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3M SPECIALTY ADHESIVES & CHENUCALS ANALYTICAL To: Leo Gehlhoff-(309727)-3M Chemicals-236-2A-01 LABORATORY Reques#t's53030 EEQM@ Tom Kestner- (3-5633)SA&C AnalyticaLlab -236-2B-II Spbiect: I-7uorockenucalIsomer Distnbution by 'PF-NMR Spectroscopy Date: December 1,1997 SAMPLE DESCRIPTIONS: FC-95,lot# 217 (T-6295);Nominalproduct= CgF17-SO3(-K)(+) INTRODUCTION: Thissamplewas subjectedtoa '9F-NMR spectraalnalysimsethod to determinetheidentitiaensd relative concentrationosf thefluorochemicailsomersand asmany otheridentifiabilmepuritycomponents as possible. EXPERIMIENTAIL: A portionofthesample solidwas totalldyissolveidnDMSO-d6 and thena 376 NIRZ 19F-NMR spectrum (FS3030.401)was acquiredusinga VarianUNITYplus 400 FT-NMR spectrometer.AidaRobbins preparedthesample foranalysiasnd shealsoacquiredand plottedtheNMR spectnan. RESULTS: The '9F-NMR spectrumwas used to determinetheidentitiaensd relativceoncentrationosf thenominal fluorochemicailsomersand threeotherimpuritycomponents inthissample.The qualitativaend quantitativceompositionarlesultwshich were derivedfrom thesingletria'l9F-NMR spectraalnalysiasre summarized inTABLE-1 on thefollowingpage. A copy of theNMR spectrumand thespectraalssignmentsdatapage areattachedforyour reference.If you have any questionsabouttheseNMR resultsp,leaseletme know. I apologizeforthedelayin completingthiswork. Tom Kestner c:JiznJohnson- EE&PC -2-3E-09 FileReference:LG53030.DOC/43 Do=@ber 1,1997 SA&C AnalyticaLlab Request# 53030 TABLE-1 Sample: T-6295 (FC-95,Lot 217) '9F-NMR Composibonal Results StructuraAlssignments 191@-N-MRRelativeMole/o Concentrations CF3(CF2).-S03(-) K(+) (Normalchain,wherex ismainly7) CF3(CF2).-CF(CF3)-(CF2S@0-3(-)K(+) (Internamlonomethyl branch, where x+y ismainly5,and x ;t0,y # 0) (CF3)2CF-(CF2S)0.3-(-)K(+) (Isopropyblranch,wherex ismainly5) C.F2,,.,,-CF(CSF033)(--)K(+) (Alphabranch,wherex ismainly6) Rf-CF2-SF4-F (CF3)3C-(CF2S)0.3-(-K)(+) (t-butbyrlanch,wherex ismainly4) CF3-(CF2).-C(CF3)2-(CFS20@3-(-)K(+) (Interngaelm-dimethyblranchw,herex+yismainly4,andx 0) PossibleCF3-SO3(-)K(+) PossibleCF3-C02(-) K(+) 70.0% 17.0% 10.3% 1.6% 0.35% 0.23% 0.15% 0.25% 0.05%