Document xd54zvpYjb8Lq00EnGGNkLmRJ

AR L426_ 3262 "444 AR 226 - 3R6.2 ~ |,=: sour Test Guideline(s) `OECD 105 (adopted 12 May 1981). Authors Mary A. Kaiser, Ph.D. (study director) Daryl P. Cobranchi, Ph.D. Robert C Buck, Ph. D. Study Completion Date 27 December 2002 ~ Test Facility DuPont Corporate Center for Analytical Sciences Experimental Station 402/5321 (and Glasgow 300) `Wilmington, DE 19880-0402 Sponsor `Telomer Research Panel c/o Rand Corporation ~ - 2 TABLE OF CONTENTS THBP. .nenensmerssommmrmmmns ssomnmm------------------wl `Table of Contents............cccuweeee 424RY8A4R 184A merssrense2e 2.0 GeSntudeyINrOMa BHOlN w.vcverrerersrsssssssssss nsession 3.0 Matane dMer thodi s..a ...o.l .vewss ersssmssssssssssssssssssies I -- nerBs 3.1 Test GUIAEHNES...ocoevvvvevnisrssssssssssssssssssssssssssss sss sss ssn srr 3.2 Chemical System ................ -- svsvsrmmsassseeserasassessen -- 3.2.1Test Substance........... -- assssererassseeeressss wens 343.3 Pats Obst Test Conduct....... aet nAa AAAA AAS wesnsnmmmmerseesssssssssnerees 8 3.6 ValidityCriteria ofthe Study. wasnsm--" essere sme 4.0 Resultsand DISCUSSION .......cuuvuverrereres rasan wsnsnsnsa------------ 5.0 CONCIUSIONS ..vvvvevevsssssssssssssssssssssases sees csiam-- essen ees 8 6.0 RetoefRn ecotrdi s...o ....n ..... se-------- esssssnsnsnsnsnene wd 7.0 DisopfToess tItaem.l.. ----------" wsssrerererasssereeessesss mS ~-- Tables FAipgpuernedsices DO i `SOLUBILITY atryorAsKate, RD. dydein RoDbaeyr. BCuockr,aPh,.DP.AD. 1.0 SUMMARY Tow yes hever sony o EEE... ~~ determined in aqueous solution at 12 C, 25 C, 37 C and 60 C Tsing a. elmer Reson Program company Stan. Does econ,TSCACT! ~~ variation of OECD method 105. The experimental mixture was shaken for at least three days and the test substance concentration determined at various intervals via gas chromatography mass spectrometry. Findings: The solubility in water was 134 pg/L (+/-29 pg/L) at 12C ; 137 (+/-53 pg/L) at 25 C; 318 pg/L b (+/-176 pg/L) at 37 C, and 225 pg/L (+/- 51 pg/L) at 60C. Conclusions: eso SE C10 60C is very low (134 to 318 ug/L). 1 2.0 `GENERAL STUDY INFORMATION ~~ Study Objectives `The objectivesofthis study were to: + Determine the water solubility between 12 C, 25 C, 37C, and 60 C in pure water. + Determine the effect of pH on water solubility at 12 C, 25 C, 37C and 60C. Test System Justification The test system was selected by the sponsor. Study Personnel TDuebtCaapNootmeeCnr forAnyi Sines iin 30, lsgow, Dela, I7H-G101 USA Nnmgemen: ine Mar, PAD. SudyDiscor MarAy Kar, PhD Durer Company ~ Tome essa rogram LS ---- : ~~ Principle Investigator: Daryl P. Cobranchi, Ph.D. DuPont Company CScoirepnocreaste Center for Analytical `Technical Personnel: Barry W. Wolstenholme Study Execution Dates Study Initiation Date: 15-1n.2001 Experimental Sart Date: 15-1200 Experimental Completion Date: 28-June 2002 Study Completion Date 12-uly2002 3.0 MATERIALS AND METHODS -- 3.1 "cTToehnsectesnoGtluruibaditleiioltniynoiefnstwhaetesrubosftaasnucebsitnawntceerisasnpdeciisfaiefdubncytitohen soafttureamtpieonramtaes,s The Solubility in wate isspecified in nits of weight pe volume ofsolution. The Slant is kg/m'; g/l may also be used. 32 Chemical System 321 TTheesttSesutbssutbastnacnece was obtsind rom Clariant Gib (Germany) a was re eviangadsochromatography. RThIe major impubritey JsEsNeNEsREnvasgneatnivealiye. Name: Synonym: Active subsance(s) CAS Name: CAS Number(s): Tomer Research Program Company Saniized. Doss not contain TSCA CBI . ~~ Structure: H Number H-24691 Lot Number: _ EMSE Sample Number. E93386-63 -- Concentration, nominal: Concentration, analyzed: an Certificate of Analysis Date: 03-Apr. 2001 Date Received: 15-June 2001 Vapor pressure: 0.023 mm Hg Suabiliy: Stable at ambient room temperature Appearance/Color: White solid Storage Conditions: Room temperature; keeptightlyclosed 322 Test Vehicle The est substance was dissolved in ulrapure water (17.6M0-em). 3231 Test Units 3T2esmt mveslseenlgsthw.erVeia2lmcLaps(nwoemrienabll)uebocraopssilwiicattheTgelfaslsonvialfsl,u1o2rompomlyomuetrerredsiianmaentedrrbedyTubber septum caps. _ 3232 Test Conditions Test solutions were kept closed during the dissolution and shaking process. STelomer Research Program Company Saniizer. Rss not contain TSCA CB s ~ 33 T1e2sCt,aCt2o5e%nr,ds3u7cttCssndof6i1S C"Exc cst subI siandswasplacecdriinI av2smd.ians ed "ctharkoemratbolg.raTphey tsasmpslevaisnsncd.oshnakeset cnownaastsatmnteiatseoumrpeendrataturveafroiro2s4 ihmoersneornves ttyecgtaisocnh,ommlasto~4g6r3p).hyInvtihtehsmeacosndpmeectthroodmseideoedoenf(iFnleewcoan orpasct,(E) cro smLeltass0g0sct hromatogavpiI y The vlwasconwtdewi0the exces c C bane mdcI onsethvesctR t d isavncecntR ovtoemcotle uspR poimcssefhe \Vielm.peTrhsaerve.ilUwlarssptuherne rceonmdouvcetdifviotmy otfhe1w7.a6rMmsEurf)scewaatnedrawasladltodcooetmwhdee(0eilodo50m Lhotconvorhethaedsvpiaacebwefaosrevsacallineg.. TThheevisaillwcosne-lraucbebdeoindetfhehrmeosvtiaatlecda,piwnassiluedne phraokxeimbatlelayt t1h0e0tpemmfporearfoasfttneufosrutre.dysT.heAsabalmeplreowaans rraetmeowvaesd ofto \edmcpeiracrmebsyiGhnEMerSd.oThmissmetoohsogadimsprlmrahepyfasnhtdtihaentehtesfibssmaentehowdasand gives -- thesameresult. DetailsoftheGC/MSexperiment + V5ilm:TcrgeDNPe(otsa] Spoise),VoIl., 210m5LE.scaFpatlc,obnsoResd,eQugrise,v1n2,mePAm1o6s55d1iUmSAe.rby + cVianlcpm:aTnreeCD0I01G.lpurpose) bs Seine 20 Fat Pows Rod, QcapuwaiiT,oPAo18a95d1rUdSAb,bcaelsogtmumnbNeoroCrI00015 + + auesnCo:ro9m9a9t9o9g%rappahrae,dpMlaumsbeSdpewictthomsslteesHsP lsoawAngceonp)eSrbicngMPGosgdseschirosmaNteowgarrakp,h DnEd {1rowoAwwAlg)o76)73$G7C3imfsrstloiwsdAegicorT(eMcShDn)liogtih, 21s5050mCpeerai oRoosd,Weiygatnodn7, DF + Cu19s80c8,hrUomhatograph et: MerlinMocs,Merkin nunca Company, HalfBay, CA 94019 + NVaUAlSgR,encpeotlpiornbrneaty,lr3n11s5010mGorsbein Pasksa,yrWemsVtICVhEi,s1,31P0AGo1s9h3e8n0 