The electrocatalytic oxidation of methanol studied at the surface of nickel disc electrode coatedwith N,N-bis(salicylidene)phenylenediamine (Salophen) legend in 0.10 M NaOH solution using cyclic voltammetry. The results showed that the Ni-salophen layer formed at the surface of electrode behaves as an efficient electrocatalyst for the oxidation of methanol in alkaline medium. The thermal analysis of Ni-salophen complex studied at temperature ranges 0–800°C in argon atmosphere. Also, FTIR was employed to prove the formation of complex on the modified electrode surface. Moreover, the effects of various parameters such as oven temperature, methanol concentration, NaOH concentration and media temperature on electro-oxidation of methanol were investigated. The kinetic parameters such as activation energy and Tafel slope were calculated for methanol oxidation on the modified electrode surface.
