimcpaSttiirbPlleat3e.86 or 486 computer (only neededifusing Orion 3E software). 55..56 OMriciroonsoRfSt23Ex2ceilnte5r.f0a(coenclayblneee(doenldyinf euesdiengd Oifriusoinn3gEOrsiooftnwa3rEe)s,oftware). 6.0 INTERFERENCES 6Q.1PIwtastrerecwoilmlmgeenndereadlltyhabtrtihnegpsHampbeleattoorpnHeaorf6.06..0. A 1:1 mixtureof TISAB and sample/Millia6t.2roSoammptleempteermapteurraetuarsethmeasytaenffdeacrtdsflwueorriedewhmeenastuhreemmeetnetr. wIatis carleicbroamtemde.nded that the sample be 6.3 The rate the samples are stirred at should be consistent with the rate the standards were stirred. 2 SUOOTT cozioy 6u:n4deArirelbeucbtbrlodees trapped under electrode can give erroneous readings. Make sure noairis trapped 1S 0 AMPLEHANDLING 7.1 No special handling necessary. 8.1 Preparation of Calibration Standards 8.1.1 8.1.2 Measure Label the 50 mLof flasksas TI0.0S5,A0B.1,Il0i.n5t,o15.01,0a0ndmL1.5plpapstmicF-v,oalluomentgrwiictfhlatshkes.date and your initials. 8.1.3 Pipette 0.05, 0.1, 0.5, 1.0, and 1.5 mLof 100 ppm fluoride standard into theappropriately labeled flasks. 8.1.4 Add approximately 30mL ofMilli-QTM water to each flask. 8.1.5 Shake the flasks to mix the solutions. 8.1.6 Eliminate air bubbles from the flasks by tipping the flasks on their sides and rolling theairin t8.h1e.f7laBsrkisnogvtehretvhoelauirmebuibnbltehse. flasks upto the 100 mL mark with Milli-QTM water. 8.1.8 Invert and shake the flasks for the final mixing. 8.1.9 Record standards in Standards Log Book. 8.2 Calibration 88.22..21IIfnvneerctespsraorbye, troewmeotvetotpapseeaflrom electrods filling hole. tissues. 8.2.3 Eject a few drops of filling solution from bottomofelectrode to wet lower seal. 8.2.4 Fill the electrode with filling solution. : 8.2.5 The meter and the F- correction, using standards ewlietchtrcoodnecaernetrtaytpiiocnaslloyfca0l.i0b5r,a0t.e1d, by direct 0.5, 1.0, manedas1u.r5epmpenmtFw-,itfholnloowbilnagnk `the manufacturer's instructions. 8.2.6 Record the slope in the appropriate log book. 8.2.7 Clean the electrode by rinsing with Milli-QTM water and wiping the sides down with lab 8.3 Storage Conditions for Standards. 8.3.1 Calibration standards are stored at room temperature. 9.0 PROCEDURES 99..111CaTlhiebrsaatmipolneatnodbeMemaesausurreemdenntee,dSsttaonbdearmdixmeedthwiotdh:TISAB using the proportions. r9.e1c.2omPmlaecnedaedstibrybatrheinTIthSeAsBammpalneufaancdtuprlearc.e the sample on the stir plate. 9.1.3 Allow the sample to mix for a few seconds before inserting the electrode. When the electrode 9s.a1m.e4 Trhaee iasssaimtnphselerectaesldhi,obrmualatdkioebnesstuthraeendtsahraedmrsee. atreempneoraaitrurbeubabsltehsetcraalpipberdatuinondesrtatnhedaerldesctarnodde.stirred at the 9.1.5 When the readings have stabilized, record the reading in the appropriate log book. 3 ~GoHOzN7E0Og. 9.2 Calibration And Measurement, Using Orion 3E Software: 9922..111CaFloilblroawtisotne:ps 8.2.1 08.2.4. 99..22..11..32 TPrheesscoFmupnuctteiornscKreeyen#w8il(lFSa).sk you to confirm the number of standards to be used, Mcoankceenatrnaytinoenceosfstahreyscthaandnagredss,toantdhewihneftohremratoironnoptraesbelnatnekdiasntdo bcleicikncolnudCeOdNiTn IthNeUcEal.ibration. 9.2.14 Place the electrode in the first standard on the stir plate and click on CONTINUE. :: s9t.a2b.i1l.i5zeOdb,seprrevsestAheCrCeEadPiTngsREoAnDtIheNgGr.aphicdisplayon the computer. When the readings have 9.2.1.6 9.2.1.7 ARfeipeeratthsetefipna9l.2s.t1a.n4daarndd, 9t.h2.e1.5compfourtethrewirlelmadiisnpilnagy stthaendsalrodpse.ofthe curve, as well as the ainntderccleipctkaonndCcOorNreTlIatNioUnE. .ReTchoerdcatlihbrsaltoipoen,dianttaericseaptu,toamnadticcoarlrleylactoiopnieidn ttoheC:a\pOprrioopnr\iDaatteal\oCgalbiobo.tkxt 9.22 Data Spreadsheet: 9to.2s.t2o.r1eSdealteactin.either NEW or OPEN from the FILE menutoopen a new or existing spreadsheet 9.2.2.2 Record the name of the spreadsheet used in the appropriate log book. 99..22.33.1FlFuoolrliodwe sMteeapssu9r.2e.m1etnhtr:ough 9.2.4 99..22..33..23 ECnltiecrk tohne tnhaemNeoEfWthSeAsMamPpLleEibnutthieonappropriate place on the screen. a9p2p3r.op4riWahteenlogthbeoroeka.dings have sbilized, click on the RECORD button and write the result in the 0.0 VALIDATION _-- 10.1 Quality Control: 102 Precision and Accuracy p10p.m3 fOltuohreirdeVuaplitdoaatisoantuPraatreadmseotleurtisonAocfcfolrudoirnidgeto Reference 13.2, the range ofdetection is 0.02 11.0 DATA ANALYSIS 111 Calculations None necessary. 11.2 Analyzing the Data None necessary. 12.0 ATTACHMENTS None 13.0 REFEREN 4 GaeTet 02709 I1n3c.1orOporriaotnedM.od1e99l1 EA940 Expandable lon Analyzer Instruction Manual, Orion Research R1e3.s2eaOrrcihonInMcoordpeolra9t6ed0,901099S1olid State Combination Fluoride Electrode Instruction Manual, Orion 4.0 REVISIONS RNeuvimsbieorn ReafosrChoannge Due Revision ; 5 onboee oR710 3E M nvir Labo oratn orymental Method . Extraction of Fluorochemicals from Rabbit Livers SOP Identification Number: AMDT-M-4 Adoption Date: /o-7/-5 Revision Number: 0 Revision Date: None re e ee------------------------ Author: Dave Christenson/Cynthia Weber Approved By: . ip Leader GdLe hd Quality Assurance Jo--3/-25 Dae U=3r1s Date Software: MS Word, 6.0 MAfafsesctSepdecDtorcousmceonptys.: M-5, Analysisof Rabbit Extractfor Fluorochemicals Using Electrospray ~6H0664 | coziad 1.1 eSEltcehocyptler:aocsTepthraiatyseimmaestushsoesddpeticostefrxootrsrcatochpteyef.xlturoarcotcihoenmiocfafllsuforroomchtehmeiclaivlesrsfrfoormarnaablbyistislibveyrs. . 1.2 1.3 Applicable Compounds: Matrices: Rabbit Livers. Fluorochemicals or other fluorinated compounds. 3 ) 2.1 Se Fluorochemicals, rabbit livers, electrospray mass spectrometer, fluorinated LA $13 TERAL 4. I 1 Syringe, capable of measuring100uL. sm cmepeste oy 44..111.43 4.1.5 PPClllaaossvttiieccsgcernitnrdiirfnueggetutbuebsesP,e15mL 4.1.6 Labels fhe Lee 4.1.8 Timer 44..11.1910 4.1.11 DAFinilastlpeyortssi,acbTaliletpapinlpanessyti:lcogn3lascsycsrvsiyonrlgiuenmgfeeitlsrt.eircs,pi0p.e2ptsm. . PP -- 4.1.12Crimpcap autovials. Ee anes 4.2.1 pAqpumeaoquuseoAumsmsoonluituiomnoAfceatmamteon(Ailudrmicahc)e,taaptperboyx.ad2d5i0ngpp2m5:0 Pmrgepaamremoan2i5u00m awacteetra.teD1i0luat1e0t0hims Lsolvuotliuomnet1r:i1c0ffloarska a2n5d0dpilputme stooluvtoiloun.me with Milli-Q 4.2.2 a(SnNodd&i,21u.C0mOJcgNaorGfbHoCsnoOad,tie)u/m0S.ob2di5icuaMmr:bBoiWnceaatiregbh(onN2aa6t.He5CBuOf)ofeisrno(tdJ.2ioTu.m1 BLcaakverorbl)ou,nmaetaetiQcacasok)ond 4.2.3 Dilute acetonitrile 4.2.4Ethyl Acetate: solution, dilute acetonitrile 1:1 withMilli-Q water. 4.2.5 Methanol 44..22..76 M1iHl,l1iH-Q.2wHat.e2rH - perfluorooctanesulfonic acid (Aldrich) 4.2.8 FC-95 (3M Specialty Chemical Division) BHE064 2 CORT 3 fmm : $.1 Ulua-Turrax T25 Grinder for grinding liver samples. 5.2 Vortex mixer 55..54 ASnhaalkyetrical Evaporator :: 7.1 Ty The rabbit livers are received frozen, and must be kept frozen until the extraction is 8.1 8P.r1e.p1araPpretepairreoRnuoroaofnoIcinantnteecrrannlaapllhsotSnattnadsnasrddiardodftsaop2proaxhimiaterlya1n2 ppm 1SHa,m1plHe.,2H,2H8.1.2 W1e00igmhLatvloelausmtet0r.1icgfloafsk.1HR,e1cHo,r2dH,t2hHe-apcetrufalluwoeriogohctt.ancsulphonic acid into a 8.1.3 Bring it upto volume with methanol, this is the stock standard. 8.1.4 Toa 250mL volumetric flask, add 3 mLsofthe stock standard and bring to volume with Milli-Q water. Calculate the actual concentration ofthe `standard. --`asctuualpmhgopnerifcluaorcocitdanc- X 3m = acwal concenaton, ppm OIL 250mL 8.2 Prepare FC-95 Anion Standards 8.2.1 Prepare FC-95 standards for the standard curve. 8.2.2 RWeeciogrhdatphperaocxtiumaaltweeliygh1t0.0 mg of FC-95 into a 100 mL volumetricflask. 8.2.3 Bring up to volume with dilute acetonitrile. 8.2.4 aDaipslpourltouextiitmohnaetosefollyauptp1iro0on0x.pwiptm1h.0dpiDlipulmtue.teactehtiosnistorliulteio1n:110:f1o0rwiatsholduitliuotne oacfetonitrile for 8.2.5 Use the 10 ppm solution to make working standards with values close to 5.0 ppm, 1.0 ppm and S00 ppb. 8.3 Prepare Beef Liver Homogenate to Use for Standards 8.3.1 8.3.2 2AW0de0digmIhLm4sL0oMgifolftlhi-eBQosvwoialtnueetri.loinvGe(rr0iinandt1ot5oama2L5.h0oemmnLom.giefNnuaogluegseunsbeoel,buottPitrolene.pcaornetaionilng oight s1umspLenadlisqoulouttsioonf tbhye sshoaluktiinogn iitnbe15twmeLenceanltiqruioftusge tubes. Be sure to re- TOCO ORTTE 8.3.3 Spike seven SStaannkdards in osftetphe9.112moLfatlhieqpuortoscewdiutrhe.thOe nfeol1lomwiLngalaimqouuorntsserovfewsoraskithneg Working Sard Approx Fal . oT Bw (Approximate Conc.) `concentration of FC-95 in liver : 8.4 8.5 8.6 8.7 Calculatethe actual value of the standards: {kelstandagd.x_concenuation (inppm) 171 mg liver'/ T ml homogenate = final concentration (pprm) of FC -95 in liver FL"C+aA.v9le5rhaiogsmeroewgpeeoinrgathtetedsoaofsfbeo4qvu0iinvmeaglleilnvitevsreroinfinsFo2Cl0-ut09i5monpLoatsoafdseMstiielurlmim-isQanletwd.atbeyr.weTihgehiannsgount of Spectrometer. Calibration 8.5.1 Extract the spiked `method. Use these beef liver standards homogenate following to establish your curve 9.13 to on the 9.23 mass of this 8.5.2 OAflttehmeapteirvfelluyo,raooscttaanndsaurldfocnuartveeamniaoyn baendgetnheeraitnetdemuaslinsgtarnadtairosd oafnrieosnpvoenrsseess concentration of the perfluorooctanesulfonate anion, Storage Conditions for Standards 8.6.1 cNoevwersetdapnldaasrtdiscacreentprriefpuageretdubweisthunetialcthhaenaanlaylsyiss.isSotnantdhaerdmsasasresspteocrterdomineter is performed. 8S.t7o.r1a"geBeeCfonlidvietrihoonmsogefonratSestamnadyarbdesfrozen after preparation. 9-1 Obtain frozen liver samples. packaged with other tissues. In spent issue, note that the fiver has norbeen 95.:23 Wesiegahditshseecstaimnpglescdailrpcecltlaynidnctutaooftafreadppprlaosxtiimcagtreilnydi1nggoufbl.iver. 99-.54 PRuetacorldabtehleolnivetrh:eweviiaglhwtiitnh tthheessttuuddyynnoutmebbeoro,k.weight, rabbit ID, date and analyst initials. GBHcOoNERE714 4 99-.76 5:8 GRmAiirdnnidusnt2ede.stt5h,heemupsLnrasolmbplweteah.etesPraumtptlheeigsr2inhdoermopgreonbeeoiunsthseolsuatmipolnewiatnhd ngorilnadrgfeorcahbuonukts2. 9-9 ATMakDeT-tEheP-gr2i2n,deroapfaritntaontdheclseaamnpiltewiwtihthme2t.h5amnLclsawfaetrereaucshinsgamaplsep.eFrollow 99--1110 mPiCnapafeipotnrtimh|maensgLsoansmipeanlstpeto)h.aen1gd5rmvionLrdtiencxegntftuorrbi.f1u5g(eSseetecuobAen.dMsLD.aTbe-lMt-h4ceWnotrrkisfhuegeettufboredwoicthumtehnetiidnengtficoa.l :- 9-12 aSspidkeesctrhiebbeedefinli8v.e3r homogenates with the appropristeamount of FC-95 standard 597-1134 aAScpdeitdakte|e.tmheLsoafmpthleessoadnidubmeceafrlbiovreratheo/msoogdeinuamtbeiscawribtohna1t0e0buufLfeorfainndtem1 amllstaandamrd,e 99..1165 9:17 CPUusatipntgthheaernsiaannmaptllhyeetisachanaldkpeviropreftto,erxa2d20d0m5tmon3L0estehcyolndasce.tate. 9-18 oCnentmhietcuegnetrfiofrug2e01t0o.2255. minutes, unil the layers are wll separated. Set the power 9:19 9-20. BRmleLomwgorvtaehdeu4astamemdLplgeloafdssothwpeinpteootpn.oTtrrhgaeannasinfcaelrlytiahceayll0eaebarvealpfor0ersaththeo1rf5mrteonsLhecateurnbdterr.yinfeusgse twuibteh wniitwhogae5n, 39:.3232 arpnprgoxtihmearteemlayi3n0intgo Vortex 15 seconds. s4a0mmpilneutuepsi.n 1mLdilute acetonitrile with an analytical pipet. 