UaSvA,amodWees16Ch0eAst, PA --_ + Th115e358m800olUUySmAe,Bwiigleremipleraineacsohanlleaedta1l2e0d0yp,.VISR,i1e3c10oGneeBn Praveya,WentChneLstSer PA Teme ResearchProgram Company Sanitized. Dons not contain TS.CA CBI ~ cooingunit, Brinkmann InstrumentsIn.OneCantiagueRoad,POBos 1019 Westbury, NY 11590 USA. GC/MS conditions: + Oven temperature: B0C for one minute increased at 20C/minute to 300C and held for 10 minutes Run ime 22 minutes. + njector: spies, 25C, purge flow S00 mL/min, purge im 0.70 mimics, saver ow 20 mmioute, 3 sample washes, no pup (quiescent), 1 infection size, (10 kL Agilent syringe), ree post injection washes with JT Bakerulrarsianalyzed cat 9263-03) methanol, sampling depth 10.0 `mmsbove the nominal positon. + Solvent delay: 5.0 mints i, detetucrnetdonoafrtr five minutes) Tons:4630, 131.0, 95.0, 63910(0prefe, rred) Ean Column: Restck RTX-200 (cifloropropylmethy]polysloxane), 60 mete, 250 an diameter, 1.00 im UiSmA.tiIcnkiotieaslsf,lcoawtasleogattu1m.bmeLr/m1i5n0u3t6e,,RceonssetanCtorfploorwa,tinoan,l1n10eBtepnrneesrsuCrierl2e5,.8B9elplsie,foanvteer,aPgeAve1l6o6c2i3ty + L3i1mcitmsofeeDetection (LOD) approximately 20 ppb; imiofquantification (LOQ) approximately 50 pb. 34 Parameters Observed ~ "sTohleuptieoankaatrsepaecoirfhiicgtehmtpewraastumrese. asfourtrheetedst substance satuinrthaeatqueeodus 35 ResultAnalysis "sTahmeeppeaarkahmeeitgehrtoorfapesataknadraeradocabraeifnuelldyfporretphaerrteesdtisnubmsettahnacneolw.as compared fo the 36 Validity Criteriaof the Study a"Tnhdeatfesetrretshuelttesstwesrubesctoannsciedwereerdevwailtihdinft5h%eopfetahkeapreaarsaomfettheer smteaansduarredds.run before: 37 Guideline Deviations Deviation 1 Conceming: ~~ Additionofthe est substance tothe vessel Deviation: "tThheetteessttvsesusbesl,tance was costed on the wall of Reason: Tlihkee s"terxuccetsurse"s,tewsthiscubhsitnatnecrefefroerdmweidthnetehdele- chromatographic injection. Impact on Study: None Pe Deviation2 Conceming: ~~ Choiceoftest method Deviation: The "flask" method recommended for 7Telomer Research Program Company Sanitized. Dass >t contain TSCA CBI 7 ~ ucsoemdporautnhdersthhaavnitnhges"olcuobliulimtny e>lu1t0iopnpm was `mceotmhpoodu"ndwshihcahviinsgresocloumbimleitnyd<ed10foprpm. Reason r"eTlhiea"blceolthuamtntheelu"tfiloanskm"etmheotdh"odifloersvsolatile compounds. : Impact on Study: None 4.0 RESULTS AND DISCUSSION `Table 1 summarizes the solubility data versus temperature. wTihtehsnoolusbiiglnitiyfaitcapntHd3i,ffpeHren1c1eainndthaeustoolguebinleiotuysfopHL(5.8) at 12Cwere megsvuerretdhe pH range. Table 2 through 7 summarize the measi 1 versuspH determinations. Tpgh/eL)solatub2i5litCy;in31w8atuegr/aLt (1+2/-C17i6su1g3/4L)pgat/L37(+/C-,29anpdg/2L2)5; p1g3/7Lp(g+//L- 5(1+-u5g3/l) at 60 C. Varying pH from 3 to 11 had no impact on the solubility ~ measurement. 