Mass spectra of seventeen bis(alkylmercapto) alkanes of the general formula R.S.C<sub>n</sub>H<sub>2n</sub>S R are presented and discussed Major ions occur by· 1) simple C-C or C-S cleavage to give ions of the type R S C<sub>m</sub>H<sub>2m+1</sub><sup>+</sup>; 2) cleavage of a C-S bond accompanied by hydrogen rearrangement; and 3) further loss of an alkyl group. The consecutive nature of breakdown in cases of double cleavage and rearrangement is established by metastable transitions.

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