The oxidation of methanol at smooth and porous, platinum and platinum/tin electrocatalysts in sulphuric acid solutions has been studied. The methods employed include linear sweep voltammetry and potentiometry at stationary and rotating electrodes. A microprocessor-based instrumental technique has been developed, which allows the simultaneous acquisition of steady-state polarisation data and a.c. impedance measurements. This system was based around a programmable potential controller used in conjunction with a frequency response analyser.