5.0 `CONCLUSIONS "aThces.olubilityo sinthe 100to 250ug/lrangefrom12Cto STelomer Research Program Company Sanlized. Doss not contain TSCA CBI 8 -- 6.0 RETENTION OF RECORDS SExtpuedryidmoenctuamlenSttsatainondimnactleurdiianlgs wbuitlnboet sliomrietdedintot:he archivesofthe DuPont study protocol; any protocol andlor report amendments or addenda or deviations; allrw datz; + onIaeboroartiogriyn-aslpseicgifniecdocrospiytoef-tspheeciffiicnarlarwepdoartta; such as personel files, instrument, equipment, refrigerator, andlor freezer raw data. 7.0 DISPOSAL OF TEST ITEM ADotfuhtPeeorrnaitrsrsGualanangsceegmooefwnttshsietaerfeuinnmtaialldrieetpsoberetxt,pwitrehaeetniroetnhmeadaistnpeionnagsnodtretsathnesdnubdtsehtesatTnrecoseytewdFialbcliylbiebtuy.srtnoirnegd, autntlheess 8.0 REFERENCE 1. OChEeCmiDcaGluipdreolpienretsifeosrTtehsetTNeos.ti1n05go:fWCahteemriScoalulbsi/lSietyc,taidoonpt1e: dP1h2ysMiacayl-1951. ~ (published uly 1995) Table 1 Water Solubility versus Temperature (C) at Autogeneous pH [ [2 as 7 1 a7 | =x1s | sa 176 [47] Tio] --_ [n=Cnu6m0bofteesrt1 s 226 | 51 Tio] 9Telomer Research Program Company Saniized. Docs notcontain TSCA cay 5 Table 2 Water Solubility versus pH at 12C Cs I 2r ulogeneouspH=58| 104 I do | 67 Tl [6] C1--Tm12 15] n= number of tests --~ 10Telomer Research Program Sompany Sanitizod. Does nol contain TSCA CBI 10 ~ Table 3 Water Solubility Raw Data : Autogeneous pH 5.8, 12C Slope Intercept [Std Dev It [5% UCL [95% LCL [Average 238.61) Sample Area Conc. (ppb) 6555.5 1 36,712 126 [2 132865] if | [3 [8141 29) [4 12e0a7| 90| 3 44510 [160| 23646 [6 [oreo 129| 18 [ |o 7 | 0 | 108] 98 51,133 38660| 135 10 [] 0 134 ppb [Peak Area used for quantitation In = number of determinations ~~ UCL = Upper Confidence Level (ppb) LCL = Lower Confidence Level (ppb) --_ 11Telomer Research Program Company Sanlized. Does not contin TSCA CBI n ~~ Table 4 Water Solubility Raw Data : Autogeneous pH 5.8, 25C [Stops Intercept [Std Dev it 195% UCL [95% LCL. [Average Set Set2 29948) | Sample |Peak Height| Peak Height| Conc (ppb) 9 1 511 595 185 [2 |"a0[sw Hee | [~--~ 1 1 53 [a aTp ma0 Aas | [5 "ea [a| oAs ra | 29798 [6 | dor | eee | Ais] 64 [7 | 450 | eos | 78 | 09) [8["d 200 | o es | [eo [208 180 137 ppb [0] - 54 | te | ~~ [Peak Height used for quantitation [*Peak too high to measure. Solid probably included in injection. In = numberof determinations UCL = Upper Confidence Level (ppb) [LCL = Lower Confidence Level (ppb) --~ 12Telomer Research Program Sompany Saniized. Boos nat conte' TSCA CBI 2 rm Table 5 Water Solubility Raw Data : Autogeneous pH, 37C [Siope 100332 [ Sample| Area Cone. s {ppb} intercept 642.42 1 4207 355 [Std Dev ho [95% UCL [95% LCL Average 176][a1[ S2083 | 2250 5 5| qo [5 [2|0i8 4T5| 22622 6 [2660| 201 | 444] 7 1828 192] [8 [3991 334 [9 [sero 521 318 ppb [Ho T7ee| "&0 | [Peak Area used for quantitation In = numberof determinations ~~ LUCCLL == LUopwpeerr CCoonnffiiddeennccee LLeevveell ((ppppbb)) -- 13Telomer Research Program `Sompany Sanitized. Doss not contain TSCA CBI 1 ~~ Table 6 Water Solubility Raw Data : Autogeneous pH, 60C [Standard run before [S_am_pl[e |SAereta|t[ArSeae|tCzon2c.]