In this research, we reported a novel method for synthesis of ZSM-5 zeolite. The synthesized zeolite was characterized using X-ray diffraction, scanning electronic microscopy and FT-IR techniques. The modified carbon paste electrode was prepared by incorporation of Ni (II)-zeolite in the carbon paste matrix. The electrochemical oxidation of methanol was investigated at the surface of this modified electrode in alkaline solution using cyclic voltammetry and chronoamperometry methods. It was found that methanol was oxidized by NiOOH generated with further electrochemical oxidation of nickel hydroxide on the surface of this modified electrode during the anodic potential sweep. The effect of some parameters such as scan rate of potential, concentration of methanol, amount of Ni (II)-zeolite was investigated on the oxidation of methanol at this electrode. Also, the rate constant for the catalytic reaction (k) of methanol was obtained. Copyright (C) 2010, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.