Document GKGg3EYVyOa35G4woqOgrr15N

DETERMINATION OF THE MELTING POINT/MELTING RANGE OF PFOS WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: 454C-106 ' OECD Guideline for Testing of Chemicals, 102 Melting Point/Melting Range ) AUTHORS: - Ronda L. Jacobs `Willard B. Nixon, Ph.D. STUDY INITIATION DATE: December 18, 1998 : STUDY COMPLETION DATE: February 24, 1999 Submitted to: 3M Corporation Environmental Laboratory P.0. Box 33331 ~ St. Paul, Minnesota 55133 WILDLIFE INTERNATIONAL LTD. Ea8s5t9o8n,CMoamrmyelracnde D2r1i6v0e1 (410) 822-8600 Page 1 of 12 HH 000032 WILDLIFE INTERNATIONAL LTD. 2 FROJCENOMSI C SPONSOR: `GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT 3M Corporation TITLE: Determination ofthe Melting Point/Melting RangeofPFOS. `WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: 454C-106 STUDY COMPLETION: February 24, 1999 "Thisstudy wasconductedincompliancevithGoodLaboratoryPractice Standardsaspublishedbythe US. Environmental Protection Agencyin40 CFR Part 792, 17 August 1989 and OECD PrinciplesofGood Laboratory Practice, OCDE/GD (92) 32, Environment Monograph No. 45, Paris 1992. STUDY DIRECTOR: " Ronda L. Jacobs, B. ~ Senior Chemist `Wildlife International Ltd. 24 #4 99 DATE 000033 WILDLIFE INTERNATIONAL LTD. "3 PROBCTNOA 4510 106 QUALITY ASSURANCE STATEMENT USS. En"vTihriosnsmteundtyawlaPsreoxteacmtiinoendAfgoernccoymipnli4a0ncCewFiRthPaGroto7d92L,ab1o7raAtuogruysPtra1c9t8i9ceanSdtaOndEaCrdDsaPsrpinucibpllesiofsbhyGoteohdde inLsapbeocrtaitoornysaPnradcatiucdei,tsOaCnDdEt/heGdDat(e9s2t)ha32t,anEnyvfiirnodnimnegnstweMroenroegproarptehdtNoo.th45e,SPtaurdiysDi1r99e2c.torTahnedLdaatbeosraotfoarlyl 'Managemeatwere as follows: ) DATEREPORTEDTO: Jr DATE CONDUCTED: STUDY DIRECTOR MANAGEMENT: Metin Pint Descqber18,1998 Decem18b,1e95r8 Deceaber 15,1998 DrfiReportundDia December1)99, Decembe23r, 199 Deceber 23,1998 FinaReport February1,1999 Febray1,199 Februny 1,199 pAMeo) LMianndaageRr.,MiQtucahleiltly,ABs.sSu.rance 2 Tonuary M99 DATE 000034 WILDLIFE INTERNATIONAL LTD. "ae TROFECTNG ASIC10% REPORT APPROVAL SPONSOR: 3M Corporation . TITLE: Determinationofthe Melting Point/Melting Rangeof PFOS. `WILDLIFE INTERNATIONAL LTD. PROJECT NUMBER: 454C-106 STUDYDIRECTOR: Ronda L. Jacobs. = `Senior Chemist MANAGEMENT: WildB Nox, PD. Manager, Analytical Chemistry DATE ~ stl -- 000035 WILDLIFE INTERNATIONAL LTD. ER `TOA F CB ONL TENE TS `Title/Cover Page ........ rrererrrererierere GoodLaboratory Practice Compliance Statement. . err es PROBCTNO; #51010 sstntisnrsmpios 1 ee 2 `ToafCb ontlene ts rrerenenas renner PT ssrser MeltingPointandMeltingRange .-... terres, rere 9 TABLE `Table 1 -DeterminationofMelting PointandMeltingRange for Perfl Sulu fono icAcr id,o Poto assic umSt alta (PFn OS)c ...... wereraee oy Appendix -PersonnelInvolvedinthe APPENDIX Study. . te 12 000036 WILDLIFE INTERNATIONAL LTD. -6- SUMMARY = 3M Corporation l| SPONSOR'S REPRESENTATIVE: Ms. Susan A. Beach Environmental Laboratory P.O. Box 33331 | ocanonorsor, sawona St. Paul, Minnesota 55133 ||AND ACOPYOFTHEFINALREPORT: WildlifeInternational Ltd. LL EastonM,aryland 21601 ___ PROIOT NOB 05 ] J WoLNERGTONLLD. PROJECTNUMBER: 454C-106 -- | [| TEST suBSTANCE: Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) [| stuoy: DeterminaotfitohneMelting Point/RMaengleotfiPnFOgS TEST DATES: _ Experimental Start - December 18, 1998 Experimental Term-iDencemabetr18i,1o99n8 [ProductCuemistryTest