923 Ttshtreuadnsysafnmepurlmtebheeinrstaoaamnpdflraeensi1hm0acale3nmntruiLmfbuesgrye.ritnugbeeo.rAtaaacuthovi0a.l2.uLmabenlytlhoentmuebsehoffivliearl,vaindg fpisler 39::2254 CCoampplanedtehoAlMdDfTor-aMn-al4yswiosrbkysheeleetcatrnodsparnaaycmhatsospasgpeecotfrosstcoupdyy.notebook leya1100u..21pQParueacltiistiyoonCnoanntdroAlc-eunortacayp-plnioctabalpeplicable 10.3 Other Validation Parameters- not applicable LODA11T.1 ANAonNeALYSIS 0000 12.1 Worksheet AMDT-M-4 13.1 AMDT-EP-22 Routine MaintoefUnlaanTacrrae 1-25 RLevoisRioenvisions Number ReasonforChange 00 Revision Dae GHoCu0e7r18 Worksheet AMDT-M.4 ta 0 F f F F Fr 1 -- tr ert EE -- a 02716 3M Environmental Laboratory Method Analysis of RaEblbeicttrLoisvperrayExMtarsasct SfpoerctFrlousocroopcyhemicals using : SOP Identification Number: AMDT-M- Adoption Date: /-( -q5 Revision Number: 0 _-- Revision Date: None Author: Dave Christenson/Cynthia Weber Approved By: roup Leader : 4 Z Quality Assurance l/es Date Wii Dae: Software: MS Word, 6.0 Affected Documents: M-4, Extractionof Fluorochemicals from Rabbit Livers 1 SHO0tY C 071F 1.1 sfSistlcuapoinepddresaf:rofdTrohrmMi/efsZdl.umbo=eyrto4shc2ioh7nedg,mlieaiscniadfolonosrtmtuhohseneirinatagnpoatprlhriyeonscpgilrsieoacoftmfeFoeCsmx-pta9rrsa5ascyetassnmiooafrns,asbMsb/pieZtc=tlri4vo9emr9e,toertrho.etThihentreetrainnsaaslluyessiosr . 1.2 Applicable Compounds: Fluorochemicals or other fluorinated compounds. : 1.3 Mflautirdsi.ces: Rabbit Livers (samples), Beef Liver (standards), other tissues and 2.1 Fspleucotrroocmheetmeirc,alrasb,biftluIovreirnsa.ted compounds,clectrospray mass specioscopy, mass 30PRECAUTIONS ~~ 3.1 Use caution with the voltage cable for the probe. When the voltage cable is plugged 3.2 Dinotno ottherpurnobtheeDpOumNpOaTboTvOe UitC'sHcaTpaHcEitPy RofOB4E00,0tphsei.reIifsprriessksoufreelegcotersicoavlesrh4oc0k0.0 psi sfitnodp tahnedprleulgeaasnedprreepslsaucree.tTheheplpuegagkedtutbuibinngg.maSyeebAe MplDuTg-geEdP. -T1r5oubleshoot back to 3.3 Do not run the pump to dryness. 4.0 SUPPLIES AND MATERIALS 4.1 Supplies 4.1.1 Nitrogen gas regulated to 140 psi. 4.1.2 Fluofix column or equivalent. 4.1.3 100 uL or 250 uL flat tip syringe for sample injection. 4.2 Reagents 44..22..12 MDiillultie-Qacweattoenrit,riallle wmaotbeirluesepdhasien,tdhiislumteetahceotdonsithroiulled1b:1e wMiitlhliM-iQllwia-teQrw.ater, 55..21 IVSGCTOriSoyr2i0n0g0e EPluemctprospray Mass Spectrometeror equivalent. 53 Specuaphysics AS300 Autosampler 5.4 10 uL Assembly 5.5 Autovials or capped centrifuge tubes. a inererencesais me. 7.0 SAMPLE HANDLING 7.1 Keep the extracted samples in capped 15 mL centrifuge tubes or in capped autovials until ready for analysis. coR7Ag 8 ALIBRATION AN] STANDARDIZATION 8.1 8P.r1e.p1araeSxteiivroeanncrbieoofenfplCriaovlceierbdursrateta.nido(anSredSestAaanMnddDoanTredMsb4la:nksebceteifonliv$e0r)are prepared during the 8.2 Calibration 8.2.1 8.2.2 ToRyuponicbtahlielysteohvneensbtseatenafdnadlraidrvdceur5rsvrteuanndaafredrs twice, each starting with 107 samples. the lowest standard Choose a sandard 3 : in he same range of conceniration a he Samples 8.3 S8.t3o.r1a"gecForveCesohrnedsdtipatlniadosatnrisdcscfanoearHpfSruetgpaeanrdteuadbrewdsistuhnelxcthh anaanlaylsyissi.sSotnanfhdearmdiscareSpsetcorieedaniner is performed. Samples and standards are NOT refrigerated. 8.4 Storage Conditions for Beef Liver Homogenates 8.4.1 Beef liver homogenates may be frozen after preparation. 9.1 Initial Set-up pon 99..11..21 RSeetcosrodftbwaacrkeitnog"pOrpeesrsautree oinn"t,heIoinnsMtorudmeenEtS"l.og. 9.1.3 Fill the solvent cylinder with mobile phase. 9.1.4 `Sceotmtihnegpouutmopfttoh"eRtuinp"o.f Stehte tphreobfel.owThteo p1r0e0s0suurLe/mshionu.lOdbbseeravte1s7d0r0optloet1s800 9.1.5 cChhipesc.kTthhee ftuipsesdhosuillidcabaet ftlhaet ewnitdhofnothjeagpgroebde.edgUesse. aInf aeyney pciheicpes taorechfeocukndfor cut off the tip of the silica with a column cutter and pull the silica through to the appropriate length. 9.1.6 nCihtercogkyeonulreankiitnrgoagreonusnudpptlhye.tiTpoufmthoen ptrhoeben.itArogfeinn.e Tmhisetreshsohuoludlbdebceonmoing out of the tip. 9.1.7 Carefully guide further. Connect the the probe into the voltage cable opening. Insert to the probe. it until it wongo'anty 9.1.8 `Gapoprtooprtihaete"Emdaistsoer"s ptaog4e2,7anadndse4t9I9o.nization Mode to ES', and the. 9.1.9Ifitis not in single ion mode goto -Option and set SIR. 9.1.10Stant Acquisition. Assigna file name, MO-DAY-YR + letter. Record it in the log book. 9.1. 11bReugnintnhienbgeeoff ltihveerruns.a.mRpluensfairQstC,rcuhnencikngbyearcuhnnsitnagndoanred sttwaincdearatd the after every 5107 samples. 91213 Wait two minutes, nd injec the next sample. 9.2 9M.a2n.u1alDrIanwje1c5t0iounl.ofsampleino a syringe. Inject the sample into the rheodyne injection por. Inject slowly. Record the sample ID in the log book. 9.2.2 Tum the valve 10 "On". 9.2.4 Record the scan number for each sample in the logbook. co2729 9.3 9U.s3i.n1g StehteupAustaompslaemptlraeyrA, B, or C. 9.3.2 vRieaclosrmdatyhebesaimnpelaecsharnudn. their positions in the instrument log book. Up to 17 9-3.3 9S.e3t.u3p.h1e samplPeursh the sample bution 99..33.33132 SSeertsianmjpelecylsoaopmps=ilz2ee = 100 ul 99..33.33154 SNaemteCytchelefitlem:eL=iv0ers 99..33.330.67 AIddednitfhye tshaempwlaeysutsoeQdueue by pressing "Enter" 9.3.38 Press "Run" o start 100v1A0.a1LQpuaAlTitIy OCoNntrol 00000 10.1. Rsputeaannkdaahresditgwahintldloacrbcdeueruvsseedsr.tyopT5httehoer7reusmnaa.mipOnlnienls.gy stIahemapsslaiemgspnilwfeiislcalbnbetefocrrheeaanntaghleey(lztaesdt5.0ac%c)epitnable 10.2 1Pr0e.c2i.s1iSoeneaMnedthoAdccVualriadcatyion Report number AMDT-M-5.0.1 1100..43 ORetfheerrtoVMaeltihdoatdiVoanliPdaatriaomneRteeprosrt Number AMDT-M-5.0.V1 1111..21. PClaoltcutlhaetisotnasndard curve, using the meanofthe two values obtained for cach 1st1a.n2da.rd1.Read peak heiogrharteass regression to determine the sfoarmptlhee scoanmcpelnetrsatfiroonms.the printout. Use linear 11.2.2lCiavelrc:ulate the mg of FC-95 anion, or other fluorochemical in the total rabbit `mg FC-95 anion in the total rabbit liver = megmFsCo-f9li5vaenriounsfedrofomrsainda.lcyusirsve x Total massofliver, gms 1111..43 PsMrtiannatdaaarcdkrheIrsDuo.elmtWasrttiaotbgelreathmaenfdsotreuednaytcenhirutsmaibmneptlrheeo,nswttiuhtdehyptbrhoienotkpo.euatk,sinliatibaell,eddatwei,thantdhepsuatmiplien tohre study folder. Staple all chromatograms together and number pages. 4 None 13.1 AMDT-EP-17 WOREVISIONS Nopon n Revision 5 Toho 3M EnvironmentalLaboratory Method Analysis of Fluoride UsiTnogn tSheeleSctkiavlearElSeecgtmreondteed Flow Analyzer With Method Identification Number: AMDT-M.-8 Adoption Date: Jp-s_g Revision Number: 0 _-- Revision Date: None Author: Deb Wri/gCynhthtia Weber } Approved By: upLeader LE <r . G* om. Quality Assurance 1/5/75 Date 1-27-95 Date Analyzer Software: IBM MS Word, 6.0 Affected Documents: AMDT-EP-26, Operation and Maintenance of the Skalar Segmented Flow 1 oT 2 1-1 This method is for the analysis for the Dohrmann DX2000 (AMDT-M fluoride, thermally extracted from samples using SloengmSeelnetcetdivFelEolwecAtnraoldyez(eIrSEw)i.tThhIe-SE1a.n)a,lyasnids collected in TISA Bfor analysis is performed using the Skalar with an 1.2 Samples can be the Dohrmann. tissues, serum, biological material, or other `materials extracted on 2.1 Skalar, segmented flow, fluoride. 3.1 Follow standard laboratory safety practices. 4.1 444S..1u11p1..p312liPSAeouasltmoyppplirpeoepctyuslp,eson,xef4ovmrodlLourmpleaersqntuciicvfcaiulcepknst,wwi1it0thc0hmapipla.sstic tips 41.4 4.1.5 nSCuaanmmubpreliredsg,perceofmlpeorn,enEtvse,rgrreefeenr to the Skalar Methodsfor components andpant 4.2 4R.e2a.g1enBtrisj 35, 30% SF.A.S. Detergent 4.2.2 4.2.3 TISAB II buffer solution: Purchase TISAB I from TSaImSpAlBerIlriandsidng2.s5omluLtioonr1: 0Di0lputpemTIfSluAoBriIdTe 1s:o1luwtiitohn Orion. To 1 liter Mainldli1-QmwLaBtreirj.. of 4.2.4 the volume up to 1 L with Mill-Q ater mNitsriccoancciedntsrolautteidonniftroircdaecciodnt(aHmNinOa)titoon,2510N(mlLasbgorfadMei)ll:i-SQlowawtleyr.aBdrdi6n4g 4.3 Standards 4.3.1 4.3.2 Stock solution, 100 ppm F: purchased from Orion. IwnittehrMmieldliia-tQe swtaatnedra.rUd,s1e0poplpymp:roDpiylluetnee1v0olmuLmsetorficstfolcaskkss,olution 10 100 mLs 4.3.3 yowWoixoltfrhuokrmMideinsolgorlfspQiiunnmdwtpaeemrrrdam.:etdeMiaaptikpeeeotsru,pstttoohceSkOfsomtlalLnodwoairfndgTiwInodSriAkcaBitneagdnsdoundaintldhuatritdnasbglbtey6, ausdidnigng the 100 nL [WorkiOngeSamndard --0pm |C mlsofStockStane dard |mlsofTeie ergmetd7iaereSstuannddaurdd| -- --S0epeemmm p -- p py p p 2] 2 S:1 Skalar Segmented Flow Auto Analyzer SansTM System equipped with ISE 6.1 interencen. High concentrations of:alkalinity, chloride, phosphate, sulfate or iron can cause 7-1 Samples should within 30 days. be stored in polyethylene boules. Samples should be analysed 8.1 P8.r1e.p1araPrteipoanreocfalCiablraitbiroantsitoannSdtaradnsdaasridn ssection 4.3, 8.2 C8.a2l.i1braTthieonstandards are analyzed at the beginning of the run. 8.3 Storage Conditions for Standards 8.3.1 sSttaannddaarrddssaarree sptroerpeardeidn actaappmeidnpiomluymporofpyelveenrey vsoixlummoentrtihc,floarskass. nNeceewssary. 9.1 Start 93.:1112.1 UPCupltaPhmrepodfcoelwdunurotehecpuompdceckns,ianircboacrswoadnsd smapmpile:r-pump tubing, 9-1.3 bTauthm. on the power of the sampler, pumps, offset potentiometer and heating 99..11..54 TtPuuutrmnthoaennretahtgeheeinnttI-elnritfneaercsfe,ainccetohmebpeaufptoperrroe,prdtiihasetpelcabayotrtamlnepsd.ubpreirnter. Make sure you 9.1.6 Let the system stabilize for approximately 30 mines. 9.2 Starting a Run 9.2.1 Create a sample table by the name of the file, and selecting FILES, press ENTER. TABLE, and CREATE, type in 9.2.2 9.2.3 9.2.4 FsPDPicirRlaCilIlnoNthntTedth,sheSesGfasaoRrammmpOapplmUleperhPlasteyae1.btlwwiTeihnh,tcgihihssn,tstwheo3ierlttdlhSeeadpinraiidpnnaptrtrrhdotepshr,esiOyseaFsntmttesipeernmlecuetormanunbbndle,weruobomgyfeptssuasmaihpilirensg,seEnS,uCm,bTeWr of and 9.2.5 SEeWt RthUe NbuGsUinTecups on the samples ds noe rod tae eon 3 CHE-4 . 9-2.5. smIeaSleyelcetbcietngiGnCRhOAePNDHTaIRtCaOSLH,anPRdAElNiAnELgLTPaIannMedEl..pSuIswfhiyitoncugh cFta7o.ntnhoetAgneatlyrseiasltPimaen, ypoyu 92.8. t2bhaUessebeolittnthe.eomsAmdoajflultshtsectsrhceerwebdeanrs.ievleirnefournttihleiotfsfsaetppprootxeirmtaitoemleyte3r/4oisnecthtfheom 9-2.6 9-2... t3hCehienctekrftahceehsicgrheeswt#s3t.andard and adjust the gain, if necessary, with GloltnooCtObeNTruRn.O(LSePleAcNtEoLr , and t analysis panel. Deselect the analysis that 9.2.7 10 retum to the Analysis Padneesle.lect analysis by Press the spacebar to bring up the local menu. pressing ENTER) Press Tab. 99.22:.98 pTSreyelpseesctEySoNuTTrAEIRRDTfGotironicsithaaorlit)c,etshte)h,eancsahlaoymospsilesertuanbnlienwghwiicthhyooruwictrheoauttedthuendseyrst9e.m2.1taogre 9-2. 10AsaefntidteosrctlshetecatrtiiSgnhTgtAtnRhueTmsboAefNrtAwoaLfrYes,SaImstpSalr.etsthaensdatmhpaltert.heMsaakmpelesu/rweasthh/aatitrhetismaemspalree.r is 9:2. 1 SOeKl.ect GRAPHICS, REAL TIME to view the progress of the analysis. 9:3 9L-o3a.d1inagnGdoastneoldCecOPtrNLiTOnARtiDOn.Lg SPteAhleeNcEtDLAa,tUaTp-rFOeisClseAtLheCsUpLacAeTbaIrOtNo barnidngenutperthtehelofciallenmaemneu(or 9.3.2 Thioghvliiegwhttthheecfailliebr(0atbieonpcruinrtveed, CURVE. agnodtporGesRsAEPNHTIECRS),.CALIBRATION 99..33..43 TToo pprriinntt tthhee lhoigwhlelveevlelsccurerevne,, SETTINGS. Change the max ppuusshh EPSRCINtTo gSeCtRoEutEoNf,graphics. Select y value to approximately 500. Go to CAL 9.3.5 pRCreUetsuRsrVnEENtoTaSEnEdRTTapnIredNssGPESRSICaN,rTdaScnhdCaERnngEteeEr.tNePtromepssrsinatPlsRoaIsmNpTbleSaCpReaEkEs4.N09,5, go 10 EDIT, 9.3.6 OToUTpPriUnTt.theSerleesculttsPRg0INtoTECRONfoTrRtOheLEpPsAoNnEoLr,PSRPNAfCoErBtAheRL,asOerU.TPUT, 9.4 9S.h4u.t1doPuwtnall the reagent-lines in Milli-Q water. 99..44..32 QLAffefttseetrthtpehosetyessnyttsietomemremitnhesares.fTroiurnrsanepdporfcofoxmtiphmleaehtteeealltyyi,n3gt0ubmmaitnohuftofentsh.weeseakmepnldesr., Lpeuamvpe alniqduid in 99..44..54 TRtehaelkeelaisnteehsetheelepcutrmopd-edeocutksa,ndaisrobaakrsinan1d00sapmppmleFropvuemmpi-gtuhb,ing. 99..44..76 OSenleFcrtidFaIyL,EwS,inproefsfstAheLcTomFpuatnedr,seldeicstplQaUyIanTdtoinetxeirtfatchee fporrogtrhaemw.eekend. 