Sulphide semiconductor materials have attracted much attention due to their excellent photoelectrochemical and high photocatalytic activities. Sulphides of transition metals are semiconductor materials with band gaps in the range of 1–2 eV which these find application in optoelectronics and as quantum dots. The research work is devoted to the electrochemical reduction of thiosulphate ions from ethylene glycol. By recording cyclic and linear polarization curves on Pt and Ni substrates, the kinetics and mechanism of the process and the influence of various factors on the electroreduction of thiosulphate ions have been studied. Polarization curves show that the electroreduction process proceeds in one-stage within a potential interval of (0.5–(–1.0)) V. According to the obtained data, the effective activation energy was calculated. The calculation results show that the electroreduction process of thiosulphate ions in ethylene glycol is accompanied by concentration polarization.