Document B5Xqyvbx438zXKaXRwdpgEyQ4

/|R Z26-037 MELTING POINT TEST SUBSTANCE Identity: N-ethylperfluorooctane sulfonamidoethanol; may also be referred to as N-EtFOSE Alcohol or FM-3422. (1-Octanesulfonamide, N-ethylI.I^^.S.S^AS.S.e.ejJ.S.S.S-heptadecafluoro-N-^-hydroxyethyl)-, CAS #1691-99-2) Remarks: Material is an off-white, waxy solid of uncharacterized purity. It was characterized as being stable at room temperature. METHOD: Method follow ed: OECD Guideline No. 102 (capillary/metal block) using a Buchi B-545 Melting Point Apparatus. GLP: No Year study was perform ed: November 19,1999 R em arks: A glass melting point capillary was filled to a height of about 1.5 cm with the test substance, packing it down with a stainless steel rod. The instrument was set for 20C/min heating rate in order to determine the approximate melting point (56C), as determined by the instrument's automatic melting point detection (based on optical transmission). Next the instrument was set for 0.1C/min heat rate, starting at 54C. There was no sign of decomposition or sublimation of the sample. The Buchi instrument was last calibrated on November 2,1999, using Vanillin (mp 81.5C), Phenacetin (mp 134.6C), and Caffeine (mp 235.9C) melting point standards. The measured melting points for Vanillin and Phenacetin were within the 0.2C accuracy specification of the standard samples. The Caffeine melting point was measured at 235.4C, so the instrument's high-temperature calibration point was adjusted at that time to agree with the 235.9C standard value. The recommended calibration interval is 1 year. RESULTS________________________________________________________ The automatic melting point detection at 0.1C/min showed a melting point of 59.6C. However, the sample was visually observed to have a melting point range, starting at 55C and finishing at 60C, with most of the melting occurring at 59.6C. 006193 CONCLUSIONS The fact that melting occurred over a range indicates the likely presence of impurities. DATA QUALITY_______________________________________________ R eliability: Klimisch ranking = 2. Sample purity was not sufficiently characterized. No information on the production lot number of the sample was provided, nor was any information on the purity of the substance indicated. Testing will be redone using a purified sample if purification can be properly done. Experience has concluded that purification generally leads to a reduction in the concentration of higher and lower molecular weight homologues, as well as, potentially, a change in the relative composition of the isomers. REFERENCES___________________________________________________ 3M Internal Correspondence from Steven P. Brinduse, SMMD Analytical Laboratory, Subject: Melting Point of N-Ethyl FOSE Alcohol, November 22,1999 OTHER___________________________________________________ Subm itter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 Last changed: 5/18/00 006194 3M Internal Correspondence To: Scott B. Strand, 3M Environmental Technology & Safety Services 778-7644, Building 02-3E-09 From: Steven P. Brinduse *236-2B-11* 736-1007 736-6377(fax) SMMD Analytical Laboratory Date: November 22, 1999 Subject: Melting Point of FM-3923 N-Ethyl FOSE Alcohol A sample of FM-3923 was submitted for measurement of melting point. Melting Point was determined using a Buchi B-545 Melting Point Apparatus. A glass melting point capillary was filled to a height of about 1.5 cm with the test substance, packing it down with a stainless steel rod. The instrument was set for 20C/min heating rate in order to determine the approximate melting point (56C), as determined by the instrument's automatic melting point detection (based on optical transmission). Next the instrument was set for 0.1C/min heat rate, starting at 54C. The automatic melting point detection showed a melting point of 59.6C. However, the sample was visually observed to have a melting point range, starting at 55C and finishing at 60C, with most of the melting occurring at 59.6C. There was no sign of decomposition or sublimation of the sample. The Buchi instrument was last calibrated on November 2,1999, using Vanillin (mp 81.5C), Phenacetin (mp 134.6C), and Caffeine (mp 235.9C) melting point standards. The measured melting points for Vanillin and Phenacetin were within the 0.2C accuracy specification of the standard samples. The Caffeine melting point was measured at 235.4C, so the instrument's high-temperature calibration point was adjusted at that time to agree with the 235.9C standard value. 4 006195