The electro-catalytic oxidation of methanol on a Ni - Cu alloy (NCA) with atomic ratio of 60/40 having previously undergone 50 potential sweep cycles in the range 0 - 600 mV vs. (Ag/AgCl) in 1 M NaOH was studied by cyclic voltammetry (CV), chronoamperometry (CA) and impedance spectroscopy ( EIS). The electro-oxidation was observed as large anodic peaks both in the anodic and early stages of the cathodic direction of potential sweep around 420 mV vs. (Ag/AgCl). The electro-catalytic surface was at least an order of magnitude superior to a pure nickel electrode for methanol oxidation. The diffusion coefficient and apparent rate constant of methanol oxidation were found to be 2.16 x 10(-4) cm(2) s(-1) and 1979.01 cm(3) mol(-1) s(-1), respectively. EIS studies were employed to unveil the charge transfer rate as well as the electrical characteristics of the catalytic surface. For the electrochemical oxidation of methanol at 5.0 M concentration, charge transfer resistance of nearly 111 Omega was obtained while the resistance of the electro-catalyst layer was ca. 329 Omega.