Methane irradiation procedure

In addition, another irradiated methane hydrate (sample F) sample was annealed at 253 K for 3 hours (sample F ) were measured by Raman spectroscopy. A scheme of experimental procedure is shown in Figure 1. 

The A -nitrososulfonamide 70 was shown to be a convenient reagent for radical trifluoromethylation. UV irradiation of lb with 70 in the presence of diacetyl as a sensitizer led to 38b in 51 % yield (Table 1, entry 8). Distinct advantage of this method is easy handling of the solid 70 instead of gaseous CF3I or of the quite unstable bis(perfluoro-aIkanoyl)peroxides. 70 is assessable from trifluoronitroso-methane 69 in a one-pot procedure [35]. Te(CF3)2 was also used as a trifluoromethyl radical source for trifluoromethylation. The reaction proceeded under UV irradiation and led to a 25 1 mixture of pyrroles lb and 2b (Table 1, entry 9) [36]. 

A novel gas-chromatographic procedure for the rapid separation of fission iodine (or bromine) from the other fission-produced elements has been reported (97). The method is based on the formation of methyl iodide when uranium is irradiated in an atmosphere of methane. A thin uniform layer of "Krylon"-lac-quered uranium dioxide (natural uranium or enriched uranium-235) was deposited on an aluminum sheet and the sheet was placed in a plastic irradiation vial which was then filled with methane, dosed, and placed in an irradiation rabbit. (The "Krylon lacquer slows down the recoil fragments before they enter the gas phase.) Following irradiation, the gaseous content of the vial was injected into a gas chromatograph. Recoil-produced CHjI, in chemical yield of about IX... 

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