Electrocatalysts of type PtSnNiTi/C were prepared by thermal decomposition of polymeric precursors. The physico-chemical and electrochemical characterization of the electrocatalysts was performed by different techniques: X-ray diffraction, transmission electron microscopy, cyclic voltammetry and chronoamperometry. The XRD results showed that the electrocatalysts comprise mainly Pt metal with face-centered cubic crystal structure. The electrocatalysts were evaluated in the absence and presence of ethanol and glycerol in sulfuric acid medium. All showed activity toward alcohols oxidation. Furthermore, the Pt50Sn20Ni25Ti5/C electrocatalyst showed the best results of cyclic voltammetry and chronoamperometry in presence of glycerol and ethanol, respectively. Cyclic voltammetry data obtained in this study indicate that the addition of Ni and Ti in PtSn electrocatalysts increases its electrocatalytic activity toward alcohols oxidation. For alcohol (ethanol and glycerol) electrooxidation, high performance liquid chromatography (HPLC) was carried out after electrolysis, for determination of the products generated from alcohol consumption. The main product found after electrolysis was acetaldehyde. (C) 2013 The Electrochemical Society. All rights reserved.