The oxidation of sulfonhydrazides with benzeneseleninic acid provides an efficient and convenient preparation of selenosulfonates. Se-Phenylp-tolueneselenosulfonate was also produced in good to excellent yield from the reaction ofp-toluenesulfonhydrazide with PhSeCl, PhSeBr3, or PhSeCl3. Sulfonhydrazides react with sulfenyl halides or with PhSBr3to produce thiosulfonates in generally high yield. The treatment ofp-toluenesulfonhydrazide with benzenetellurinic acid, PhTeCl3, or PhTeBr3afforded only diphenyl ditelluride and not the corresponding tellurosulfonate.