100v1A0.a1ulQupaaliTtyIOCoNntrol 0000000000 10.1. IasRciucgnenipftaiacbsaltneatnscdthaarandndg(aermdiidnwiptoleahbkieghhuesicegdoh.ntcoTechnceauarrtsei,mooanni)lneyivnteghresyas1ma0pmlpsealsmepswliebsle,fboreIefratahneallayssted. 4 CORTE amy 10.2 10.3 10.4 Precision andAccuracy 10.2. 1See Method Validation Report number AMDT-M-8.0.V Other Validation Parameters Refer to Method Validation Report Number AMDT-M-8.0.V1 11.1 11.2 11.3 11.4 Calculations 11. 1. The standard curve is plotted by the Skalar software. 11.1.2All calculations are done by the Skalar software. better. * should be 0.995 or iPWrrteihptaearltlehpesapscrtkeuaaddgysehndeueomtcbsuemtroensotnusmtmahanerdpirpzilneatcodeuattisan,. tiIhnniectislatuldu,eddyastfaeomlpdtheelre: pvMroianltkuomeuer3,, cawonepdiygihontsdtuosgeedtehce.r summary sheet and tape nto the study notebook. Back up all data and f the spreadsheets `onto study disk and backup disks. E1l1e.c4t.ro1niGcLDPatsatudies: Electronic data is copied onto the Study floppy disk for each 11.4.20sttuhdeyr,asntuddailess:oAdllaadatisaciospcioepdioendtoonatfaolofplpoypdpiysdkistkhatthiast stored in is stored the lab, in the lab. None 13.1 13.2 13.3 DAXMD2T0-0M0:-Or1g,anTihcerHmaallidEextArnaacltyizoenr-oLfiFvleuroride by Means of a Modified Dohrmann Skalar Methods, #335, Skalar Methods Manual AMDT-EP-26, Operation and Maintenance of the Skalar Segmented Flow Analyzer Revision Number Reason for change Revision Dae 5 coz726 3M Environmental Laboratory Method `Thermal Extraction ofOrFglaunoiricdeHablyidMeeAannaslyozefar M- oSdeirfuimed Dohrmann DX2000 Method Identification Number: AMDT-M-14 Revision Number: 0 Adoption Date: /0-3 7 Revision Date: None _-- Author: Rich Youngblom Approved by: rGooupweLre)ader . 0/5) Dite 2s Quality4Ass4urance 2 A Fez Date Software: MS Word 5.1a Affected Documents: AMDTE-xMp-an2daFbllueorIiodneAMneaalsyuzerrement by Meansof an Orion EA940. AMDT-OErgPa-n3ic RHoaultidieneAnMaaliynzteernance ofa Modified Doi hrmann DX2000 LOY {0 SCOPE , APPLICABLE COMPQUNDS, AND MATRICES 1.1 Scop fluoride e: fr oTmhivsarmieoutshomadtriiscfeosr. t he operation The fluoride oisfatyDpoicharllmyacnonllDecXt2e0d 0in0TwIhSeAnBitsiosluutsieodn to fo extract r analysis `1w.i2thApanpliiocnsaeblleectCiovmepeloeuctnrdodse:. Fluorochemicals or other fluorinated compounds. 1.3 Matrices: Biological fluids, particularly serum. 2.0 KEYWORDS '2.D1X2F0l0uo0r,idfel,uofrlouocrhienmei,ceaxltsr.action, pyrolysis, ionization, ion selective electrode, Dohrmann, halide, 3.0 PRECAUTIONS 3.1 Glassware and exhaust gases can be extremely hot. 3.2 Glassware is fragile, broken glass may cause injuries. 3.3 3.4 SProelsvseunrtibzaedsegdasseasm,pplreospemracyomflparshe,ssmeadygnaesehdatnodallilngowprtachteimctesodrreqyuidroedw.n before starting run e3.q5uiPpotmeennttial biohazards due to the biological matrices. Use appropriate personal protective 4.0 SUPPLIES AND MATERIALS 4.1 Compressed Oxygen, Hydrocarbon free, regulated to 30 PSL. 4.2 Compressed Helium, High Purity Grade, regulated to 45 PSL. 4.3 Quartz glass sample boat with TeflonTM tubing, Dohrmann 890-097 or equivalent. 4.4 Quartz glass combustion tube, Reliance Glass G-9405-012 or equivalent. 4.5 4.6 SOraimopnle94co0l9l9e9ctTiootnavliaIlosn,iHc DSPtrEe.ngth Adjustment Buffer (TISAB II) or equivalent. 47 Mill water 4.8 Polystyrene pipeties. 4.9 Activated Charcoal, E. Merck 2005 orequivalent. 4.10 Hamilon Syringe or equivalent 4.11 Miscellaneous laboratory glassware 5.0 EQUIPMENT. 514 Excel Spreadsheet, version 5.0 or greater 5.1 5.2 IRoBsMemcoomupnattiDbolher3m8a6nnorD4X8260c0o0mpOurtegra.nic Halide Analyzer, modified for fluoride extraction. 5.3 DX2000 software, version 1.00, modified for fluoride extraction. 6.0 INTERFERENCES 6.1 Sample size is limited to approximately 100 yl. This may vary from matrix to matrix. ro 9 7.0 SAMPLE HANDLING 7-1 Samples are to be handled with plastic pipettes. A new pipette is to be used for each sample. 8.0 CALIBRATION AND STANDARDIZATION 8.1 Preparation of Calibration Standards R8.e1f.e1rTthoeprsottaoncdoalrdfsorrtehqautiprreodjefcotr.each project will need to be appropriate for that individual project. 88..11..32 TFyoprircaablbliyt 5s0e-r5u0m0sptupdmiesF,Cu-s9e5beinefmestehraunmolassttahnedmaartdrsixa.re used. 82 Calibration - Overview `cTuhrevenoirs mraeqluicraleidbrtahteiponroicsetdhuereflluiosrtieddebceulrovwe i(sAuMsDedT.-M.2). However,ifan optional spiked serum a8n2d.1coAmbcuasltiibnragtitohnecmuursvienfgorthtehesaDmXe20me0t0hoisdsgeannedramtaetdribxy tsyppiekiasngthseamspalmepslewsittho kbenotewsntesdtandards s8p.i2.k2edT.ypically, three replicatesof each standard and five concentrationsofstandards will be. R8.e2c.o3veSrteadndFar(dugc)uornvethwielyl-abxeisp.lotGteenderaastMeaasrseSgrpeiskseidonFc(uurgv)eoanndthcealxc-ualxaitseatnhed eSqtuaantdiaorndfMorastshe line a8.n2d.4thMears2svaSlpuie,k*eFdC-F95(uigs) 6=0.(0A4m%ouFntthesrpeifkoerde i0n.m60L0)4.xis (tCheonfea.ctoofrsutsaenddatordcoinnvperptm)FCx-9(50.t6o00F4)* 8.2.5 Standard Mass Recovered F (ug) = (TISAB volume in mL) x (Orion reading in ppm) 8.3 Calibration - Procedure 8b8e33..u11se1dSitRfaurttnheU2pporrevmioorusesCalmepalneCsyccolnetsaiwnheednhisgtahrtcionngceinntsrtartuimoennstofefalcuhodraiyd.e.More clean cycles may 832 Blanks 88.33..22..12 PFroerpraarbebistasmtpuldeiesu,siunsgebtheeefsasmeerummetahsotdhse amnatdritxy.pe ofmatrix as the test sample. 8an3a.l2y.z3e sPautmpsleeruacmcbolradnikngintoDmoehtrhmoadnAnMbDoaTt.-MC-o2mbfuosrtthseaimopnlesealsecdteisvecreilbeecdtriondeseacntailoynsi9s..0 and j8bu.ed3f.og2re.em4epnrFotocroefreadtbihbneigtopwseitrutadhtioetsrh,ettchhaeleirbmereaadttiieonrng.riesaBsdtuianmbglefsoawrmiapthlbelrseasnupnketicsltatmthopilsheilsitsmohirotiucilaldrrebeaeacd0h.ei0dn3,gsopr(ppumrnetvoiilroilunoswt4he8er 8h.o3u.rs2)..5 before prFoocreneodni-nrgabwbiitth stthuediceasl,ibrtahteiobnl.ank readings should reach a predetermined ion concentration c8o.3m.b2u.s6tiIotnm.ay be necessary to mix approximately 50 mg of charcoal with the sample to aid CORI oGd ewee.nt 88.333..3 1S[tPahnedearrsdcrCuumrviefrozen, day (=30 mL). thaw at least cnough to complete the standard curve analysis for the 8q8u33a..n33t..i32tySoPtfiarpttehtewtiestth1an0tdh0ae4rLldooowfnebsoetresfitsnaentdrhaeurmmdatcironintxco.enDtForohartrimroanab.nbintUsssatimundpgileeas,Hbauomsaetil4tounLsoyfrisntgaen,daerjedcatandfeijxeecdt it on 8or33in.4thebAteleefassetr3ruemp.licates should be used for the may be used at the discretion ofthe analyst. lowest standard concentration; more replicates 8r8e33p..l33ic..a65teRsC,uornmubnaulasntIoStthhseetrasnsadaammrpdplsle.eafIsofdroentshecartriesbpteladincdiaantreds.eisctIsiniodgninci9af.ti3ecaainnntdldyaatdnaiaftlfhyearzteenttahecfcnrooermwditrnhegepltoiotchaAetMreDtrTewp-olMa.ce2s.the 8o.l3d.3re.p7liWcahteenanadlltshtaatntdhaerdnsewharveeplbiecaetne rwuinl,l cbaelcuusleadtetothcealrc2u.lart2e tmhuesrtebgreeastsiloenasctu0r.v9e5.. least 0.95, consult with supervisor. Ifit is not at c8h3a.n3g.e8d.ANneeww ssttaannddaarrdd ccuurrvvee mshaoyuladlbsoebreurnuwnhaetnthtehdeicscormebtuisontoifonthteubaenaolryssta.mple matrix is 8.4 Storage Conditions for Standards 8T8.y.44p..i21caSlNtleoyr,wasgFteCarn-de9aq5rudissrteaamnredenastrtsdosrfesodrhoasuttlardnodboaermdptsreeamprpaeerdreaedtpueartnedleeiannsttplooannstctiehceasicmnrodeniwtvihtd.oupalbostttalensd,ards used. 99..11.1TyCpoimcbaulsOtpieornattbinegtCeomnpderiattiuornes:= 950C. 99..11..32 VOaxpyogreiznaatniodnH/Derlyiiunmg ftliomwe == 52040c/smecionnudtse.. 9.1.4 Bake time = 300 seconds. 99.22.1StIafrttheUpprPorgorcaemdiusrneo:t started, start the EOX program on the PC. 99..22..32 POuptetnhethfeumSaYcSe TmEodMulSeEaTnUdPthweicnedllowi.n the READY mode. 9.2.4 9f.o2u.n5d Close Wihn etnhe tthhee oSvYenSThaEsMreSaEchTeUdPthweiRndEoAwD. Y CELL CHECK menu. temperature, run the CLEAN BOAT program 9.2.6 See AMDT-EP-3 for details ofthe Dohrmann software. 99.33.1SaOmppelnetEhxetSraAcMtiPoLnEPrHocAeTdCurHe:and pipette 1004L of sample into necessary 0 mix approximately 50 mgof charcoal with the sample to the aid cBoOmAbTus.tioInt.maIyftbheis is dstoanned,arcdhacrucrovael. should also be mixed in while establishing the baseline and when generating the 9.3.2 Close SAMPLE HATCH. . COoRv75P 73 alll> remove any TISAB remaining on th tube. 9.3.3 Add appropriate volumeof TISAB solution or 1:1 TISAB:Milli-QTM water mixture to a 2l.a0bemleLd soafm1p:l1 eTcIoSlAleBc:tMioinllviial-. QTMTywpaitcearllmyix0t.u6rem.L to 15 mL are used. For rabbit studies, use 1.0 or 9.3.4 Place the vial so that the tipof the COMBUSTION TUBE is in the TISAB at least 0.25 inches. Gases 9.3.5 Run the rEeOleXas-eWd AduTrEinRg ppryoroglryasmisfmouusntd bubble through the in the RUN menu. TISAB. 9.3.6 93.7 IWfhuendniltuhteeEd OTXISpArBogwraasm uissefdintioshceodl,lercetmtohevesatmhpelceo,llaedcdtiaonn evqiaulalfrvoomlutmheecoofmMbiulsltiio-nQTMtuwbae.ter to the TISAB to make 1:1 TISAB:Milli-QTTM. 9.3.8 Rinse the end ofthe combustion tube with Milli-QTM water and wipe with a KIMWIPE to 9.3.9 `witha Open the sample hatch and remove any remaining ash from the boat. cotton tipped applicator and/or vacuumed out. It maybenecessary to Ash can be removed scrap particlesoffthe bottom with a spatula or other similar device. A drop of Milli-QTM water may be added to the `btooaaitd in the Clean Cycle. 9.3.10 Close the hatch. 9.3.11 93.12 SRaumnplteheisCrLeEadAyNfoBr OanAalTyspirsobgyraimo.n selective electrode (AMDT-M-2). 9.4 Sample Calculations 9.4.1 Use the standard curveto calculate the sample value. 9.4.2 Sample Mass Recovered F (ug) = (TISAB vol in mL) x (Orionreadinginppm -intercept) (Slope) 1 VALIDATION. EE a, 10.1 Quality Control 10.1.1 Daily Start Up Check Samples: Once the standard curve is established, each day of analysis is started by analyzing QC samples. The QC samples are to be the same as the lowest `concentration spiked samples usedto generate the standard curve. Each concentration must be rdeopnliecaintetriispnlioctatneecuenslseasrsy.the first two replicates are within 20%ofthe standard curve, thenathird 10.2 Precision and Fluoride Notebooks Accuracy: 2,3, and 5. PSreeceimsieotnhaondddaecvceulroapcmyevnatriaensalwyhseisn aanndalsyazmipnlgesaanmapllyessiosfidnifferent matrices and different reference compounds. 103 Other Validation Parameters: NA 1.0 DATA ANALYSIS 111 Cateuations 1LLI For the standard curve, use regression analysis in Excel, version 5.0 or greater. 