Results Med | (vevoronm: None, 400C,discolorationobserved "OECD 102_ 1 000037 WILDLIFE INTERNATIONAL LTD. -7- INTRODUCTION PROHTO:E454C01T06 `WildlifeInternationalLtd.attemptedtodeterminethemelting pointandmeltingrangeofthetestsubstance PFOS (perfluorooctane sulfonic acid, potassium salt). This study was condubycWitldelidfe International Lid. for 3MCorporation attheWildlife International Ltd.analyticalchemistry facilityin Easton, Maryland.The study was performed following procedures in the OECD Guideline for Testing of Chemicals, 102, Melting ' Point/Melting Range(1). Theexperimentalportionofthisstudywasconducted on December18, 1998. The originalrawdatageneratedbyWildlifeInternationalLid.and acopyofthefinalreportare filed underProject - `Number454C-106 inarchives locatedontheWildlife International Ltd. site. PURPOSE "Thepurposeof thisstudywastodeterminethemeltingpointandmeltingrange of Perfluorooctane Sulfonic: Acid,PotassiumSalt (PFOS) EXPERIMENTAL DESIGN Themelting pointisdefined as the temperatureatwhich the phase transition from asolidto a liquid state. atatmospheric pressureoccurs. For somesubstances, the transition ocours over arange oftemperaturesdefined asthe melting range. Subsamplesofthe test substancewere heatedin ameltingpointtubein atemperature- controlled heating block. Measurements of the melting point/melting range were limited to 400C (approximately 673K),themaximumspecificationfortheinstrumentationused.The temperatawhticuhrfiene dropletsadhere uniformly to the wallof the meltingpoint tubewouldbeaccepted as the meltingpoint. Ifa temperaturerangewasnoted between the formation of the fine droplets (beginning ofmelting) and transition to. `aliquid (endofmelting), ameltingrangewouldbereported. A Bichi MeltingPoint B-540instrumentwasused. 000038 WILDLIFE INTERNATIONAL LTD. 5. PROJECT NO.: 454C-106 MATER ANI D MA ETL HOS DS TestSubstance `Thetestsubstancewasreceived from 3MCorporation onOctober 29, 1998andwasassignedWildlife Intemational Lid.identificationnumber 4675 uponreceipt. Thetestsubstance, awhitepowder,wasideatified as: FC- Lot9Nu5 mbe,r: 217,ExpirationDate: 2008. Thetestsubstwaasnstcoreedunderambientconditions. Test Procedure ABikhiMeling PointB-540instrumentvith meltingpointtubessuppliedby BOchiwasused.The Bichi Melting Point B-540instrumcatwas calibrated andinspected just prouiseousirng anthraquinone and 1,8- `naphthalimide. - "The melting point and melting range determination attemptswere performedas follows. Subsamploefs thetestsubstance were transferredtofourmeltingpointcapillary tubesto adepthof approximately 3 mm. The tubes weretamped topackthetest substance. One subsample was subjectteod a rapid temperaturescanto determine an approxmeiltimngapotinet. An approximate meltingpoint could notbedetermined.The test `substance turned 2 lightbrowncolor and theablackened. Fine drowep re l note obst ervs ed.Theinstrumweants thenprogrammedtoincrement thetemperatureover rangeof 300to 400C at a ateof1C/minute. The nelingpointandrangedeterminationsforthe remainingthreesubsampleswereattempted. Atnotimeduring the testingof Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS)were fine droplets observed to adhere uniformly or otherwiseto thewallsofthe melting point tubes. The three remainingsubsarmeapctledeinsa similar mannerastherapidtemperaturescansubsample. The whitepowdertumedto alight brown.Asthe temperatureincreased,PerfluorSoulofconticaAcnide,Potassium Salt (PFOS) darkened until iteventually turned black. When approaching 400C, someofthetest substance losttheblackened color andturedto a clear, cryliksepatrticaulalte. The remainingtestsubstancestayedblack.Thebaropresmsuree watsrrecoridedcat the timeofthe melting point/melting range determinations. 