Reaction gas chromatography/mass spectrometry. Part IX: Post-column hydrodesulfurization in capillary GC/MS as an aid in structure elucidation of cyclic sulfides within mixtures

This article describes a method that assists in structure determination of cyclic sulfides mixtures by GC/MS. The method involves the use of a gas-phase hydrodesulfurization microreactor (AP-56 catalyst, reaction temperture 300-315°C, hydrogen as a carrier and reagent gas) located between the capillary column (OV-17) and the mass spectrometer. The presence of a microreactor in such a position does not essentially affect the chromatographic separation achieved by using the capillary column. Combined analysis of the mass spectra registered for the original sulfides and the hydrodesulfurization products permits the structure determination of each effluent to be made more reliably. This is illustrated by the investigation of a reaction mixture containing the structural and geometric isomers of methyl-substituted thiabicyclononanes.