11.1.2 To calculate the fluoride contraction in the sample, see method AMDT-M-2. s:oR7c*2 11.2 Analyzing the Data al1er1se2s.wti1htahn2in5m20u0%s%tooffbeethaaetcalhveeoartsahgteer0.oa95fnodtrhtgohrseeeaottuewtrol..ie"rOiAusntylgireseruastc"ehrmotauhtyalnieb2res0es0xh%coluoulfddetbhdeeipafovtiewnrotaegodefootufhtetihtnhorsteeeh.etrdweaaptloaircaanteds noted in the Final Report along with the reason it was considered an outlir. None 13.1 349, Rosemount revision B, Dohrmann December DX2000 1993) Organic Halide Analyzer Operator's Manual (Manual 915- A1n3.a2lyzAeMrDT-M-2 Fluoride Measurement by Meansofan Orion EA940 Expandable Ion A1n3.a3lyAzMerDT-EP-3 Routine Maintenance ofa Modified Dohrmann DX2000 Organic Halide Revision Number ReasonforChange Revision Date 6 opaCu0s2l73 9.1.3 Amendment to analytical protocol AMDT-011095.1 a cozs 73 Attachment GLP Study Protocol Amendment Study Number: AMDT-011095.1 Study Title: Single Dose Dermal Absoption/Toxicityof T-60676, T-6068 and T-6069 in Rabbits Study Director: James D. Johnson e-- Amsen--dme--nt D--ate:--No-- vemb--er -- 10, 1--995 ------`A-- mend-- ment--Num--ber-- : 1 `This amendment modifies the following portionofthe protocol: AMDT-M-14-0 specifies using bovine serum for blanks and QC check samples in the thermal extraction. However, rabbit serym from the control animals (AMDT-110394.1) than the samples. was used was used because the bovine serum blanks werehigher . Approved by: shar tudy tor Wag 2s Date c0TR7n34 OHO 9.3 Quality Assurance Unit Statement Auachment D GLP Study Quality Assurance Statement Study Title:Single-dose Dermal Absorption/Toxicity Study of T-6067, T-6068 and T-6069 in Rabbits' Study Number: AMDT-011095.1 Name of Auditor: Kari Rambo This study has been inspected by the Quality Assurance Unit asindicated in the following table. `The findings were reported to the study director and`management. Inspection Dates Eom Io -- Phase 11-15-95 11-20-95 Final Report Date Inspection Reported to Management StudyDirector 11-20-95 11-20-95 ' Lie Le QAU Auditor 2-2 95" Date coir736 erring, 9.4 Key Personnel Involved in the Study CoRVSY FOSY 3M Environmental Laboratory Key Personnel Thermal extraction Jim Johnson followed by analysis using Orion ion analyzer: Deb Wright DReicahnnYoPulnugmbmleorm Analysisofliver extracts Jim Johnson using electrospray mass spectrometry: Dave Christenson a`nTahleyrzmearl weixttrhafcotniosnelfeocltlivoeweedlebcytraondael:ysis using Skalar segmented flow Jim Johnson RDiecbh WYroiugnhgtblom . Deann Plummer Documentation and Jim Johnson Reporting: Rich Youngblom Quality Assurance Unit: CGyanltehViaanWeBbusekrirk Kari Rambo c02728 Treesn | 9.11 Data Cozi39 d9e.1t1e.r1miSnuemdmbayrtyhearnmdalraewxtdraatcat;ionugfoFl"lionwewdhoblyealniavleyrsiass using Orion ion analyzer. CoR740 G-- Summaryof Combustion Data - Liver AMDT-011095.1, HWI 6329-152 As Referenced in Final Report section 6.0 DATA ANALYSIS TotalMueganFlpueorriDdoesien GWrhooulpe*Liver ng Std. Dev. Control Group 12.5 + 2.1 4.0 mg/kg dose (T6067) 12.5 + 1.6 16 mg/kg dose (T6067) 14.7 + 4.0 40 mg/kg dose (T6067) 16.5 + 5.2 Fabric exposure (T6068)** 15.7 + 4.2 Fabric exposure(T6069)** 12.8 + 3.7 *Calculated as the mean of triplicate samples from each of three male and three female rabbits. **Administered as a 10 cm x 10 cm pieceoftest material (fabric). CoR7i2 Gaaaul L122 28 0 ivveerrsbplkeatnk iivveerrssppkk2s iivveerrssppkksd vieverrbsapnkks:2 FsE2sraiit2 FsF2arriitaa FsF2sz7riiso3z LLiivveerrbbikk 21 UUvveerrssppkk1z FsFzeraorest FFssazrriaasga FFss2a7i1a32a FFssz2r7iiest2 FsFasr2z73i1a Frs2sr2a22 FFs2ar1at12 PFs222ra7t1a FFs22rr227123 FsF2s0200088..21 FsF2s820r81s.t3 FsF2sa7r1iss3z FFsezarres Fares pAcotuma.l Apveormag.e Liver Wlheolre % inliver inliver burned weight reviy 97% (o1W1nW0) (WW) (g00r11a32m45s) (grams) e8ss% 0os7a2s 0o14r7 19077%% 220603 o01a2r8 95% 021585 o0r1i4z0 001647 0183 0011314 eeseit aottees oouws eees 0021078 ow o0i1em 776s8 0o2s5e0 0o12z8 ooa7n% 113170 00110206 0022218 020 o01i6: eeoss 0012m0 o01s2e4 76104s 0011720 ote ooeess 77144 ooits 0183 0o1i3s5 55777 o0a178 ooums 757s7 o0s2s0 021s 0187 00115s0 0101 77266 eas 0o1e4r2 ots o01u%s 6s2209 o0s2s6 017 0o1s6s ssezz oastse 00114 sseozs ol01e5s5 0160 001137 essess o02z5s5 0211 020 001137 oi 26211 ei oairse oles oi o0i1s 031 sseiss aie TiontwahloFl-e liver (ug) ReTISZLXLS Dosage (mg/kg) 101 oo 13s oo 80 oo m7 4p 10s 40 13s 40 ms oo 129 oo 11 00 143 40 to 40 Page 1 COR7AQ Snanet L134s2.a8 io FF5522880000..12 FFs52278200--31 FF5s22712244..32 FFss22773377.12 lFi5v2er73b7in.k3-1 llvveesrssppkkt2 Fli5v2e8r0s1p.k13 FF5s22880011..32 FF5522772200.12 FF5522713230.13 FFss2217333323 FF5s22778888.21 LFi5v2e7r8b8k.31 ULivveerr sbpikk12 FL5v2e7r3s0.p1k2 FFs522773300..23 FF5s22773311..12 FFs522183012.-31 FF5s2288020.232 FsFs7217414..12 FFs522171344..31 FF5522173344..32 F522177744.21 Fs27743 Actual % iPnPlMivFe-r fey (0.W4W32) 00.11658 00.215857 00..119623 00.114855 89% 013.1404 8916%% 00.097234 0032782 00126512 00222056 00128224 00.127098 00.115645 00.370610 110181%% 11.0082 0032378 00136830 00.210620 0025828 00220474 00248514 0022273 00218873 00127145 Average ipnplmivFe-r (WW) 0253 024 0154 021 0228 0205 0166 038 0175 037 0327 023 028 bLuimveerd (g0r1a3m8s) 00111228 00111%9 0011s2t9 0011427 00..112334 00..114394 00111192 0o1u2s8 00113303 001132%8 0011433 00112415 00..111460 00..116600 00111233 00115s8 00115088 00111500 0011524 00115512 00111416 o01e8s 0011232 Wlhiovelre (wgeriagmhst) s55s.a4 a52504 882200 262s5 625 67877 678677 668877 677 667777 668800 680 578 57799 590 95000 771s9 4751s9 448555 sseaii 7s1a1n 770111 TiontwahlolF-e liver (uo) 140 168 5s 207 187 139 "3 184 103 257 148 138 160 RPTIS2LXLS, (Dmoasrakg)e 40 160 160 160 18.0 160 180 400 "00 "00 400 "00 "00 Page2 oRRGE L122 28 i % PAcMtuaEl iniver FFssz2r2iz21 vy (o0Wu3W) FsF2erie2ta 00220110 FFss2a7r22923 Fs2600.1 ootis s 0204 FFss22880003.32 00114883 FsFs2zrriieez1 Fs27t6 0011675 oir FFss2z7a2se.21 0a1t6e6 FFssa2r7e2r8.t3 P0r21s FFss2z7r8a7r.23 o0i2s2 ULivveerrbbiikk21 00225505 UUvveerrssiinnda21 1ea% 111136 ssaanrizry 003;80 ssaa7r3isr-1a 00226058 sasreraassaz oatmoar s52a7m3e61 2736.3 oolsees oss s52772266.12 sare 0o1s3 01m ssaarr3a2z21 o[ar us sa5r27a320a1 sams ooatne 0121 U52v7e3r0s3pk Uverspics 08s 0081223 08222 0880 UUvneerrssppckss 01s02e%s 112113 UUvveerrssopxks? 080771889 212892 Uverspks 083s 23 ApveormaFg.e inliver WW) 03% 020 0212 073 0181 0203 ozs 020 ot60 0150 ois oot ver Wvheolre bumed weight (0g0r11a1m%5s) (a772m200s) 0o1m27 e7a2t0 0oo1t3en5 z7e&111 o01u105 771111 00117 3613 0011251 677093 0ow1s2 779885 0o1i0 M7122 o01i47 72 001112s2 ooitse 70 001212 7T0O 00117 S53350 0011610 7s2a0s o0u1s7 772298 0011825 774444 0oi 1% e7s4t4 0011103 sseit 0 O62 eeos 00111630 84s 0014103 0o0i2e 00112405 RPTISZLXLS Tiontwahlo.w er Dosage (ug) (maiko) 27 Fane 1s Fane 151 Fae 17 Fabie 153 Fame 15 Fac 21 Fane 108 Fabre 17 Fabre 12 Fano 104 Fabric 124 Fabre Pages 900686 coz744 9.11.2 Summary and raw data; analysis of liver extracts using electrospray mass spectrometry. DTihriescdtaotra,isanlotthoruegqhuisruepdpotrotrievaec,hitnhtehecoonpcilnuisoinoonftsthaetedStiundy Final Report detail. Section 6.0, and therefore is not discussed in SCHOOORTE sETaeyo OR-- FeuvogrnormtsFasovranAmount UMaoatrohuormssa:netre PPR SPie JJ arConeaioAnslA"pFags O .Clndeusn STSnoegteaoCootuenCuama Tat0in034 Pe wis (ss 5VY P GSH Stnplm epse.aksser Corea (ted die to rCeogloasid `Screening. Caoes a FaseVG200 Emcor MS oySgav NE CTW obfeHeO nCw omases pluated AS Sei WIE J `SJNil Se Wiss Owen | rms no wo wo m mo ow w FolmE ww AS 8E| m Hmao ew w owd w ww EEE (boraadte J mm eeoowwwo NnWowo wWow wo [EE - [rFaotse m jec w w wowe 3ww Fae e m [EEow w ww"oo ww3o WE- smote azar Rowocroicraanww1sratucohbatnaoeco7a3neoe5bsyTsoinneo gophaimdop ntlss5ieo 1 emds blingo AMDni m e1iess Set y 45,pTBt oe e 43Sg AusOd coz746 li | Lay reo eo eae | eo m [WWiRe13622,CM9P5DLi1Sa80z <[\ | || wow wr |i we ae wo | ST 2100 sna- rwee rea) om 202 5<= wron 1060 | ze Ed | g ii fr AU JL a eA A | oIemRay Te TFTE ee - =| i wo J To " vm, EO ae rl J { | mal | | |i I| CTR | 3 ERIN [Hw # 6329-151 sfezcwoLiez || || hh 4 a wo oo s- no | ere e ow T &g |) JUVI | | | 1owes Sn in 27" PL |I hvoerd ||| JUL I 1 l LL | Tr Si henaesm Ay || ||+ d9e.1t1e.r3miSnuemdmbayrtyhearnmdalraewxtdraatcat;ionppfomllFo"wiendsbeyruamnaalsysis using Skalar segmented flow analyzer with ion selective electrode. CORTE0) Gratin + RE: 6329-152 SERUM SAMPLES AMDT 11095.1 Date of Analysis: 8/22, 8/23, and 8/28/95 Analyst: DDW SE SkalalDam The samples are burned in the Dohrman at 950 C using 0.10 mL of the serum. The gas is collected in 2.0 mL of 1:1 TISAB/Milli-Q water. The samples are then analyzed on a (ISE) Method. Skalar Segmented Flow Analyzer using the lon Specific Electrode TISAB buffer is added to each sample as it proceeds through the system. The `sa ion mple then selective goes through a electrode and t he he arteefdermeinxciengelceocitlrboedfeoirse mtehaesuporteedn.tiaTlhbeetswigeneanl tihs e amplified and related to the fluoride concentration. The instrument was calibrated in the ranges of 0.015 - 0.15 sn ppm and 0.15- 1.50 ppm plotted using the inverse fluoride. logarithm The standard curve for the option. The standard curve high range for the low was range is linear. All standards using these curves. All and samples results below w0e.0r0e0t1hepnpcmalacpupleaatredobnytthheerSakwa ldaartasoafstware A quality control standard was analyzed every 10 samples to check for accuracy and drift. - Raw data is taken from the appropriate calibrated rangeof the Skalar printout and summarized on an Excel spreadsheet. The final results are adjusted for the collection volume and any subsequent dilution.s COR753 --------- Ast) 59 - SSEURUMMSMOAFMAPasLRzEsS1Y52 AMDT 110950 UStwatCalaTsesan Dmlcnoduirosmte BoE UR 3 HBBoEauLl aa0w sooenn asonew ooSmwp HBamw0% oewa aonm oomm Dulcooduri:ime BrWosennaa BOL ass oeoohk le on eoiwmm oh 0aoonnn [EHmEiH 1D os le on Doalroulrsie B Bmaodi em n6 FE eoemwm eoiwwm oan aoinnn an BHEdoh eons ookm on Dulaordowrrosmte BBBaoaelriain BHHiEmade oilpme ooommn coaowwn ooonns eoimnn DucteGdrovleos ro m BRiaemlimal0e%e BEL 0eo08saa ooonme on RBeol ma ooam oenm Delecovsesine BB Bloia mmBIimC 04 ie oe0n amaeen aSoenw ooonnm + Avepenesere te. DOW sams TC0PAY ABLE CORTSRL.Ll 2 ow 2 SERUM CURVE 2 CA7-R2L7-T9O5N Cw ES Skalac Qute HWT (229-152. ADT 11015. SpD e m RSeuwlst DfITlIvAD aD aSLoFoCOnS Sed FCCOSoSon Gp SMpiukmed F) AMwase Reored Re%nny wr SsoKuZ Ska 000m6 om 322000 aooooosro uuMm0m oo om isi SSSkkiozers 00o00pss 02200 ooamwmed masommm ow on im ssskaeeis2 ooommm 22000 oooommm aaa0w ois on new Sskkiio012 O0101 2200 ooooor Mi0o0 om om om Ski03 012 20 ook io sSSkkiiineuesz oaolnls 222000 ooommm nl1eu0oo ow om sx sswksao:l o0m3 Sk:03 0m 2200 20 oooor ook 30x0000 om on wm sSkwssweiz 0oa 2200 oomoed Wseoo 1m om SKs03 0% 20 oor smo SERUM CURVE1 (CARLTON) 7275 ] | [2 wl -- J -- TTTTo | fw T 1 T11 IH fawTl TTTT | TT ~~ TT Boo T 1 TT i wS lL --1 T Z | foe Boole TTTT +R m woe s se oeTomTwmT1m]ie | Preston seRcavacRPT oR758 Paget 3 SERU7M27C.U3R5VE 2 CARLTON SBue eRSmeune DIfToSAlD LSSioceon FCoom3eeSn SaMruds) ReMoaewrd Re%nny SSSiKeklS: 00o0mm6 0Z2o0 oooommme MMeemoo oooeoost ooonnu hiimmee STAOApDDyEVATON: loiranmas SSSkEhi@eeLas 00ae0% dG2oo0 oooommm wwsoemms 0oall0eo ooonhn iiInmmk STAOAhDoD,EATON: otiian SSSkEa@asI: 0o0mmm d22o00 do0eo0sm aaemel o0ol1nis oGollnss llleoeww STANDARrDsDEVITN: Slaoinns SSSKkiOiOwdL oo0l1il0 d32o00 ooommme le0ebs oo0xna o0bph2 easeee STANDARDrDsEVATION: Soinoe SSSkKmiEom a0olmhs d220o0 ddoooo imwn0oe o00%ml 0oa2nn8 un ie STANOMaDsD,SVATN. oosise SSKkIiOnLz o0m3 SkEos om 32l00o ooooomm Hw3e0os0 oGoekw obasem ierero STANDMDhDsE,VATION. 5oi0ss: SSSkkKinI:s 0o0w%% 22000 ooommme Sms0wo0e 1i1%m2 0oCrm3e a7em STANDpArIDeDEVATION. oooems mSmERS EGTeO TIT | |e l|}t or IioFi | | y y=07212x+0083 | T| T; R'wT 0967 TT1i ] 1 7 T | : | | T| T| . 7 T Ii I T | | [ee sereavac sum COR7S jo soni ouactiosnm mans AODracnaAtkmihom:eo5w0CO8S3K3A0LA2R0D0ATAIWIDATASERUMSSS12D1 Seple Samp CSaSnd RSeREl oe o DITISKS QiS(oell)ApFG. B`SEwCioOn FCoCn9s35AdSnM edRM ecowrTd R :3 mTaew 1mm dwWoe wowm SCDo0o SSsemmnaal ooonmws oaommm wwbewm DTDoo ooSSSmeaammaedrr ooommn ooonnm lamemm bo Smear ow am ow =a= s DBWoo oosmSmamana o10wm% od0mw om me CARCI ==Ss is bo sSaaarnm ooomr 2B0o oonn aima = a o[ Bbo iamtsa oooinir BBIoaohnn dddmmk oooeommm aaammwoo ooanhmooosnn loonmme 28 n on amme &Sn wmx oooinns on IIIooo WGubbw SisMmw doomow mmmooo naneee ooonnn womene Baw im H3 Biha 1 obne ow FI a So Przel! B 5 e mew oowm B0ooaoew xie Lhe3 oo rama 005 0 ow om 5 Cw Pat 3 r A Soe Soe Re sans era ---- So bed. Reed.Fn BnBoo oorhnmm aoasons ; 0Bnoooowmnw iiibem XWBooo pmhaeanm Yo em ooonnus aor nnoomwoom iiimpe ook a H ATR nWboo omawaemn 8 ooonin ox ax 2w20 ommol oom IeR waomm Sh om saaewms mes oeosnh ok ooounn on wx ourr voem awmees oooooo pd bm oa 2 FR 0ow 0 an b15wG oemm aawm aonks oewn wm i5a eT ran e pHf 5 m Womom iLah oomm mdeess eokb eonn eorx 5Sa ommeaxh oaoan ki nx on 1n2o0oamaew 4w i%e moe mheen cbee oonw uUwE now on 82 55So pFohaommmne ooo0io0ons6r nn20 oaowoo nwe wnaoinne & 4 por a wah 0 otme I ow oon aw = G Go m mma oinn 0 eoown iiyo "F ==E - m 006. 