000039 WILDLIFE INTERNATIONAL LTD. L- FROBETNG 4340106 RESULTS MelingPoint and Meling Range "Theresultsofthemeltingpointandmeltingrangedeterminationsarepresented in Table 1. Fine droplets `werenotobservedtoadhereuniformlyorotherwisetothewallsofthemelting pointtubes. Therefaomerltein,g pointra/ngemfoe rPelrft luoi roonctagneSulfonic Acid, PotassiumSalt (PFOS) was notdetermined. CONCLUSIONS Aproductchemistrytestwasperformed todeterminethephysicalcharacteristics ofthetestsubstance Perfluorooctane Sulfonie Acid, Potassium Salt (PFOS). Themeltingpoint/melting rangewasnotobservaend the cour lde notbf edeo terr mine ed. 000040 WILDLIFE INTERNATIONAL LTD. "10+ | REFERENCES PROJECT NO: 454C-106 1. OrganisationforEconomicCooperation andDevelopment. 102. GuidfeorlTiesntiengof Chemicals, 102: MeltingPoint/Melting Range. ) 000041 WILDLIFE INTERNATIONAL LTD. -u- PROMCTROZ ASICS Table 1 DeteofrMelmingPioinntanadMetltinigRaong nfor Perfluorooctane Sulfonic Acid, Potassium Salt (PFOS) _Sibmple SisDmple GAmmo)mt Repl 3 InGnsdieemt CC) 1 BaPrroesmseutei (am) 0 MePloiizg comin) None cbserved NRialgineg Cad K) Noa abserved Rep2 3 1 mm [-- None observed Rep3 3 1 mm None observed None observed -- ee 000042 WILDLIFE INTERNATIONAL LD. 12. PROJECT NO. 434C-106 APPENDIXI Personnel Involved in the Study "The followingkeyWildlifeInternatioLntadl. personnelwereinvolved in theconductor managementof this study: 1. WillarBd.Nixon, Ph.D., Manager, Analytical Chemistry 2 Ronda L. Jacobs, Senior Chemist 3. Keri Leach, Technician 000043 MELTING POINT TEST SUBSTANCE Identity: Perfluorooctanesulfonate; may also be referred to as PFOS or FC-95. (1-Octanesulfonic acid, 1,1,2.2,3,3.4,4,5,5,6,67.7.8,8.8heptadecafluoro-, potassium salt, CAS # 2795-393) Remarks: The test substance is a white powder. Sample was taken from 3M lot number 217. Sample was stored under ambient conditions pNrMioRr taontdesteilneg.menPturailtyandaeltyesremsinteedchtnoiqbuees8.0.49% by LC/MS, 'H-HMR, *FMETHOD Method: OECD 102 GLP: Yes Year completed: 1998 Remarks: Study utilized a Biichi Melting Point B-540 instrument, calibrated and inspected just prior to use sing anthraquinone and 1,8 naphthalimide. RESULTS Melting point value in C: >400C (No melting observed). Decomposition (yes-temperature C/ no fambiguous): No Sublimation(yes/no/ambiguous): No Remarks: Measurements of the melting point / melting range were limited to 400C, the maximum specification for the instrument used. Fine droplets were not observed to adhere uniformly or otherwise to the walls of the melting point tubes. CONCLUSIONS The melting point /melting range was not observed and therefore could not be determined. Remarks: While no meltingofthe test substance was evident, discoloration of the test samples was observed. The white powder tumed toa light brown and eventually black as temperatures rose. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 000044 DATA QUALITY Reliability: Kiimisch ranking 1. REFERENCES Study conducted at the requestof 3M Company by Wildiife International, Ltd. of Easton, Maryland. OTHER Last changed: 5/3/00 000045