A two phase electrolysis method has been developed for preparation of thiocyanating reagent. The electrolyses were carried out using graphite electrodes using a two phase electrolytic medium made up of an aqueous solution of ammonium thiocyanate in 0.25 M H2SO4 and a nonaqueous solvent. The effect of experimental parameters, such as temperature and duration of electrolysis, nature of the nonaqueous solvent and volume fraction of the nonaqueous phase, on the process current efficiency were studied. The voltammetric studies in the nonaqueous phase established that trithiocyanate, (SCN)(3)(-1), was produced in the aqueous phase and was subsequently extracted into the nonaqueous phase.