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AR22>-D0% PROTOCOL DETERMINATION OF THE MELTING POINT/MELTING RANGE OF PFOS OECD Guideline for Testing o f Chemicals, 103 Melting Poinl/Melting Range 3M Lab Request No. U2723 Submitted to 3M Corporation Environmental Laboratory P.O .Box 33331 St. Paul, Minnesota 55133 Wildlife International ltd 8598 Commerce Drive Easton, Maryland 21601 (410) 822-8600 December 2,1998 PROTOCOL NO.: 454/120298/103/SUB454 3M LAB R E Q U ^ S g N O .^ 2 3 W il d l if e In t e r n a t io n a l l td . 2- - DETERMINATION OF THE MELTING POINT/MELTING RANGE OFPFOS SPONSOR: 3M Corporation Environmental Laboratory P.O .B ox 33331 S t Paul, Minnesota 55133 SPONSOR'S REPRESENTATIVE: Ms. Susan A. Beach TESTING FACILITY: W ildlife International Ltd. 8598 Commerce Drive Easton, Maryland 21601 STUDY DIRECTOR: Ronda Jacobs Senior Chemist LABORATORY MANAGEMENT: W illard B. Nixon, Ph.D. Manager o f Chemistry FOR LABORATORY USE ONLY Proposed Dates: Experimental Start Date: __ Experimental / O 'N <r o / s ' J^PQ- 1 0 __________ Termination Date: -- LAL--(2LSL--L Project No.: tC )C p_______ Int/Date: __------------------------------------ Test Substance No.: ____________________ Receipt Date: -- 9 O c T ------ PROTOCOL APPROVAL SPONSOR'S REPRESENTATIVE PROTOCOL NO.: 454/120298/103/SUB454 n L. 9? DATE /Mf DATE /A 17 DATI 3M LAB REQUEST NO. U2723 000047 W il d l if e In ter n a tio n a l ltd . -3 - IN T R O D U C T IO N W ildlife International Ltd. will determine the melting point or melting range o f PFOS (perfluorooctane sulfonic acid, potassium salt). The study will be conducted at the W ildlife International Ltd. analytical chemistry facility in Easton, Maryland. The study will be performed following procedures in OECD Guideline for Testing of Chemicals, 102, M elting Point/Melting Range (1). Raw data for all w ork performed at W ildlife International Ltd. and a copy o f the final report will be filed by project number in archives located at W ildlife International Ltd. or at an alternative location to be specified in v' the final report PURPOSE The purpose o f this study is to determine the melting point or melting range o f PFOS. EXPERIM ENTAL DESIGN The m elting point is defined as the temperature at which the phase transition from a solid to a liquid state at atmospheric pressure occurs. For some substances, the transition occurs over a range o f temperatures defined as the melting range. Subsamples o f the test substance will be heated in a melting point tube in a temperature-controlled heating block containing a melting point capillary. Measurement o f melting points will be limited to s400C (approximately 673 K), the maximum specified for the instrumentation used. The temperature at which fine droplets adhere uniformly to the wall o f the melting point tube will be accepted as the melting point If a range o ftemperature is noted between the formation o f the fine droplets (beginning o f melting) and transition to a liquid (end o f melting), a melting range will be reported M ATERIALS AND M ETHODS Teat Substance The Sponsor will be asked to provide the following information concerning the test substance, if available: Chemical Name (or designation) Lot or Batch Number Purity Composition (for multi-component mixtures) Empirical formulais) Expiration Date The attached form IDENTIFICATION O F TEST SUBSTANCE BY SPONSOR (Appendix I) is to be used to provide available information. The Sponsor is responsible for information on the purity and composition o f the test substance, as well as all information related to the safe handling o f the test PROTOCOL NO.: 454/120298/103/SUB454 3M LAB REQUEST NO. U2723 000048 W il d l if e In t e r n a t io n a l l td . -4 - substance. The Sponsor also agrees to accept any unused test substance or test substance containers remaining at the end o f the study. Test Procedure The melting point or range will be determined using a Bchi Melting Point B-540 instrument with melting point tubes supplied by Bchi. The instrument will be calibrated prior to use with a minimum of two reference standards. Subsamples o f the test substance will be transferred to a minimum o f three capillary tubes to a depth o f approximately 3 mm. Tubes will be tamped to pack the test substance. Following an initial rapid scan(s) to determine an approximate melting point, the instrument will be programmed to increment the temperature over the melting point or range at a rate not to exceed 1C/minute. The temperature at which fine droplets uniformly adhere to the tube wall will be accepted as the melting point If the temperature increases significantly (approximately 2C or more) between the formation o f the fine droplets adhering to the tube walls until liquification, a melting range will be reported. The melting point or range will be recorded in C and reported both in C and K. The barometric pressure will be recorded at the time o f measurement o f the melting point or range. Sample Handling and Safety The Sponsor will identify any special handling or safety precautions to be used with the above referenced test substance. A ll normal precautions with respect to handling and storage will be taken. Sample and Test Substance Retention U pon completion o f testing, portions o f the test substance used as part o f this study will be disposed o f in accordance w ith federal, state and local regulations. Any unused portion o f the test substance will be returned to the Sponsor. RECORDS TO BE MAINTAINED Records to be maintained for data generated by Wildlife International Ltd. will include, but not be limited to: .. 