Electrocatalytic oxidation of methanol on a nickel disc electrode coated with nickel dimethyglyoxime complex (NiDMG), conditioned by potential recycling in a potential range of 100-700 mV (versus SCE) is studied by cyclic voltammetry in alkaline medium (0.10 M NaOH). The results show that the NiODMG layer formed at the surface of electrode behaves as an efficient electrocatalyst for the oxidation of methanol in alkaline medium via Ni(III) species with the cross exchange reaction occurring through out the layer at a low concentration of methanol. A plausible mechanism was proposed for catalytic oxidation of methanol at this modified electrode. Moreover, the effects of various parameters such as oven temperature, ligand concentration, potential scan rates, methanol concentration and media temperature on the electro-oxidation of methanol were investigated. (c) 2005 Elsevier B.V. All rights reserved.