Document a1Md9xyV6q46MR8QXRdvr0n8X
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%