20 poueo2w im E SSsey ans s STL 5 F8F8I opammmas Bom fibibusd & B BBBBoooOtoeaoWo osEolmooamaemoaaoawmmeoe aooso onooowoeomooeem POToom eli am 3 ope " Bow Dp ope o Fe Bow Bom FF EFRI O-N PPooeem a=Ei2d Ww ue BBoOnoWE Bowe ew wm ae ae os es num en ;PiOTm =E= LEu&S B Bo oo om m om moeoowr omom B g= 23 g === a 3= Page3. g ET p riann sI soounrsesane Sat Ren Rey YA LC8 Can PPCooommme oE eoou omm PPooEm ow oBwomow 7 Sammie PPPPooooEEEE * `Standard 00 oo me fokoonn ooomnmooun Eooooammwm BOER uw oat 1% ie om 1176 SSEERRUUMMBBLLK1K2 0000ss 2200 ootwo 1o0m6 orPPooBmow e.miE 8S5n hEson 0004 ad nono F 20 00Tose Page 1 MM - = - gg== =E B&E 3f erfge isons SDA OySe ROY co on n Bwo oemn Noon ooonnn on nBn0oo ooooonk anoaonan Xo aBo nohmno "hw oownno Ba nnnooommoooSoe o [I A m FT forpnis ow nWBooooeok aGin owew oWwm a0s en ow sE 8ow m o Fr oooinns on omR BIoooowomha Boab on Ioxn essmwe aoawwm soohsh eeonnn ow he sF8R0 omTaaw we ooonhn 1 om mBnoooooeak keGdRm Gsaemn ae dme a0bn8 o0enn ow 5S SoT mwim oowoio 8 eomom ooun nmBo ootee noe sw a am me a es am 5PA0 mmea 5 mn ooonnn on BBooooonma ieesse on nou an 5aa@ mmo"nanhe oo1nBn ew n 0 oon wox w ==S g2 oa mmmmms oonn w nowooea =E . a88 ow Fa 002 20 aeo2l os ggE sexs Spl Soe ontad emt ReonayfDIaTt OySa(nL: pou OY20, FC535 CM {BeesReamer oaao smsicaoannn no er ao00nns on w2omn Wowol a1wm wodwmm daaewwo im am awe ooools ooobhn ex me o5 oans bn oh on 22 g g83 Paes E= == 3 g Epiayn eve enn eons Sol Sa % DUTISAN QS AGITHUCYS Coy Nas `LCEoaZBmEeoa ow ow Bdgn ii EE ES E ZiEz LPBPoEtraESlmE1el2e EER 1% im lw. 2 pomow g88]= Pam OB B@mEmEEL os og SPR623 2un SwP 2o50-1 010 ooun 20 0200 010 00100 22 004 00 01s u2s% oooomm m2000 o0k0 om new a0n2 asem = == 8x VCashINE A, 85 ix ao 0 ow i pi B Page 1 Soe Asons oye SkSoodReRoneyTol (0) EE ou ci = Reamer ei am w un[oo rmEise Ho a oo00ons aon 000 ooaknb ooomnw 200 on on %B whae amme Dh oo0on0r aw in oes nn200 aankon ooonsn 0 heVmean raWe0o PH oo 00w0 owoonw ooonww WBBooo sSSweealrn oaolins i Bix as 2B20 owooww 00 on aSimkm dn aaoemm mawemo oboees ooommw ounm 5Bboo sSbeaunsx oa0o0nrs BwBooownm iiIwnm oomm bawe oass oolwe heme i85 ssaVeann oooin s$o0 SSooww on 22Wooomm 4aa%m ooooamn dadomo aoaese oaonxn em 5a SBiiaxx ooax0n oor BWwmoooomwok ds1mk% oaewmm mmeoooode uonn nwre won in 3B a ano 3S a mrammaa ew aoonnn in om 00wonooww ooahan == 8doua reoamnis ioaonn 2 oown oons E== 0 Fa 00 0 00 om Pouez = = eeSE Ee ates Re I H ES g3 sSs - & = 5 8 = H os mm pinn, oumeea 5 Sota Ry ISASCO Str AG PPPooommpool ow om Eo P= PPooommEEe uoEoomnnoonmom PBpPo Ho ooOooeTR SEmEdOwsSinBRose ooonnEoToomm L "" `SERUMBLK " `SERUMBLK. 005 00 20 20 or on 09 oer RCS CoNMT 22g== g= a B 3 oo Sa dx owmm oin 200 00 an om me ow en om ff8o Law mx 006 20 ow an PF 2 - E SpT l SweL SiS n m RD eh E RI emyut isons ntG(SPERpT enAe ERRT pCC Mi Nunooo haaemyme No me ooooon WW 0 oowow ooopnp qm uNBooo hmhmnne ooaonn wn u i 0 1% BB0 ooooonnw aoonan nook on a nan Bh aownno an B0 awow an oasemw uPnIo hoes fry 5" shexn ooonrn on Booonoom ow aSimhm oon em me oe en uw B wooowaa ooooon wm a wW2 oeomolm 11T%0H sseemm Gaaeew ooohs oneonn Mm i55 mwYioammn inSowx hoitno on w2Wooeaoe oSswee oetmme wmdeeen beoeeb ooowwn borw "5Samfrexy aoionn on 5 he nBoooooonww oiiwnn 0 ow a aoa hn n n ooWon 8 aw nnooowokon Se on a1 " aGm en nan PooAm "i on n0 omooonm 3aSes ==2 = = 5 isons Se SasS Sd it RaelerReyme y TIGSoaQoSi BF aio 38FC C93Co5nahiSMipRMamaer Rory a"ooooawm yw ooonnn a Bo FEE oEeoTman BF BooH oam B Boo owe ooonnn ih we F nooaE tke I 00%S tammTwoanoeIoun ooe oe onom 5 BEoom mm 3 o5io woe nFHBR ooooooknmI ude noomtewee a cuwe oonm geee FFV [III m Bowe =oooo oWn w NFBI oooonk BO iw am ome en ow yom " 2 xB) a 8s= 283$8 = &= rors 5 EER svar eE asc Salt DITISAB GY Som Ack EC 3 ConMa Me lPPPPIPPCiCoOEoomEEEEpEmRmBEeBEREoeEEEwuEEEgBEEoE E23 BERoeREoLm RE ow R SRAM 00 " SK a2 SPK 250.1 009 ox iJ BE -F 2a SSPe2n5a02 o0l2y1 0 om in g 20 20 M0 010 Am 3% oo 00M 200 200 01s 00 on 03 jew gsm m20 op010 4m3 oooomn o2o00 00%6 0osw nimm =< = = BE a 9g - iE c Swe Sk m See m B dr ew o ney E a R s(enOas ptRroot Abe wB3Nooo ow [+w3r PLhEooTau R P yB3OT o=m wmwoown nB o no owMmoWmie omam oaawn ams oewmoon PF3yA ooeEmme `FRI =&o5n 24 B o B Boto weW n oam em a we aw we en em ow ow e PbA Po ooam oo"ore = IBBBo ooodwaee lalemnootonommooaaownmnooauonuen ooemen euoweee nooo 5SFB E Oo aTm 3m o>0in = nono 0omom emw i bPi o om oo FA] o+-n = h hhLooouom ooo Io om B= 2aaaG3 TpnRee w"wonw [4 BBho OoWom0 maoaanm an eoe oma a = Sdaa5 wmmmma o==o B BBooho mo ameoomm mmeoeBeEe oooswoomm m B=F3B Page2 - sens com EE a DRTEI NhySElR CRCEMM 6aa eBamiuxx no hm o0o0ns on n00 anowwn o1insa Wo is nnnooo n en hom aaann0 00wonookw ooonam bio te oom HBioN beeaesn A bn o0No0ons on nowoowh ooonnw n Bwoo oael a00n BBoo isnna oo 010 o0ommw am oIBmn oomm aGwm oom mo aoaswk eoonnn ehonmm H oanho obonn 0m Im oon Gwe om ol 2g g= E 283 E & panes DCIhrmA,enstngSoaur1ektsusm rasens Rime MAIR WATAT SERUMA ra e a e DLTOyS(IoaPSLAAA)AEISSBeEeCCn Fo Co7it c SMdi a Rem Rre y :DP: osostmaaw tm woWwsowol imn mmom CSo omoeoamsnnoooenoaeomea boom ono oomm bWBoo osmSeeaaanms [=r of0Rea% Roo0nd 8a m g= "Bi osoemDait me 0% o1Fn%o on oe nFEoTeE 3 === 8aSg 5nwo ommem 3 mm ooann ow 30h ak ow wH BBooooawllnN3Sdkw oawummm Gm aahewe We eoonsn 0h aaepn n0eI% 0p um = 3 3NN o a hrad ro Thee ooonons Wm BFBroooooomn ER etne o F5R ohma ohn oo-wn B0nooo0n0ooaona P ! - pe : rss RbSBrR p bSoopl SuSnduetTopReam ARLT emyO Trot SoinmyCa al LCAT C T2ops oNBa35 n I Wo bH n ux oowoonr on 00nowaoww ooSnne no ow 3Xvoo n sswemiann bu ue oooonn Ge oem n2Woweem iiimbe aoomm Gaemw aoask ooennp Lobe o i smVin B a bx oownno on n02 awoemw osapmn ew me on on um sao anmm Bo ws aoaoonn 0 0oeooww ooonnp ow a bBPoo AahHmms u ee aawtonn om Bnnooowww ooonnp . 558 epfosss 5D twa oo0onr 00 w0 omoown oaanen 0 on am ew ew 5swoasE mnn ny oaoin on W20 omoawm k lne s mdw omweem aaonsn an oaannm an oaennn 0% ae an ao" aa aDnxuo o0hown om Boookan aipm em am os os oem == EB an Ww EbyS8 04@ amwaann poari 2Wnom wom eaImm saomwm elniwee ooanmk oaawn em a B oaez sexs |S S ede eSruan(tRen =a TDGp pa. Reg, frate m (on I s sy o @@ emBBixx Bo as o00os oooorr F 0 owTom 0FowTon annoo ruhaso oouousn u [OT 1wwoonnow aoimn 7Hnoo srwaWamatns no men N00o% aor 00 20 ooml oiwn 00m oemm Geem ooins on om on0o sWbnair a9 oh wno w 1 ok as om me ow oamn ame e a 8 ==g 83o EEg pages B 1995-08-22 13:41 OutPut of : 95082281 Software :. version 6.1 c1990,53 operator + Dow Date of the Analysis : 1995-08-22 0:04 Analysis Pile Name : C:\SKALAR\DATA\HWIDATA\SERUM\95082281 od This ASHoeyTon6j2Co2ur9v-e5YW Caulibon CTalluiobrriadetio1.n5order = Inverse Logarithm stope i 5s s0000s Result = 100 [x=-"5e=1] xcL 5 === Scclooorrprreeeccottfeeddthvveaalluueseleocoftfrottdhheee scaomnpcleentration 1 aa2iz= -0o.l0o0o0o0r0z . 20 = 1.20078 CFalluiobrriadteioLn order = 2 Correlation : x = 0.99917 Result = a2 * x* + a1 * x + a0 aaa081==me ~T0oul0o0o0o0z0s 0loossi . sampler Nuvmpbser i+ ysA1000 WSaesmhple TTiimnee Mr Time :| 15200 sseecc.. 1. sec TsaPkoeciaulp needle Hoight + : NSoinnegle 70 mm. Diluter dnieleudtlieonHeiFgahcttor :: 8100 mm Redsilaumtpiloen Dilution Volume runs :ii2.5 1 ml. URosperrocfesi.le |: No . mr wns COR773 2 1995-08-22 13:41 Fluoride 1.5 PSiagtnhalnumtybpeer DesycsotleomrNumber diReLsuatmeple ddiilG oTuhtrpeusthold Window event Output of : :: De3bubbled :: 0Yos i: HNoo :: 04095 : Off Fluoride L 5512 ssTTaannddaarrdd :: IIggnnoorree 8834 ssTTaannddaarrdd :: IIggnnoorree s565 ssTTaannddaarrdd :: Igno0r.e150 8578 ssTTaannddaarrdd :: 00..360000 88910 ssTTaannddaarrdd :: 11..520000 ODridmeernsi:onInv: erPsPeK Logarithm sttrairgtgerValLuiemit :: Peak shape: 5108000 DSeUc Pointed oSNtdArt iiggnnoorree :: 16200 SSeecc FiMelatseurre window i: N7o5 4% Rfeogremnuelraation : No output: sear PSaitghnalnumtbyepre :: De0bubbled DesycsotleomrNumber i: K0o aReistaumtpele ii NNoo QdlG Touhtrpeusthold :: 04095 Window event : Off 95082281 SUTTNG COR774 2 1995-08-22 13:41 output of : 95082281 5812 ssTTaannddaradr:d: 00..001350 5843 85 ssTTaannddaarr::dd sTandar:d 00..003600 0.120 8376 ssTTaannddaardr:d: Igno0r.e150 8589 sTsTaannddaarrdd :: IIggnnoorree o8r10dersT: an2dard : Ignore sDtiamretnsViaolnue: PPM : 500 DU PtoraikggesrhLaimpite:: P1o8i0n0teSdec eSNtdArt iiggnnoorree ::16200 SSeecc FMielatseurre window i: F7o5% fRoergmeunlearatio: n cd:=: c3No output: #.4888 Suosier COR7IS @ 1995-08-22 13:41 Output of : 95082281 Pluoride 1.5 Pluoride L oon Pen Pos Typ Ident Ch Result 7 Time Ch Result ? Time 2w1 t aiw InitialTraWcaesrh Drift 33 3 10..406643 11468 3 ow 21605 4400..06075554 384 4 0.6770 00 0 54 5821 83 standWaars1dh Standard 2 33 3 00..006673 0073 standard 3 3 0.091 763216 44 00..00308545 1098059 44 00..0058735 00 87 8854 9, 56 sSttaanndadradr4d5 Standard 6 33 3 001.112078 0.157 11423557 4400..01910771 1611 4 0.1517 00 o0 1110 8887 12 89 ssttaannddaarr78dd 33 00.621788 standar9d 3 11232 11976806 4400..42155225 2136 40.6046 o0 0 13 a210 standarDrdif1t0 33 111446860 15 w Wash 3 0.063 22438160 4400..66786130 2727 4 0.0055 00 0 1176 uu 18 u SSEERRUUMMBBLLKK 21 33 00.009789 SPK 62-1 3 0.097 32080377 4400..00471308 3185 40.0730 00 0 2109 uwu 21 .u SSPPKK 6622--32 SPK 250-1 333 00..113231 . 33533693 0.133 3713 44 00..11204868 40.1245 000 223 uu 2.u SSPPKK 225500--32 33 00.1226772 BLK 3 01105 43086838 440.0.22445838 4237 4 0.0856 000 225 a 2278 wu DriBfLtK 33 1011405974 F5271W3a-s1h 33 00..009643 44548186. 4400..06677332 4823 40.0055 00 o 3209 uu 3 ou 5$25721782-32-19 33 00..008882 F52715-1 3 0.084 54191338 440.0.00568621 S5426813 4400..00456072 00 o 332 ouu 34 ou PF5522870398--11 33 00..009889 F52724-1 3 01050 55861335 4400..00754834 5991 4 0.0604 00 00 3365 uou 37 ou PF5522870317--11 33 00..008859 52729-1 3 0.075 66314603 4400..00552877 6515 4 0.0405 00 0 3398 wa 10 ou DWraisfht 33 01..046634 SPK 62-1 3 0.095 66962930 4400..06075554 7042 4 0.0715 00 0 4a2 ouu 43 ou SPSKPK25602--12 SPK 250-2 333 0001..211536716 77329229 7566 4400..11621122 4 0.2380 00 0 4454 ouu 4475 ouu BLBKLCK 33 001.008818 SSPPKK 6622--21 33 00.1110031 77971471 4400..00547490 88206972 4 0.0794 00 0 4498 ouu 50.4 SSPPKK 225500--21 33 00..221053 Drift 3 11475 8441 4400..01892597 88769127 44 00..62800977 00 00 5521 wu SPK 2Y5o0-s3h 33 009.62433 s9o142a 440o.looss a 53 u SPK 250-4 3 0.238 9318 4 0.2241 0 Page 1 of 2 Coots CORT76 av 1995-08-22 13:41 output of : ssos2zs: Fluoride 1.5 Pluoride ou I= Pos Typ Ident Ch Result ? Time Ch Result 7 Time s55 ouuou FA 213BB3LL1KK 333 000..000878775 ss504a4ss20 4440.b0.0l05o31s87s2 P2781 3 0.068 10017 4 0.0161 0o00 as5&5 uuou FFS55222707303120---111 333 000..000886357 P2741 3 0.081 111000331643753 10715 444 000...006884837707 4 0.043% a &6 aoowu [HE Fs1D3Wr4ai-sf1he 333 001..004866632 1i110218433063 444000...00e08783d%7s P2174 3 0090 11417 4 0.0617 oao 8&7 u u SBFESSK2217216922---111 333 000...010909402 11111173384%55 444000...000766074861 aa 8%Touua 7a seSSKKK2866022.