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A method for structure determination of cyclic sulphides within mixtures is described. It involves the use of a vapour phase hydrodesulphhtion micro-reactor (Raney nickel) located between the chromatographic column and the mass spectrometer (hydrogen and deuterium are used as carrier and reagent gases). A comparative examination of the mass spectra of the cydic sulphides, as well as of the hydrocarbons and their deuterio analogues (deuterium atoms are bonded to carbon atoms which had been attached to sulphnr) derived from the sulphides under the catalytic conditions employed, permits unambiguous determination of the size of the heterocycle and the position of the substituents.

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