1. A copy o f the signed protocol. 2. Identification and characterization o f the test substance, if provided by the Sponsor. 3. Dates o f initiation and completion o f the study. PROTOCOL NO.: 454/120298/103/SUB454 3M LAB REQUEST NO. U2723 000049 W il d l if e Internatio nal ltd . -5 - 4. Dates o f experimental start and termination. 5. Storage conditions o f the test substance. 6. Test substance use log. 7. The instrument temperature program. 8. Individual and mean melting point measurements expressed in C and K. 9. Statistical calculations. 10. Test conditions. 11. A copy o f the final report. FINAL REPORT A final repeat of the results o fthe study will be prepared by W ildlife International Ltd. The report will include, but not be limited to the following, when applicable: 1. Name and address o f the facility performing the study. 2. Dates upon which the study was initiated and completed. 3. A statem ent o f compliance signed by the Study Director addressing any exceptions to Good Laboratory Practice Standards 4. Purpose and procedure, as stated in the approved protocol, including all amendments and deviations to the protocol. 5. The test substance identification, including name, chemical abstract number or code number, purity, composition, empirical formula, molecular formula, manufacturer's lotftatch number, dissociation in water, method o f analysis, or other information provided by the Sponsor. 6. Description ofthe test method or reference to the method used along w ith any modifications made. 7. Individual and mean values obtained for the melting point or range expressed in C and K. 8. Description o f any problems experienced and how they were resolved. 9. A statement prepared by the Quality Assurance Unit listing the dates that study inspections and audits were made and any findings that were recorded. CHANGING O F PRO TOCOL Planned changes to the protocol will be in the form o f written amendments signed by the Study Director and the Sponsor. Amendments will be considered as part o f the protocol and will be attached to the final protocol. Any other changes will be in the form o f written deviations filed with the raw data. All changes to the protocol will be indicated in the final report. PROTOCOLNO.: 454/120298/103/SUB454 3M LAB REQUEST NO. U2723 000050 W il d l if e Internatio nal ltd. 6- - GOOD LABORATORY PRACTICES * This study will be conducted according to the Good Laboratory Practices described in OECD (ISBN 92-84-12367-9) and EPA (40 CFR Parts 160 and/or 792). Each study conducted by W ildlife International Ltd. is routinely examined by the Wildlife International Ltd. Quality Assurance U nit for compliance with Good Laboratory Practices, Standard Operating Procedures and the specified protocol. A statement o f compliance with Good Laboratory Practices will be prepared for all portions o f the study conducted by W ildlife International Ltd. The Sponsor will be responsible for compliance with Good Laboratory Practices for procedures performed by other laboratories. Raw data for all work performed at W ildlife International Ltd. and a copy o f the final report will be filed by project number in archives located on the W ildlife International Ltd. site or at an alternative location to be specified in the final report. PROTOCOL NO.: 454/120298/103/SUB454 3M LAB REQUEST NO. U2723 000051 W il d l if e In ter n a tio n a l ltd. -7 REFERENCES 1. O rganisation fo r Econom ic Cooperation and Development. 102. G uideline'for Testing o f Chemicals, M elting Point/Melting Range. PROTOCOL NO.: 454/120298/103/SUB454 3M LAB REQUEST NO. U2723 000052 W il d l if e Internatio nal ltd. 8- - APPENDIXI IDENTIFICATION OF TEST SUBSTANCE BY SPONSOR ' To be Completed by Sponsor I. Test Substance Identity (name to be used in the report): Perfluorooctane Sulfonic Acid. Potassium Salt IWCC1 Sample Code or Batch Number: Lot 217____________________________________________ Purity (% Active Ingredient): 98.9%_____________ Expiration Date: 2008__________ n . Test Substance Characterization Have the identity, strength, purity and composition or other characteristics which appropriately define the test substance been determined prior to the start o f this study in accordance with GLP Standards? Y es___ No X HI. Test Substance Storage Conditions Please indicate the recommended storage conditions at Wildlife International Ltd. Ambient room temperature._______________________________________________________ Has the stability o f the test substance under these storage conditions been determined in accordance with GLP Standards? Y es____ No X Other pertinent stability inform ation:_______________________________________________ IV. Toxicity Information: M am m alian: R atLD 50 251 m e/ke Mouse LD50 N/A A quatic: Invertebrate Toxicity (EC/LC50) Fish Toxicity (LC50) Daphnia magna: 27m e/L__________ Raiflbow trQUt; 11 fng/L___ Daphnia magna: 50 me/L__________ Fathead minnow: 38m g/L Other Toxicity Information (including findings o f chronic and subchronic tests): See MSDS. ______________________________________________________________ PROTOCOL NO 454/170798/1OVSTTR454 T AO BOILING POINT TEST SUBSTANCE Identity: Perfluorooctanesulfonate; may also be referred to as PFOS or FC-95. (1-Octanesulfonic acid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-, potassium salt, CAS # 2795-39-3) Remarks: Testing was not conducted. Boiling point would be in excess of 400C. 000054