-312 333 000..11243433 11133214108%4 444 000..33039a8916 BLK 3 0470 1364s 4 0.1850 : 0 77755% a 7% Ps28DVr0ai3fs-th1 333 0010040376353 11132329839%05 444 000...06067059543% F716 3 0.095 13345 4 0.0601 0 77788.a4u 8u FPPSS2a221718677111 333 0001.00009597 1113335835%2: 444 000...00059892580 PS2135-1 3 0098 14045 40.0738 88auuu 8u BFPSSS2227771323662-111 333 000..000968338 111444332729015 44400.0..000458776358 F521351 3 0.001 14745 4 0.0430 o0 85owau 8 SKDWr6ai2fs-th1 333 0101150006433 1113543039387 444 000...008a03s898% sex 62-2 3 0.140 15430 40.1338 0 0 8930 auu 52 w sSeKk D22r35i00f12t 333 001i1.33360%48 1i1s53e90s76n20 444o00l..383e00e00c8 Vash 3 01063 16213 4 0.0088 oa WE Iw Runout Wash 3 0.063 16447 4 loose a Page 2 of 2 -oTTEY cor? _ 0.223865 Calibration curve of $5082281 Fluoride L CF em | i }: i | /yd ye / || ya / oan L|i o odordeerrr: z2 [e-- rrioessy 20|| ovoreT cozirg A Calibration curve of 85082281: Fluoride 1.5 | 17087549 EXTENT NOTA 0 06317MIENEA] yd y | |: | / /A / 4 | | ||eo 0 Order: 1nveerrseetLeomgearrittthmnHeasured ss:aWmm os 02779 aon |ill | | all lag 5 - lay rl J er Lal |] | .. | [I pr Escbit | Fivhelo | OrtlPEait pene1 4 = Loc.) Co2'781 El Rau data of 95062281 : Fluoride 1.5 ass CIEoEo FTTH65J 5 WY 740 [IPH EA] - A : 3 I|a | 445% $44 C0,o fl 1 . 8Ap ud A. ||sfg 0 EscoE8x9it35|FiHelp | Crtl-P=cdit peaks 1 Tine 13935 20044 CO2782 2 Rau data of 5082Flu2ori8de11.5 ss Pathno: 3 TiEne: EKEKE Value: MPFZEEN Delo'(Z] 1| 1 IY al | ; | | 9 1 I J J | be, ARHu?45h " |[o ho Te ho] CT o E 0274 83 33 1995-08-22 17:22 output of : ss0822c1 Software : version 6.1 1990,93 Operator + oow Date of the Analysis : 1995-08-22 13:41 Analysis File Name : C:\SKALAR\DATA\KWIDATA\SERUM\950822C1 SAwodBl1a0l9a5s.) SHeeWCcEoon(nC3tu2r9ea-e1752 FCalluiobrriadteio1n.5order = Inverse Logarithm Slope cas aaonn Result = 100 [x2-52a] x5aC== SGclooomrpmreeeccotifeaddthvveaalleuleelecootffrottdhheee sSaommpBliemracion 1 aaaiz0:== -10o.9l0o09o0o0%70a CFalluiobrriadteio1n order = 2 Correlation : r = 0.99910 Res=ua2l*xt* + a%x1 +a0 a2ai0z== 00.0000002030 oloceis . Sampler HTSuyammpbpeelre Tine |`+1 sa1000 30 sec. WMTaarkseh upTTiimnee |[1s1i2n0glsseeecc.. snePeedcliealHeight |: F70o.ne.ma. Diluter nddeiiellduultteiioonnHeiVFgoahlctutnoer ;; 2180.05 mn mi. ReDsilauntpiioon runs ii1 Ruesperrociesl.e :: Ho Lm 027" 84 3 1995-08-22 17:22 output of: Fluoride 1.5 DPSeiacgtonhtaolnr.utmpesr :Y: eDe3sbubbled aiRSeytssuattmoepnleHusber :i0o iio aVaiiiGnidoTowhureetvspehnoutltd}|| o04f0f8s 15o52 sssttTaaannndddaaarrrddd i:: IIIoggmnnooorrreee 5256% sasTTtaaannndddaaarrrdad :|i IIggnnooorreie, s 9788 sostTtaaannndddaaarrrdad iii 001...362000000 OD8i1rm0deenrsa:itoannTdnav+ reaPrsFs: Loga1r.i5t0h0m PstatraaikrctoesrhVaaplLeuienit |:: P15o80i000nteDSdUac Nsneat'aasrutraii'ggwnnioonrradeow G1: 20750 4sSeecc FiREoelfgtaeeunrtearation :fiNoo output: meas Fluoride L DePScaigtonhlaolnrumtbrepre :iDoe0bubbled lRSeyussattmoepnleNusber iil0oo WaaiiilnodoTowuhtrpeeuvstehnotld ||i 04095 off ssoszzct Ed COR785 1995-08-22 17:22 output of : 950822c1 3821 ssTTaannddaarrdd :: 00..003105 8843 ssTTaannddaarrdd :: 00..009600 5865 87 ssTTaannddaarrdd :: 00..112500 sTandard : Ignore 5898 ssTTaannddaarrdd :: IIggnnoorree o8r10dersT: a2ndard : Ignore sDtiamretnsiVoanl:uPeP:K 500 DU PtoraikggesrhLaimpite:: P18o0i0nteSdec NstdArt iiggnnoorree :: 61200 SSeecc FMielatseurre window Regeneration :: : N7o5 No ofourtmuplaut:: #c.d#:e=eck3 %* COR786 1995-08-22 17:22 Output of : 9508221 Tlioride 1.5 Fluoride L Pe "en Pos Typ Ident Ch Result ? Time Ch Result Time w1t ciw InitialTraWcaesrh 33 10..407663 2 qa Drift 3 1.488 21605 44 00..09038021 386 4 0.9386 00 0 43 o8w1 5 82 standWaars1dh 33 00.1006663 standard 2 3 0.073 671354 44 00..00018542 911 4 0.0282 00 0 7 8843 8 85 Ssttaannddaradr4d3 33 001100982 standard 5 3 01129 11206816 44 00..00868356 1435 4 0.1183 00 0 19,0 786 11 88 SSttaannddaarr76dd 33 00..218516 standar8d 3 0614 11768115 4400..12561902 1955 40.4788 00 0 1132 s910 StSatnadnarddar19d0 33 11.243682 14 a Drift 3 11488 22310384 44 00..97291132 2483 4 0.9385 00 0 1165 owu 17 u SERUM BLWKash1 33 00.008663 SERUMBLK 2 3 0084 22873213 4400..00502882 3006 4 0.0493 00 0 189 uu 2u SSPPKK 6622--21 33 00..110384 33316804 SPK 62-3 3 0.124 3533 4400..01828450 4 0.1120 00 o 222 uu 23 u SSPPKK 225500--21 33 00..219897 SPK 250-3 3 0.275 33871804 44 00..12885354 4060 4 0.2644 00 0 2254 u.u 2% a BBLLKK 33 00.1018074 44420318 440.0.00585263 00 Drift 3 10449 4584 4 0.9125 0 2287 uw 29 u PS271W1a-s1h 33 00..008603 F52719-1 3 0.076 44973859 44 00..00401882 5111 40.0340 00 0 331 ouu 32 u $F5522772215--11 33 00..007715 $52727-1 3 0.071 55425893 4400..00235278 5633 40.0239 00 0 334 ouu 35 ou FF5522781016--12 33 00..006729 F52719-2 3 0.067 55987117 44 00..00220694 6155 4 0.0172 00 0 337% wuu 38 d F$5522772215--22 33 00..006636 Drift 3 1.489 66530395 44 00..00018584 6685 40.9390 00 0 4309 uw 41 ou SPK W6a2-s1h 33 00..102643 SPK 250-1 3 0.313 76093236 4400..10101822 7213 4 0.2938 00 0 4432 ouu 44 ou BBLLKK 33 00..008892. SPK 62-1 3 0.094 77535884 4400..00548610 7736 4 0.0671 o0 0 4465 ouu 47 u SSPPKK 6622--32 33 00..110182 SPK 62-4 3 0.119 78901814 4400..00984800 8261 4 0.1047 000 4498 uu SSPPKK 225500--21 33 00.1219749 88641314 4400..21779617 00 5510 owa DWraifsth 33 01..046534 89708255 4400..05018527 o0 5532 wuu SPOBSLK 33 0o) a 9a3d0e9 440.001!2630 00 Page 1 of 2 . Ld a 31 CORTS? 1995-08-22 17:22 output of : 9508221 Fluoride 1.5 Fluoride L Pos Typ 5554 uu 5576 uu 5598 uu 6601 uu 6632 wa 665 uu 667 uu 668 uu 77au W2t rw Ident 52127B-L2K PF5522781036--22 $F5522772138--22 P5522773185--22 DWraifsth $5522870294--22 $SP5K273672--12 SPSKPK 25602--12 SPK D2r5i0f-t2 RunOut WWaasshh 22% Ch Result 33 00.007747 33 00..007714 33 00..007629 33 00..008792 33 10.1502663 33 00.1007724 33 00..007815 33 00..105906 33 10..521325 33 00..006633 7 Time 99645882 109080348 1100138541 1100751316 1110182876 1111243143 1111756817 1112913162 1122426826 1122790337 peu Ch Result F Time 440.0.00330607 00 4400..00234152 00 4400..00226019 00 4400..00227116 0 44 00..90605832 00 4400..00236015 00 440.0.00254114 00 4400..10464927 00 4400..29351503 00 440.0.00008822 00 Page 2 of 2 oT C3788 3 0.2278088 Calibration curve EITM ETYE of 95082201 Fluoride L IYI o s MIE | t{ $ - | | || 0 order: 2 | Measured v1 0.39810 900 woven Cco2789 Calibration vs of ROLE Fiore 1.5 I CXTTYREN TENTH NTs 0-06s3o MITNEA] | J| ; 4 3 ii{! | | | a | om] rd Li || om0 e oe'rrA eioMeasmured roiLanenmTM4TM095 GOO COR730 4 ~] I I ml Cl | Las [i Cll i EE li AA 1995-08-23 11:00 OutPut of : 950823A1 Software : version 6.1 c1990,93 operator + Dow Date of the Analysis : 1995-08-23 06:55 Analysis Pile Name : C:\SKALAR\DATA\EWIDATA\SERUM\950823A1 ow Malis AhSMorDzoTmC1C2120o94Sv1.21e Color CFalluiobrriadteio1n.5order = Inverse Logarithm slope fas sas Result = 10l [x=5-a] 5Gx C== CSclooomrpmreeeccottfaeddthvveaallelueelecootffrottdhheee osaammpellee:racion 1 aaoizC== 0o.l0o0o0o0r0s -2liesa CFalluiobrriadetio.n order = 2 Correlation : x = 0.99897 Result = a2 * x + al * x + a0 aa2zi0=:% 000.l50o00o60000z00s . sampler THSuaimmpbpeelre Tine i+ ls30a100se0c. AVarsh TTiinmee Take up {1i .S12i0nglsseeecc.. naoPcadcliealHeight ; N7o0nema. Diluter adnfieileuudttliieoonnHeVFtoaolchuttnoer ::| 82100.5 mm ml. ReDislaumtpiloon runs |i1 RUseeprrocfeisle : Mo . TXT ' LL cozy9z 1995-08-23 11:00 output of : 950823A1 Pluoride 1.5 SPiagtnhalnumtybpeer :: De3bubbled DesycsotleonrNumber :: 0Yes dRieLstauntpele i: HFoo d4i6l Touhtrpeusthold :: 04095 : Window event : Off Fluoride L s512 53 ssTTaannddaarrdd sTandard :: : IIggnnoorree Ignore 854 86 ssTTaannddaarrdd :: IIggnnoorree sTandard : = 0.150 $878 ssTTaannddaarrdd :: 00..360000 85910 ssTTaannddaarrdd :: 11..250000 DOirmdeonrsi: onInv: erPsPeK Logarithm tsrtiagrgterValLuiemit Peak shape :: 1580000 DSUec : Pointed NStdArt iiggnnoorree :: 16200 Measure window : 75 &SSeecc FRielgteenreration i: NFoo foourtnplaut: se.ess SPiagtnhalnumtbyepre :: De0bubbled Descysotleomr Number i: M0o aiReLsuatmeple ii FHoo d4iilG oTuhtrpeusthold :: 04095 Window event : off "versa OR793 4 1995-08-23 11:00 output of : ssosz3A1 8s521 sastmtaaannndddaaarrrdaa |i 000...00081%05 58555 seStttaaannndddaaarrrddd:i o00.l.3i03n%0 555575 sssTtaaannndddaaarrrddd ||| Trfoaonmmeoorrrsee DO2ri1dm0eern"sS:iToan3nda: rdPe| Toners PEsertaiaksrgtesrhvaaplLeuiemit ||i P1So00i000nteSDdeuc NoSnetdsh"srutreiiggwnnioonrredeow | 736502"0 SSeacc RfFeoigrlemtnueelrarationc4sii|crsNeo output. seer ii o2794 4 1995-08-23 11:00 OutPut of : 950823A1 Pluoride 1.5 Pluoride L Page 1 of 2 pon peu Pos Typ Ident Ch Result F Time Ch Result Time w1 t iw 2a InitialTraWcaesrh Drift 33 3 10.405624 11465 20695 4400..05006403 384 4 0.5067 00 o 43 sow1 5 82 StandarWdash1 33 00..006694 standar2d 3 01073 763125 4400..00016705 910 40.0266 00 o 76 8s43 8 85 SSttaannddaradr4d3 33 001.0099 Standar5d 3 01129 11028660 440.0.00961045 1436 40.1186 0o 0 190 8876 11 88 SSttaannddaarr76dd 33 00.125778 Standar8d 3 0.618 11768160 4400..21451093 1960 40.3698 00 1132 88910 stSatnadnarddar19d0 33 1111426363 4a Drift 3 11510 22311304 440.0.54076944 2485 4 0.5109 00 0 1165 owu 17 u SERUMWaBsLhK 33 00..006848 SERUM BLK 3 0.082 22782343 4400..00056706 3010 40.0468 000 1198 uu 20 u SSPPKK 6622--21 33 001.101958 . 33316816 SPK 62-3 3 0.115 3533 4400..01705034 4 0.1012 00 0 221 uu 23 u SSPPKK 225500--21 33 00..210484 SPK 250-3 3 0.225 33878171 4400..11935741 4063 40.2081 00 0 225 uu 2a SSPPKK 225500--54 33 00..225297 Drift 3 11505 44243172, 4400..22300984 4587 40.5104 0o 0 2287 uw 29 u SPK 25W0a-s6h 33 00..308674 BLK 3 00092 44983179 44 00..20905620 5112 4 0.0651 0o 0 330 ouu 32 u P52801B-L2K 33 00..008725 F52720-2 3 0.077 55426824 44 00..00432518 5636 4 0.0365 00 0 33 oouu 35 ou 5522778383--22 33 00..007775 F52730-2 3 0.074 55988162 4400..00337211 6162 4 0.0294 00 0 3376 uu 38 a $F5522870321--22 33 00..007662 Drift 3 1.506 66531338 440.0.00304115 6688 4 0.5106 00 0 039 ouw au F5271W4a-s2h 33 00..006840 P52734-2 3 0.076 67903307 44 00..00406205 7215 40.0346 0o 0 4432 oouu iu SFP5K277642--21 33 00.1017172. SPK 250-1 3 0.153 77536951 4400..00396621 7740 40.1460 00 0 444765 ouuu SPK 250BB-LL2KK 33 3 00011.001887553 887209681495 4440.00..001556115777 00 low ved 0 5iouu 50 a SSPPKK 6622--21 33 00..100825 Drift 3 11520 88641368 440.0.00852117 8790 40.5129 00 0 5s2owu 53 u SPK W6a2s-h3 SPK 250-1 333 00.l103624 0.136 99104205 4400..01026300 9314 40.1277 00 0 GaGa. COR7rs35 ys 1995-08-23 11:00 output of : ssos2aa - Pluoride 1.5 Pluoride Pon on Pos Typ dent Ch Result 7 Time Cn Result 7 Time $$54 S6 uu u 57 SSKK SK 222355000.0-432 33 3 000...322531318 d25a04s39e50 444 o0ol.li2es0ae3es4 BLK 3 009 10014 4 0.0651 00 0 38Bouuu au PPsS22711225B--L22K 333 000..0008773 111000331638s59 444 000...000435716705 7528032 3 0.075 10715 4 0.0316 000 88Guoaw 6u P2D7rV1iafs6th 333 0011.1005672452 111011821933181 444000...00s09i83s04 P2202 3 0.078 11433 4 0.0304 00 &&6 uuou 6 S7PP55K22'01681277-221 333 000...000787536 i11i1es3d9si2 4440.00.0.04a38m4701 Sx 622 3 009 12117 4 bloon4 00 T7T2oouuuw 5a sSSPKKK222555000.321 333 000.l12i3e18s 1i1322463e45ss7 444o00..a.7733407e%0 Drift 3 1537 121) 4 03137 o 9 WCoToww Runout aWasshh 33 00.1008644 1133209425 4400..00008600 Page 2 of 2 da COR796 * Calibration curve of SSOZZAE Fluide L o [EXTTTNNIYIIYE 6 Jen 0o4 ozes SMITIITNEA] | i i i; Le Y/ eves | pow | Order 2 | = r 0.99897 TOOLS CoR797 4 |] // [toma= EEL EFTYENTTENYE 6 NEI 0.c4ciAMTIIry 64] :[I| / |a. ; |3 | + a es: ew | Pi CCR7e8 48 ia|i lolI |A | Il stil I. Rau data of SS0820A1 : Fluoride 1.5 ws [ZTE 7550 MUST 25% [ISIPHed] 24 4 | :i 3 2 . 