Document oeyqvDwrgzOE7MKGgE8EMdgy8

&tfGt' fa> iooosnyAP* \ 3M SPECIALTY ADHESIVES & CHEMICALS ANALYTICAL LABORATORY ' To: ' From: Leo Gehlhoff- (309727) -3M Chemicals - 236-2A-01 Tom Kestner - (3-5633) SA&C Analytical Lab - 236-2B-11 Request # 's 53030 ARXU-05CM Subject: Fluorochemical Isomer Distribution by 19F-NMR Spectroscopy Date: December 1, 1997 SAMPLE DESCRIPTIONS: * FC-95, lot # 217 (T-6295); Nominal product = CFi7-S03(-) K(+) INTRODUCTION: This sample was subjected to a 19F-NMR spectral analysis method to determine the identities and relative concentrations of the fluorochemical isomers and as many other identifiable impurity components as possible. EXPERIMENTAL: A portion of the sample solid was totally dissolved in DMSO-d and then a 376 MHz 19F-NMR spectrum (F53030.401) was acquired using a Varian UNITYplus 400 FT-NMR spectrometer. Aida Robbins prepared the sample for analysis and she also acquired and plotted the NMR spectrum. RESULTS: The 19F-NMR spectrum was used to determine the identities and relative concentrations o f the nominal fluorochemical isomers and three other impurity components in this sample. The qualitative and quantitative compositional results which were derived from the single trial 19F-NMR spectral analysis are summarized in TABLE-1 on the following page. A copy of the NMR spectrum and the spectral assignments data page are attached for your reference. If you have any questions about these NMR results, please let me know. I apologize for the delay in completing this work. Tom Kestner c: Jim Johnson - EE&PC - 2-3E-09 File Reference: LG53030.DOC/43 CG0778 December 1, 1997 SA&C Analytical Lab Request # 53030 TABLE-1 Sample: T-6295 (FC-95, Lot 217) 1S>F-NMR Compositional Results Structural Assignments `T-NM R Relative Mole% Concentrations C F 3(C F 2V S 0 3(- ) K (+ ) (Normal chain, where x is mainly 7) C F j iC F ^ - C F iC F a H C F ^ - S 0 3(-) K (+ ) (Internal monomethyl branch, where x+y is mainly 5, and x * 0, y * 0) (C F 3)2C F -(C F 2)X- S 0 3(-) K (+ ) (Isopropyl branch, where x is mainly 5) CxF 2x+i-C F (C F 3)- S 0 3(-) K (+ ) (Alpha branch, where x is mainly 6) R f- C F 2- S F 4- F (C F 3)3C -(C F 2X - S 0 3(-) K (+ ) (t-butyl branch, where x is mainly 4) CF3-(CF2)x-C(CF3)2-(CF2)y- S03(-) K(+) (Internal gem-dim ethyl branch, where x+y is mainly 4, and x * 0 ) Possible CF3-S 03(-) K(+) Possible CF3-C 02(-) K(+) 70.0% 17.0% 10.3% 1.6% 0.35% 0.23% 0.15% 0.25% 0.05% 000773