Document KG33w13Y60GJNobZ59dBn3NK0

3M SPECIALTY ADHESIVES & CHIEMICALS ANALYTICAL To: Leo Gehlhoff-(309727)-3M Chemicals-236-2A-01 LABORATORY Request#'s53030 From: Tom Kestner-(3-5633)SA&C AnalyticaLlab -236-2B-1I Subject: F7uorochemical Isomer Disoibutionby 19F-AMR Spectroscopy Date: December 1, 1997 SAMPLE DESCRIPTIONS: * FC-95, lot# 217 (T-6295);Nominal product= CgF17-SO3(-) K(+) INTRODUCTION: This samplewas subjectedto a '9F-NNM spectraalnalysimsethod to detern-dnteheidentitieasnd relative concentrationosf thefluorochemicailsomersand as many otheridentifiabilmepuritycomponents as possible. EXPERIMENTAL: A portionof thesamplesolidwas totafldyissolvedinDMSO-d6and thena 376 NiRz 'T-NNM spectrum (F53030.401)was acquiredusinga VarianUNITYplus 40OFT-NMR spectrometer.AidaRobbins preparedthesampleforanalysisand shealsoacquiredand plottedtheNMR spectrum. RIESLIILTS: The '9F-NMR spectrumwas used to determinetheidentitiaensd relativceoncentrationosf thenominal fluorochen@cailsomersand threeotherimpuritycomponents inthissample.The qualitativaend quantitativceompositionarlesultwshich were derivedfrom thesingletria'l9F-NMR spectraalnalysiasre summarized inTABLE-1 on thefollowingpage. A copy oftheNMR spectnunand thespectraalssignmentsdatapage areattachedforyour reference.If you have any questionsabouttheseNMR resultsp,leaseletme know. I apologizeforthedelayin completingthiswork. Tom Kestner c:Jim Johnson- EE&PC - 2-3E-09 FileRefc=ce: LG53030.DOC/43 De=nber 1,1997 SA&C AnalyticaLlab Request4 53030 TABLE-1 Sample: T-6295 (FC-95,Lot 217) "F-NNIR CompositionalResults StructuralAssignments 19F-NMR RelativeMolel/oConcentrations CF3(CF2),.-SO3K((-+)) (Nomialchain,wherex isrnaird7y) CF3(CF2),,-CF(CF3)-(CFS20@3-(-)K(+) (Internamlonomethylbranch, where x+v ismainly5.and x # 0,y ;t0) (CF3)2CF-(CF2S)0.3-(-)K(+) (Isopropyblmncl4 wherex ismainly5) C,F2,,,,-CF(CF3S)0-3(-) K(+) (Alphabranch,wherex ismainly6) Rf-CF2-SF4-F (CF3)3C-(CF2S)0.3-(-K)(+) (t-butyblranck wherex ismainly4) CF3-(CF2).7C(CF3)2-(CFS20@3-(-)K(+) (interngaelm-dimethyblranchw,herex+yismainly4,andx 0) PossibleCF3-SO3(-)K(+) PossibleCF3-CO2(-) K(+) 70.0% 17.0% 10.3% 1.6% 0.35% 0.23% 0.15% 0.25% 0.05%