45 ot | 7] szs3 2f a xm 37) (ion4 | [leaf] I 3 \ 0 4560 Tine EscoExit | FiHeln | Crtl-Pedit peaks | ' 9560 over CORECO > or EE Pathno: 3 _ TineIGEEEN Value:MEINDelta:(2) | ~ - | ;| | | | | 3 | ol | | | ie gs i [10LH7 | i | pl seste e ne d { [| = To pe Rl c32z01 1995-08-23 15:23 output of : ssozamy Sof'tware : version 6.1 c1990,3 Operator + DDW Date of the Analysis : 1995-08-23 10:50 Analysis Pile Name : C:\SKALAR\DATA\WIDATA\SERUM\35082381 FClauloirbirdaetio1n.5order = Inverse Logarithm S1ope cation x-a x = corrected value of the sample Result = 10l 5 Set he elkeshe a0a201: -00.i0ia0s0am0s0 CFalluiobrriadteio1n order = 2 Correlation : x = 0.99924 Result = a2 * x* + a1 x + a0 a0a220= 0TS.Ol0lo0ooo0sa0rs0er i Sampler HSTiaykmpbpeelre ine j| hs30ao0s0ec. VMTaarksoh up TTihnee |[S1ii%n0gnlseeec. Snheeecdilael Height | N70onemm. Dituter adnieTleuudttliieoonnHeFviaoctgtuhomret:|| 328005 mm m1. ReBsilaentpiioen runs i|1 [ Reprocaes" | Mo mr cAomowr =1h1i0h9sS fHooTx62e2392-21)5 Conde COOO2LE02 5 1995-08-23 15:23 output of : Fluoride 1.5 SPiagtnhalnumtybpeer :; Da3bubbled Dseycsotleonr aiLute Number i:: 0Yes No Ro4is1anTphlreeshold :i 4M0o95 W4iinGdoowutpeuvtent :: o0ff 5s2i 3 ssTTaannddaarrdd sTandard :: : IIggnnoorree Ignore si sTandard : Ignore R $7 S sTanH dard 58 sTandard :: Tng0r.y3,0,0 0.600 8910 ssTTaannddaarrdd :: 11..520000 sDOtiramdreetrns:ivoanlIunev: erPsPeK : L5o0g0ariDtUhm sPttorAairkgtgesrhiagpnLeoirneit ::: P1o8i00nteSdec 60 Sec . FNHiodlatseurreigwnionredow i:: N17o250 S1%ec ofRoeurgmteunpleauratti:onsaa: nNo Fluoride L PSaitghnalnumtbyepre Decolor :: D0ebubbled i Xo dSiylsuttoen Number Resanple i: X0o `No W44i41n16dooTwuhtrepevustehnotld ::i 04095 off 95082381 0055 CORE03 = 1995-08-23 15:23 output of : 95082381 - 5sl2 53 ssTtaannddaarrdd :: sTandard : 00..003105 0.060 8s54 86 ssTtaannddaarrdd :: sTandard : 00..102500 0.150 5578 89 ssTtaannddaarrdd sTandard :: : IIggnnoorree Ignore o5r1d0ersT: a2ndard : Ignore tsDrtiiamgretgnesrviaolnLuien:it~PPM:: 1580000 SDeUc NsPtedAarkts"ihiggnnaoorrpee e::: P60ointeSdec 120 Sec FRiMeelgatesenurereratwiionndow i: | N7o5 No ofourtmpuulta:: c84.i4z0e038 Jiteise 0oR804 5 1995-08-23 15:23 output of : ssos2381 Page 1 of 2 Pluoride 1.5 Fluoride 1 on oon Pon Typ Ident Ch Result 7 Time Ch Result 7 Time WiFRC Eiv InitialTrDaWrciaefsrth 333 10L.4i07s66e5 iow Wash 3 0.065 23186265 4440.00.0.5305138%89 627 4 0.003 0 45 a88213 Tse Ssstttaaannndddaraadrr23ddl 333 000..0009%78 Standar4d 3 0.11 1037813710 4445bolllo9okcveeess 1363 4 oon 0 8910 888675 SSstttaaannndddaarraddr7d65 333 000...21115277 11I74s8i364 444 5o6...i39s31e00r1 11 88 Standar8a 3 0.21 los 4 olives 003 3 1u132 a88510 stSatnadnardDdreirs19at0 33 3 111.442873005 ow Wash 3 0.065 223451813736 444oobl.assii0on%s 2127 40.0038 oo o 1176 uu 18 u SSEERSUEMMRUBNBBLLLKKK 33 3 000...000788874 233100814520 444 0b6..l00o89a53643 8 u SK 62-1 3 0.007 3363 4 0.0814 o F22r2 u uw 23 wu SSSKKK23660220--123 333 o00..i43l24s1 SK 2302 3 0.233 33370338%4 444 060..110000ks5 does 4 o.gu 0o 2250 auuw aw SSPKR iD2r23i40f13t 333 010.4030s48 Vash 3 0.065 44434285s3". 444o0o..i5ib1e7e14 4825 4 0.0038 0a 2sFr0 uus 12BB4XX2 333 000.01230308 Fa Ps2726-2 3 0082 455021841506 444 6o0...i03z59e86e% aed 4olds 0 ZHWoouuu FH PFP5a2213733625222 333 000...000778860 52135.2 3 0.07 es339l83y44 044 .000..30033648877 eiss 40.0309 a0 3%7 ou 33 4 7PS522D77r12i11f-4t8 33 3 0100.050707445 Wash 3 01063 e66s33o0%l3 444 o000...00s32a561i83 6933 4 0.0038 oo aod 4o$a4u 8 EPPs7ap2is3pi4d y33 o00.102m7875. rs27234 3 01003 7n730e35m33 s44 o00..0m3330m381 7368 4 0.0894 o8 tow otimalinpiteS20500 GsFHouu 9a SKInBBiL1xK 333 000l0608as)2 sk 62.1 3 000 81703s1s;7 444 000.l.a00e44se1ss8 8267 4 0.0888 03 BH5E 4u SSKKD66r22i-e23 333 0011411801356 s861e49is2s 444 000...130018335207 5 3S82u0ov EsmkWaaash 333 0o01i0s6%3 3ai0h3a5 4440o0.t0H0e3 -- C92805 5 1995-08-23 15:23 output of : 95082381 Pluoride 1.5 Pluoride L Pos Typ 5554 uu 557% uu 5598 uu 6610 uu 6632 wa 665 uu 6676 uu 668 uu 7 7 u 7732 ouu 7754dw 77% uu 7798 uu 8810 uu 8832 uu 8851 wd WE Iw Ident SPK 250B-L3K BBLLKK P5522773226--22 FF5522773359--22 DWraisfht FF5522771316--42 BBULKK BBLLKK SSPPKK 6622--21 SSPPKK 225500--12 DWraisfht SSPPKK 122540--13 SPK 124B-L2K FS2711B-L4K SPPK52711294--41 DWraisfht Runout Wash Pow Ch Result 33 001.122944 33 00.1017042 33 00..008700 33 00..007638 33 01..046457 33 00..006736 33 001.118225 33 0011007831 33 00.1110052 33 00..117748 33 01.1046954 33 00..126065 33 001.110650 33 00..00896 33 00.103799 33 011046751 3 0.065 7 Time 99646994 109081471 1100316973 1100751453 1110088921 1111423435 1111756994 1121192432 1122426899 1122684159 1132292923 1133531493 113368963 1144201444 1144536976 1144976463 15218 Pen Ch Result P Time 4400..21515185 00 4400..00728379 0 4400..00317430 00 4400..00211050 00 44 00..05013582 0o 44 0#..04820887 00 4400..11172671 00 440.0.00231927 00 440.0.00872972 0o 4400..11678157 00 4400..50200308 00 4400..11599593 o0 4400..10583399 00 440.0.00464838 00 4400..01336161 00 4400..05013787 00 40.0038 0 Page 2 of 2 POLES COZS0S 2 - Calibration curve of 95082381 : Fluoride L [* 2150330 CXTTF NNENTE YE 6eeNae RReEt0S0a 0401s Mee] i t | | | | | 1 -| | || o Order : 2 Measured r: 0.00021 00 coors 92807 57 | C| d | i i | | | | [-- | 0 -_-- . ye Measured -- 2095 Te Se P Co2808 : Po ntsosuze Pari 1.5 ro, ETERNITY WY ere -- | |- : 4 - | '| NLI. | ll | lle | 1 : far Wells I: -- ------ Te =o OUUTeS 5 COZ809 Rau data of 95082381 : Fluoride 1.5 4095 ] Pathno:_3 Tine: RCH Ualue: MPZTFEN Delta: [Z3 -- [es2 4 P `i Hi a It 74 .A CAR re Raga ref 0 | ase Tine EscEXit |FizHel | Crtl-PEdit peaks | 5@ |v ll ! 9560 "006408 C02810 o owdats of : Fors & 2 i 3 B|i A eldlb [o UR Ae | 8935 SF Te | iaastt LdIa he Re J Tine ' 13935 PVE. o2811 | ZIT) Rav data of 95082381 Fluoride 15 CTH 13510 ORY 576 Cr 7I-- I~ || |]i| | No . Ng | fi J [| TU| Te be | \ 6 l| ule To. ho a COR812 Software : version 6.1 c1990,93 Operator + oow Dat of the Analysis : 1995-08-28 07:32 Analysis Pils Name : C:\SKALAR\DATA\EWIDATA\SERUM)\950826A1 QA os+"Colas R lss Secon Comer Candt CPalluiobrriadteio1n.5order = Inverse Logarithm Stops a= rarer Rosure = 100 [x25a] 5aX==iScloorgpreectomfedtahvealuenslecoftmrotdheemsaamplees FaaOi2== -10o.l0a04 0070s0 . CFallufobrriadteion order = 2 Correlation : x = 0.99897 Result = a2 % x +a1 tx + 20 2aa0i2l= -0T0o.0l0o0so0o0:s0s Sampler Diluter HWSTuaaymsmpbhpeelre TTiimmee |ii: l13S20A010s0se0ecc.. STAParekceiaulpTine :[1sNoinneglseec. necdle Helght | 70 ma. ddniiellsuudttliieoonnHoVPioahlctutnoer || 2810005 mm al. ReDsilaumtpiloon runs i Ruesperrocfeis"le :: Xo mr 0040 C0813 1995-08-28 15:03 Output of : Fluoride 1.5 DePSdiagtonhlaolnrumtbrepr i|: DYee3sbubbled RdSoiyslsautmtopenleNumber ||| k0o No WaaiiinsldooTwuhtepeeuavtnenotla ;i | 0109s ote 8213 ssotTTaaannndddaaarrrddd :: IIIgggnnnooorrreee 65851 sasTttaaannndddaaarrrddd:: IIggnnooor-reie,so 88758 assTttaaannndddaaarrradd: 100...263000000 DO8ri1dm0eern"ss:iToannTdaav: erraPsre: Loga1r5i0t0hm PSsertiaagkrgtesrhvaaplLeuienit i:: P1So80i000nteSDdauc MNsetdaAsrutr'eiiogwnnioonrradsow i;| 17f25o0 3SSeecc fRFoierlgmteuenlrearation |iNoe tia Fluoride L DpSeaistoohntaolnrutmyepre :| rDe0ebubbled aiRSeLyssuattmeepnleNumber ii fo0o W5aii0nidoTowuhtepoeusvtnenotla || | 84095 ofr ssoszear 60460 - coRs14 f 1995-08-28 15:03 output of : ssoszam1 51552 Satttaaannndddaaarrrddd Si tmandard 0o0..l0081%05 0l08 55576 sTstaaannndddaarrradd ||| tanc00e.1s9%% l5$95o TTTaaannndddaaarrrddd ||| TTToeannmeoerrrsse SDstiramdreotnrs'viToa3nts: TPTe 500 pu . FrEreieasgesrhapienit || P19e0s0nebsec FiNenolaa"tseurradnwoitnedow [| 9n33e% sec oRfueotgrpeunmeearatioTneiqt:iir|cehrhe . sore" CoR815 1995-08-28 15:03 output of + ssoszens Pliorids 1.5 riuorsde Pos Typ 1dent oon oon ChResult Tine Ch Res7uTlimte YiHl dW i InitiTairlawcnaemr van 333 1U04.50n638 3 00a Pom ssa 3 oof xd06e8s 4d400o.00m085 35 4 oes 9 0 75 3oms2s 35 sSstttaananddnaardrddss: Stnamas 333 3 og0i0og5rs ood gs3e9on7 ise fd4oo0oen0mse8 gas 10% 200 Q iH5,oos3we67 Loss sSstttaannnaddaawrraadsss Shines 333 3 oooadlress 14 13 m0 stnderato 3 Lae diieehes ge s1oo0dmBiRe% iommo 000 oo0 i1i60es% ou ssmmusBDtVraaaisfmmht 333 3 o0104o68n5s ost eidsshrse den 4o4 oondsedes 00% das se) 0 00 omwoouuu mowou sTsaetReCeEsdN 3O 3 aoNdonh sae dood ampre ffd0oo%e%Eng aa joi oo0Q 00 Sking 3 o 2i 3 u ou msim Bnagw 333 o00o0s2d8 oes FH Dire 3 14g ae49pe5 ann 4o0osi Ben joe iss 4oie 2 mFiouou omouw EmEEEtonwaThsash 333 o0o00e0e6sSs8 i4s3sy0s f44oooeaeosss a oue 90oo 0 oBnoowuw Bou E BEEEn ELN 33S0oooo0on S00 mai 3 oon Jnsees jE fffoooe%usm fome aes joo oo0oo 0 36 Ei u ou se Seod arinit 3 ach 333 3 UoonoEems 006s wou exam 3 oR aegnnh d4oooauuns gs 4 ok 0O0O 0 $o9dw ao eBBAnANCCeTZ SED 333 o000d68es Sole 77S33E3 am 44feoolneemsnse joe pe foo 00o 0oo ies wou BBoouu SsIsGoi rset 333 0o030s%s 3 oles Fay 3 oo spgaares gas if foosoe: 400% a fowe 0o 0 H0 H 4 $0 podaihi mmo 3333 000D0cg8eg aogsMt d 4tooweonsnoo0 doom Page 1 of 2 a 0251642 1995-08-28 15:03 Output of : ssoszear Fluoride 1.5 Pluoride & on oon Pos Trp 1dent Ch Res7uTlimte Ch ResuTlimte 5ss% uuou 7 ou PBPS5222178326305-444 33 3 000.0.000788505 PS2130-4 3 0.073 a3364de8os4 10016 44 4 0o0l.0o09343a5ss8 4 olora 0 o5 uoouu au PS5E2KT0I602T2-E41 333 000..1000077673 SK 62-2 3 0117 1l100o33s36s6s 1011s 444golllooossaes3sy0 4 0.tass 00 0 fGaovua u smDaWrailsfht 333 O011l406e25 SK2507 3 023s i1110a0s%: iris 444 0o0.i36ie0er9ss3s 4 gies o0 3 G& uouuw 8u sKizBBeLXiK 333 00O11s009o33 Pad 3 0l085 11111137346s13 12113 44 00o..0i603i84 4 blger 9 7[72 au 75 PFP72211124444 333 000.1000880306 P2294 3 0.079 1i13n36c54ri1 13817 444 ob0llloboseeee3ss) 4 oles 0a 777%% wa 7a 528D0Wrai3sf4ht 333 001.1400886858 PS2ii6e 3 0081 11132339339463 13sie 444 o00l..oa94g0ne01y 4 0.oss o 0 [78i4 aa1 uu SPPES2K27186272--841 33 3 000.0.0809175 Sek 62-2 3 0.122 11143306s45es . 444 00l..oo0e3ge8ss2 1421s 4o.v5e1 o0a a 8882 aouuw 8 SsK12D1r24i4f12t 333 01o1ll5s0sa8 Wash 3 01068 11144475347940 11361 444 o0oln.ee3sos6d 4 0.4031 00 Wt Iw Runout Wash 3 0.068 13235 4 o.oo Page 2 of 2 CJ coRs1y 67 TI "Calibration curve of ssogoent : Fluoride L || 0.281781 CETOWNTEETYE 6NEins 0.007237 aYEN67] | | | | | ;i | 0 | I 1. | | | J : [----- | | uLL 0 odOrdeerr:i2z Measured 0 rir:o0s.9w38w97 500 | or 02818 &* [Calibration curve of 9508280 Fluoride 1.5 | | 1.6003117 CETTON EWNOOT T ETE inyI 00T eosH se | 4 MIEN ea) -- | | | |1 Be{ | el | | || J: | |[o.0670050 L||rooe rOrdei r : Imnvere se LorgaritshmWeaesurel a osmosr: ei8m651 tom s|s Ee 1 G0R819 ss a Rou dataof 85062681 Fluori1d.ea5t -- ~ oa v |} |3 \ ce| L|o | |1 4 . a | Io 04 TT | fo | 0 Excrbait 1 Fre GEA eTTine " ;4% EN Wh|| 5000 --eeerrr cozszo - Rau data of 95062001 Fluoride 1.5 rs CTUEE ToSo550 UY 27-- re 7 -- a 5 ;i || a of ip An A* By HS . S88| aad | | w= Tine 950 EscoExit | Fivheln | OrtI-PoEait peaks | Soorrs o28z21 "085 CETTE RRTaSu d5ata%of 9W50Y6260E 1 FlE uorideT 1.5 -- Ww A : 3 EY \ Pega?Nf @ fw dg a ad $1140| oligo 0 | ess Tine 1393s EscExit | Fivheln | Ortl-PoEait peaks 1 ovorm o28z2 7 ouan of 50 Fran 1.5 I CET EE FTTH 13370 MUN42I6 T [IyY Xen eal W \ i2; io(NT o . Pm rin rh EF TEE H10 i87 SSttainnddaradas7 11 l1.a00o0 CO C2L8I23 13 1995-08-- 29 05:38 output of : 95082881 Software : version 6.1 c1990,93 operator +oo Date of the Analysis : 1995-08-28 11:47 Analysis Pile Name : C:\SKALAR\DATA\HWIDATA\SERUM\35082831 AonDwT Y1a0lSi.s SpoonzC3o2r37vies a) CFlauloirbirdaetio1n.5order = Inverse Logaritha s10pe rr Rrosult = 10l [x=-"5=cl] X1== 5= Scclooorrprreeeccttofeeddthvveaalleuuselecootffrottdhneee csaomnpcleentration 1 aat2 == -o0l.o0o0o0r0:0 20 = -1l18875 CTalluiobrriadteio1n order = 2 Correlation : r = 0.99313 Result = a2 % x +al * x + a0 2aa02is== 00o.ll00o00o00e20s00s . sampler TyNupmeber +iYsA000 WSaasmhple TTiimmee Az Time :: 15200 sseecc.. 