The electrocatalytic oxidation of methanol on an aluminum electrode modified by Pt microparticles dispersed into nickel hexacyanoferrate (NiHCF) film in 0.1 M sulfuric acid solution as supporting electrolyte is described. It has been shown that the presence of NiHCF film improves considerably the catalytic efficiency of deposited Pt and Pt alloys microparticles toward the electrooxidation of methanol. The essential role of Pt-M alloys (M is Ru, Ir or Sn) on the enhancement of electrocatalytic activity of Pt particle toward the methanol oxidation was also demonstrated. The effect of some experimental factors such as NiHCF film thickness, Pt amount dispersed in the NiHCF film, concentration of Ru, Sn and Ir salts in the co-deposition solutions and medium temperature was studied and optimum conditions were suggested. Finally, the long term stability of modified electrodes has also is studied. (c) 2007 Elsevier B.V. All rights reserved.