Document K6ZbM8RYnrY3D4XGkaLe6xk36

41220 R. Howells GC/MS analysesofthesesampleswere accomplishedusinga 25 m X 0.32mm BP- IGC column to introducethesamplesintotheFinniganSSQ-70 mass spectrometerT.he samplecomponents were ionized usingchemicalionizatiownithmethaneasthereagentgas.The GC column was operatedfrom 40 to300 C ata rateoflo degreesperminute.The resultosftheseanalysescombined withtheircorrespondinGgC/FID area percentsshow thefollowing: Component I.D. L-10059 N.P, N-ETFOSE Lot W.R. N-ETFOSE Lot547 N-Ethyl-carboxamid(eRsf-C(O)N(Et)H) 0.22% 1.76% N-ETFOS Amide (CSF17SO2N(Et)H) 0.04% 0.13% C2F5SO2N(Et)CMCH20H C3F7SO2N(Et)CH2CH20H 0.01% 0.13% 0.12% 1.17% C4F9SO2N(Et)CH2CIbOH 0.11% 1.52% CsFl7SO2N(Et)2 0.03% 0.04% C5FiiSO2N(Et)CH2CH20H C6Fl3SO2N(Et)CH2CH20H 0.03% 0.51% 1.34% 3.52% C8Fl7SO2N(Et)CH2CH2CI 0.08% 0.16% C7Fl5SO2N(Et)CH2CH20H 0.82% 1.40% N-ETFOSE CsFl7SO2N(Et)CH2CH20H CBF15SO2N(Et)CH2CH20H 96.09% 0.78% 87.16% 0.50% C8Fl7SO2N(Et)(CH2CH20)2H 0.17% CsHl7SO2N(Et)H 0.16% 0.37% C8Fl7SO2N(Et)CH2CH2OCO2CH2CH3 (orsimilar) 0.21% 0.22% OtherHigh Boilers 0.28% 0.59% Component I.D. N-Methyl-carboxamides(Rf-C(O)N(Me)H) C2F5S02N(Nle)CH2CH20H -C8Fl7SO2N(Mf,)2 C3F7SO2N(Me)CH2CH20H C8Fl7SO2N(Me)H C4F9SO2N(Me)Cli2CH20H C5FiiSO2N(Me)CH2CH20H C6Fl3SO2N(Me)CH2CH20H C8Fl7SO2N(Me)CH2CH2CI C7Fl5SO2N(Me)CH2CH20H N-MEFOSE- CsFl7SO2N(Me)CH2CFhOH CgF19SO2N(Me)CH2CMOH CsFl7SO2N(Me)(CH2CH20)2H C8Hl7SO2N(Me)H Other High Boilers L-1276 N-MEFOSE Lot 1.46% 0.24% trace 1.15% trace 1.62% 1.34% 5.05% 0.13% 1.69% 83.88% 0.87% 0.34% 0.54% 1.55% Furtherwork has been done by GC on thesesamples which involvesderivatizatiofn thealcoholswith trifluoroacetainchydride(TFAA) and againwithBSA (togivethetrimethylsileytlhers).This work was designedtoinvestigattehe potentiaplroblems thatcould be overlookedby any one method of analysis. Preliminaryresultshow thatanalyzingtheETFOSE underivatizedcould hidea significanatmount of N-ETFOS Amide under the C-3 alcoholpeak inwide range material.However, analyzingthe same materialthathas been derivatizewdith TFAA shows thatany BtFOSE-chloride thatispresentinthe sample isnow completelymasked by the derivatizedC-8 alcohol.The BSA derivativehas not been evaluatedyet,but similarproblems are expected because of the number of differenctomponents inthesample. The same sortofproblems willmost likelyexistwith MEFOSE and willbe even more complicatedin theanalysisof MEFOSEA. 7/2/93 REQ 41343 1.Grant Cyr-MS analysesofthesesampleswere accomplishedusinga 25 m X 0.32mm HP- I GC column to introducethesamplesintotheFinniganSSQ-70 mass spectrometerT.he sample components were ionized usingchemicalionizatiownithmethaneasthereagentgas.The GC column was operatedfrom 40 to300 C ata rateoflodegreesperminute.The resultosftheseanalysecsombined withtheircorrespondinGgC/FID area percentshow thefollowing: Component I.D. N-Ethyl-carboxamid(ePsf-C(O)N(Et)H) C6Fl3SO2N(Et)H C2F5SO2N(Et)CH2CH20H C7Fl5SO2N(Et)H N-ETFOS Amide (C8Fl7SO2N(Et)H) C6Fl3SO2N(Et)2 C3F7SO2N(Et)CH2CH20H C4F9SO2N(Et)CH2CH20H C5FiiSO2N(Et)CH2CH20H C6Fl3SO2N(Et)CH2CH20H C7Fl5SO2N(Et)CH2CH20H N-ETFOSE C8Fl7SO2N(Et)CH2CH20H W.R. N-ETFOSE Precut 97900-112-1 68.34% 1.28% tram trace 0.41% 1.41% 1.53% 0.62% 1.48% 20.16% 3.52% 1.14% W.R. N-ETFOSE main cut 97900-112-2 1.27% 0.32% trace trace tmce trace 0.51% 0.42% 2.16% 60.86% 22.55% 11.92% Component I.D. N.R. N-MEFOSE B.P. 132 97900-107-2 mw 137 possibly -SO2N(Md)CE12CII20C7Fi5SO2N(Me)CH2CH20H .N-MEFOSE CaFl7SO2N(Nle)CH2CH20H CgFi9SO2N(Me)CH2CH20H -C8Fl7SO2N(Me)(CH2CH20)2H C8Hl7SO2N(Me)H OtherHigh Boilers Component I.D. N-Ethyl-carboxamide(sRf-C(O)N(Et)M C3F7SO2N(Et)H C4F9SO2N(Et)H C5Fi iSO2N(Et)H C6Fl3SO2N(Et)H C7Fl5SO2N(Et)H N-ETFOS Amide C8Fl7SO2N(Et)H) CgFi5SO2N(F,t)H numerous otherimpuritieosf most homologs thatincludehydrides,chlorineinthebackbone,and unidentifiehdighboilers 0.58% 0.41% 98.19% 0.59% trace trace 0.23 % W.R. N-ETFOS Amide 97900-111 10.23% trace 0.71% 3.58% 52.50% 20.06% 12.93% trace trace