1. sec. TsaPkoeciaulp needle Height : | NSoinnegle 70 mm. Diluter ddniielleuudttliieoonnHeVFioaglchuttmoer ::: 281.005 mn ml. RoDislaumtpiioen runs 1ii RUesperrocfeisle :: Ho x ooorre coz82q4 1995-08-29 06:38 Plucride 1.5 PSiagtnhalnumtbyeper . Descysotleomr.Number dRielsuatmeple idiGl oTuhtrpeusthold Window event output of : :: De3bubbled :: 0Yes :i NNoo :: 04095 : Off Pluoride L 5821 ssTTaannddaarrdd :: IIggnnoorree 8843 ssTTaannddaarrdd :: IIggnnoorree 8565 ssTTaannddaarrdd :: Ign0o.r1e50 8878 ssTTaannddaarrdd :: 00..630000 88910 ssTTaannddaarrdd :: 11..520000 DOridmeernsi: onInv: erPsPeH Logarithm tsrtiagrgterValLuiemit :: 1580000 DSUec sPteAarktsihgnaorpee:: P60ointeSdec MeeNadsureigwnionredow :: 17520 %Sec FRielgteenreration :i NFoo ofourtmpuulta:: #a.4as . sPiagtnhalnumtbyepre :: De0bubbled DseycsotleomrNumber :i 0No RdeisLaumtpele ii KNoo idiGl oTuhtrpeusthold :: 04095 Window event : Off 95082881 querer TM 22825 1995-08-29 06:38 [Ep -- : 855312 TsTetananndddaaarrraad:i| 000...0001%%5 s88e54 57 ssstTtaeannndddaaarrrdad Standard i| 000/..41070%0 toners s5539o SETTfaaannndddaaarrrdad ||| TlTooonnneeerrrsss tsDOrtiriamdgreogtnres'rvi:ao3lnLuie:nepe|"Ts 1s80000 Sbeuc osPnteaaa"rke shilafopineoorree+ Hoanura window [| FG0ootntegsseec | 15 3 - FfRioelrgtmeeunrlearationousli|chNeo output' Sint --HOO0T2I5S26 1995-08-29 06:38 output of : 95082881 : Fluoride 1.5 Pluoride L . Pow Pow Pos Typ Ident Ch Result 7 Time Ch Result Time 1 wt iw 2a InitiaTlrWacaesrh Drift 33 3 10.406645 1474 21625 4401..05094243 387 4 1.6075 00 0 43 o8w1 5 82 standaWrdash1 Standar2d 333 00..006659 0085 671267 4400..00014141 S03 40.0394 00 0 7 8843 8 85 SSttaannddaarr3&dd 33 000.101535 standard 5 3 0133 11206837 4400..00588601 1439 4 0.1182 00 0 190 8876 1 s8 SSttaannddaarr76dd 33 00..218506 Standard 8 3 0.618 11768175 4400..31153242 1963 4 0.6720 00 0 1132 88910 4a stsatnadnadradrd109 Drift 33 3 110242780 11498 22311337 44 11..62080978 2487 4 1.6438 00 0 1165 wu 17 u SERUMBLWKash1 33 00..008665 SERUM BLK 2 3 0.082 22863826 4400..00402404 3011 40.0343 00 0 189 wuu 20 u SSPPKK 6622--21 33 001.112178 . 33138693 SPK 124-1 3 0.293 3540 44 00..01904862 4 0.3291 00 0 221 uwu 2 wu SPK 12B4L-K2 33 0010019379 BLK 3 01082 33879124 4400..10267072 4064 40.0353 00 0 2254 u u 2a P25522773157--44 33 00..008912 Drift 3 11455 44244124, 44 00..00353146 4588 4 1.5730 00 0 2287 uw 29 u P527W36a-s4h 33 00..008605 P52726-4 3 0.078 44983165 44 00..00034148 5116 40.0269 00 0 3310 ouu 2 wu FF5522773392--44 33 00..007724 F52711-8 3 0.075 55426838 4400..00211603 5635 4 0.0227 00 0 334 ouu 35 ou $52719B-L8K 33 001007709 SPK 62-1 3 0.093 55891322 4400..00219283 6165 4 0.0545 00 0 3376 ouu 38 a SPSKPK12642--12 33 00./019086 Drift 3 1460 66531451 44 00..00739815 6689 4 1.5857 00 0 1309 wu au SPK 12W4as-h2 33 00..107654 BLK 3 01126 76094014 4400..10708444 7215 4 0.1074 00 0 4432 oouu au F52725B-L8K 33 001.008894. 52721-8 3 0.080 77336869 4400..00436970 7733 40.0316 00 0 4455 oouu 7 ou F5$522070162-78- 33 00.0007767 F52713-8 3 0.071 87099124 4400..00226477 8266 4 0.0157 00 0 489 uu 50 a 5F252772138--88 33 00l1007722 Drift 3 1.463 88641339 4400..00116613 8789 4 1.5898 00 0 5521 uow 53 ou 5o 271i 5-8 3 00.007%6 F52738-8 3 01073 091B33 4 S"e024s: 9313 4 0.0191 00 Page 1 of 2 004m COTE? Mm 1995-08-29 06:38 output of : 95082881 Pluoride 1.5 Pluoride L oon peu Pos Typ Ident Ch Result F Time Ch Result ? Time 5554 uu 5% u $SP5K280692--81 33 00..007828 SPK 62-2 3 0.100 99646828 4400..00146551 9838 4 0.0648 00 0 5578 uu 59 u SSPPKK 112244--12 33 001.113261 BLE 3 0.083 1100109104 10364 4400..01929210 4 0.0362 00 0 6610 uu 62 a SPK 62B-L1K 33 00..017046 Drift 3 11460 1100751348 10888 44 00..00715927 4 1.5857 00 0 663 wu 65 u SPR W6a2s-h2 33 00..100695 SPK 124-1 3 0.147 1111214209 11414 4400..00709494 4 0.1393 000 6676 uu 68 u SPK 12B4L-K2 33. 00..018495 1111756952 44 00..01447275 BLK 3 0.084 11941 4 0.0378 00 0 67 uu 7 ou 57522772347--88 33 00..008833 F52801-8 3 0.099 1122219104 12466 44 00..00336629 40.0643 000 723 uou 74a F5522773230--88 33 001.007888 Drift 3 11465 .1122684104 12988 44 00..00426609 4 1.3940 00 0 7765 wu 7u 5278W8a-s8h 33 00..007615 SPK 62-1 3 0.094 1133323169 13514 44 00..00014544 4 0.0558 00 0 7789 uu 80 a SPSKEK12642--12 33 00./110206 Drift 3 11468 1133689626 4400..01605734 14039 4 1.5982 00 0 W8E1 wrw Runout WWaasshh 33 00..006655 1144521840 44 00..00004444 00 Page 2 of 2 GOOLEe COTSZ8 ws Calibration curve of $5082881: Fluoride L ome Channel 0 Heasured: SMH Concentration: NNUGEYZZ) Del ta: | t $ | | + 0.000776 +4 o order: 2 Weasured | roms a00 | ToT C2829 remem Cotati rvs of SEER * Fonte 1.8 | CETTYNEN TERE 6 Neen 0.06sesSMTITNEA] | 1.7548074 | | py J i [I . | Jo oxsmn || 0 Order InverseLosaritheMeasured 5: swe 4085 COR830 Sa 4 ---- Raudata of SS062881 Fluoride 1.5 |i 40es ZTE NTT 5 RYT 75 [IITHEA] || Nd on . 4 | v 3 i 3 | | < A wa . AJ Ic Tive TEsceixit | Fiweln | Cril-PoEdit pesks 1 QA lthAWse[| S000 "008062485351 Raudataof 35062681 Fluori1d.5e Patino 3 _Tine:IN Volve: MPZITMMDelta: [Z0 4035 - oo | ' i 7 oA i | Rm 5% W% | . on . Excebuit 1 Freie | GTR pe o- 3 F006 Te | lissia 0 CUOras COR832 a [Rau data of 9502881: Fluoride 1.5 | CYT ENENNITTS 535 MUNITY 45 [INITHA] 4085 | lg Lil 3:i . I. sva4 wey2 oy ' a Dba. ha RHI WANCER CTR | ess Tine EscExit |FivHaln 1 Ortl-PEait peaks | 11 13035 Sov. 02833 po C2 Rau data of 95082881 Fluoride 1.5 -- SEN3_{EiTnETe E757C70 WUPalTuo8: 5[57Ieee] _ ' | : | AA . EscoExIt | Fishel | Crtl-PEdit peaks | 060468 02834 M 5 Te i d9e.1t1e.r4miSnuemdmbayrtyhearnmdalraewxtdraatcat;iopnpfmolFl"oiwnedsebryuamnaalsysis using Orion ion analyzer. Booty 02835 HWI 6329-152 DAoMhDrmTan0n11S09e5r.u1m Analysis Analysis Dates: 08/02/95 - 08/18/95 ADlXl2s0e0r0umOrsgaamnpilcesHawleirdee thermally Analyzer extracted by and collected ainmoad1i:f1iemdillDioQhrwmaatnenr and TexIpSaAndBabsolleutiioonn.anaTlhyezesra.mpTlehse wDeorhermmeaansnurweadsocnalainbrOatreidonusEiAng94304ppm, 4`T0hpepOmr,io6n2pwpams,ca1l0i0bpraptme,d 124ppm, by direct 250ppm, and measurement 500ppm with no FC-95 blank standards. correction sulsoipneg, 0i.n0te5rpcpempt,, 0a.n1dppcmor,re0l.a5tpiponm,we1r.e0prpemcoarndded1i.n5tphpem aFp*prsotapnrdiaartdes.logTbohoek. 2A).sAunmmainrityiatlabclaeliibsraitnicolnudceudr,veshwoiwtihnsgttahnedaprpd mdeFv"iaitnioena,ch%RsaSmDp,leR(sveaelpuaege and equation of the line is on pages 3 - 5. Psaamgpelse6s -we1r9eshbeoiwngthaenaelxyczeelds.prTehadeshDeoehtrtmhaatnwnaFsCg-e9n5erianitteidalwchaelinbrtahteion curve was not reading below used 0.05 to is bgeenleorwattehethOeridoatnacianlitbhreatsiporneaadnsdhesehto.uldAnbey Orion considered an estimate. THohweeFvCe-r,95duineittioalpcraolbilbreamtsiownitchurbvleanwkasshsapviiknegdhiingthoebrorveiandeinsgesrutmh.an the tsaakmepnlefsr,otmhestbuldaynk#sHamWpIle6s32an9d-1Q23C rcahbebictk #saFm5p2l4e2s3,aftFe5r20384/61,1/a9n5d wFe5r2e330. TFh5i2s73w9o,ulFd52a7ff3e6ctofallthtehedadyay2 4, day 8 samples, samples. and 52726, F52732, This first 3stduadyysowfassadmipslcionngti.nued after day 8 because nothing was found in the Page 1 of 19 Ey 02836 Lus2 DGorsoaugpe:1 Omgkg Fluoride concentHrawtion63in25r-ab1b5i2t serum (ppm 3) FSa5m2pl7e F271 DOaSyt 0505 0O3wh2 037 obses sopasys 081 0338 FF222315 F227 0o8u3s1 0408 0022978 0528 0o6s9s1 0498 s08s0a0 dst F508 0472 054 ods ode DGorsoaugpe:2 4mgkg SFaSm2p7lTes F718 ODaSyBi 0810 04D0w02 0402 ooawrs 0500 aoryss 0349 FFSiIs FS 00790 ou2 0046100 032 00431747 omy a0dae 0331 F209 112 038 0301 0303 GrDoosuagpe3: 16mgkg SFe5m2p7l26e F215 D0a8y6i6 0810 D0a3ysz 031 D0a3y5s os7 poaeyss 0563 FF820210 FZ 007461 0775 0odss9 0451 00873110 0438 ooarsae 04st F788 037 0511 0383 02% DoGsraougpe:4 40mgig FSa5m7pl0e D0.a1y8i5 D04a7ysz o03a4yss FFS2218012 0087524 0043822 0042e84 FF227344 F274 007712 092 oooa sa1s oossee 0870 GrDoousapg'es:10X10 fabric S75a2m7p1l2e D0a9y514 0Da8y0z op.aiy5s8 FFS222093 0096488 004d57 00447542 FS222786 0190664 o04s1s9 0o0441s1z F277 08% 0538 0443 N: GDorsoaugpe:6 10 X 10fabric FFS5a22m37p1l57e "Da11y03971 Do0aayr82250Do9as6yu4 FF2a7s6 F272 00782%5 108 o0e4s9s3 0337 0080131 ozs Foss 07s 032 0am RiCOgR,837 nov sis sum Tt mEiTha TawoofemotaIh aS5e TMD i Ce HS ns i gelry CSnn hesemi wea5n eoEol i [uwrmnelaii EmTmme oommme ome 8O2022 8 10 TE mo 2 FSFcurhcm iooenm om ier wa[uraoieit Tm LEE TTEaR OGhamm [rc S29 0S2020 coSm uammm oe oGoeomm wR Tam mm O03 Wdmnwrsn TTTaEmeR oEonmammn o0or1 1Dd2o0 camh ge oaGnmm . Usommwars omrolemee ooommmyy poowwenmssmsee ocoomws Wdmmtna TEmaemm ooGRduEamW 0So1 302300 M abmw DBwmmmapn oooamsnem occooowmms accooomesmosmmmsec Cn slewaaoss SSSaamnsmi TavEmE ohaemms 08or11 DG20o0 B w sm oM ohwas l11ama0e coouuumm nognyumosmesev coCmeeomsen D TDonms wTTEeR oGwmwmem 003 d23o00 ooommme hwheoe xooxr d1ee4ww%s SSoeourr gootsiossemesev soUonosme SSQREF & memoemems mvmmmm oOGTmmE oSOr RI10 SbBRw mMEogxx njroemmms caoaamm aocroommmoeemmeser oCmweome 8 bo STUDY 320152 serum Sumple SwOnwoele a(Aemcxiutns)g SiunOtntoyreg fTmIldS)AvD mLsFpCeSdSsonoocpoimC)nD cpohv%)er ssAoacmugFn-le (usMpgih?es)d rotMssaepesussnd emm2i Zend TTTaAAsSS 00I2WT 0061 0011 01 Bend TRS 02 01 2200 2200 0000MM 0000MM 2200 16051%% 20 6o% 360648000 33620 006b0o0oss 060k o03o89d4 SsTrOeEVe. 092 ace 0105723% ois 20 66% 39440 06004 oases SMSooopmmmpd2 TTTGRSSS 00OMmMS 0011 01 Mopmd TZ6S 03es 01 2200 2200 0000MM G0o0MM 050 50 2Se1%% Gx 8653772200 74300 1V2i0o0n8 17008 o0or6ee9gr7s2 swSTmnOEeeV.e 007209382 orem 0 Sox 730 lave erie i 83 a2 = SERUMCURVE 2 CARLTON | 23238? `5 02 on a espns o T Py Te wn TU #6323-152 Seeumt S1D RGG Amec)s oSlaC moprleg TmISAe B mLFCOSContocPeCmOS gre)%y pAmcFekne (pM9%a)shs iuMnransssa BaTzpwoons soz o000m%7 000111 001 01 272000 oe 20 om &@ sx oo1z1zs ous 0G00a08r228 ex 173 ore oan prsocae) 22usuepronms2 o00z5 0011 0O2m0 0011 2200 ooaokm 2Z0o oooomm 2E0B 220 1Wxx ax i1oae em 0O8r0e 080 oorrse ods 7ax 4 060 BBBUw nNK Bun ooosoit 000111 3300 20 oom 01 30 31278 ooazr 0176 126 0128 FFFaaImmOoeMRA Fanson ooooooiworss 0011 G1 7300 30 oom 01 20 . o0[s311007 0o0o00m88s10407 070 00730 FFaarmwoaA FFaOmAoLA ooootm 0011 oo 01 2200 20 00% 01 30 07sa4z 112 00087442s oz oes 00866 SFmaemteOI A T 0o0o0m1I 0H1 v]30 01 20 om o0o7u8ms1 0o00o08r67!s0 ex 100 ous sae 2s0opmma B2us0ppm2 O0O%K 0011 03 01 2200 oGoomM 20 oom 2& 20 1s1x9% ex slaass 4@ 0or6e0 06% oodreess ons os oi 30 4 BSwCRUB o0m0a 0011 2200 o2i4s0 0358 000284465. 00058 223 SSSEEERRRUUUMMMBBBLLLAAANNNKCK 0000oo2sm428 000.111 SERWMBUNC 0052 01 22230000 3 SERUMBLNK 00 114.20228 001.14120225 Tos 0108 2 01 20 Tos 0108 < | STUDY (329-152 SE. un TRSUimSpeT mgAoacng)i (SQmaim)oprlge) fTeiIinlvDd msLpFkCadOSCsoonGcboanF)nCO mohvy%e) pwacaunantlg sGMp9ea7e)sd me"M(soagssts)ed 60% 01 35 SSSREMMMBLEBNLC 000o01sss0s 000111 22Zo00 SERUMBLOK ous 01 70 1208 108 00112078 0.108 jx oir SSwCReRWWeMMBsBLLNNCK ooommmee 000111 332000 om FERz 00 01 20 0 2 0o7s3e7 0838 o00o52r8 0083 mx ar ous Ge SSMMEEZZeO1Z FSEeanse ooim oan 0011 01 2200 zo 0000M oom om 01 380 3m0e msxx 81% s1e;s ser gormee ome ooiadn omy x am oe 0% fBaralecd moum 0o1i 230g zo oom oor oi zo Bo eax sseas 129 ose S03i0R1 0128 [eBrunyne FEmaoA ooomooen 000111 313000 ame 01 2p ooszss oss ooo0sszss2 oss 0367 00847 FFamaoomni FFoEnO ooomm ome 0011 01 7300 36 or 01 30 00373775 oa 000037377s oo7as orm oom FFSETTMMOOAA FamONT oamoswss ove 0011 01 Z7o0 70 Famaoni over 01 70 0087504 02 ooo0sms0e oom os o0m24 22: 2Fopnt aa2rorrus o0mMe Oe 0011 01 2200 20 samadw O06 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