|] landafter each [95% UCL [65% LCC [5--[3otriasas2e8sse|| sample. 1 |4sos00|3se225| (2p0pb7) |__2 [289007]266224] 196 | 319066| 273785| 219| 225266| 226886] 175 20] [5 [276743] 263077] 214 [6 [335225]240121 249) 201) |_8 [180304|326528288|| [fo [285294 [212958 ~~ I[nP=eankuAmrbeearuosfeddeftoerrmqiuannattiitoantsion ULCCLL == LUopwpeerrCCoonnffiiddeenncceeLLeevveell ((ppppb)b) 1Telomer Research Program Zompany Sanlizod. Doss ict contain TSCACEN w ~~ Table 7 Water Solubility vs. pH Raw Data at 12C [So:C e ToqSssameon Per5%otGone2A5dooh aSse uLooLt I ms3 IH"% h"2ii1e7 5 Ir or remem | Soyme iSEogarr 575 2Tu1os7r sSosbuoort wolo asSaoir ::7 s7I Eaves Top] ~~ So5 e HTn | Sample pH Pe 5:akHeight 57 Conc.(ppb | oSsseuoot WAonnbh TpoHuir 1i:s i bov:nsussd Fr aversge wap |] [Peak Area used for quantitation In = number of (determinations JUCL = Upper Confidence Level (ppb) LCL = Lower Confidence Level (ppb) ~ Whose Sse ogre Zomoany Sanitized. Doss ne' conta'n TSCA CBI is ~~ Appendix A o Chemical iia il 8 H-24691 Analysis Summary The subject material was analyzed by gas chromatography using a standard method to assess its composition. This analysis showed that the material comprised] f the subject material. Thebalances not a limitofqu: of .02%. Further analysis by. Suggests fi single impurity, whose chemical structure i Chro Finally, any the subject - Tandem material Ma: was evaluated by High Performance Liquid C/MS/MS) for the presence of t a detection limit of ppm. Neither material was observed to be present Based upon these analyses, we determine and confirm the composition conclude that of H-24691 to methods are in be as follows: hand to ~ Material Wt. % (+0.3) 16Telomer Research Program Aa Sanat pian net nig Ter ray ~ Appendix B Solubility Determination- Modified ASTM Procedure 1. A concentrated (~50% w/w) solutionof 8-2A in GC grade methanol was prepared. 2. Approximately 200 uL were placed into a standard screw-cap GC vial 3. The open vial is placed in awarm locationto evaporate the solvent 4. After the methanol had evaporated, the 8-2A was observed to collect on the upper surfacesofthe GC vial 5. The vial was then removed and allowed to cool to room temperature. 6. Ultrapure]8 MQ water was carefully added to the vial, filling it all the way to the top (litle or no headspace). 7. The septum was tumed upside down so that the silicone rubber side was facing towards the solution. 8. The vials were then capped and placed in a temperature controlled shaker table operating at ~100 rpm. 9. The vials were shakenfor a minimumof 4 dayspriorto analysis. 10. The vials were then removed to the GC/MS auto-sampler tray, temperature ~~ controlled. 11. The GC/MS was calibrated against 8-2A samplesprepared in methanol. -- 17Telomer Research Program Company Sanitized. Docs not contain TSCA TE "