Electrochemical treatment of distillery spent wash was carried out using different combinations of aluminum and iron electrodes in batch mode of operation. The spent wash was characterized for various parameters as per standard method of analysis and the treatment results were analyzed in terms of chemical oxygen demand (COD) removal efficiency of the spent wash. The experiments were performed to study the effect of operating parameters such as current density, pH of the spent wash, agitation speed, electrolysis time and the distance between the electrodes on the COD removal efficiency of the spent wash. It was observed that aluminum electrodes were more suitable for treatment of distillery spent wash as compared to iron electrodes. The maximum COD removal efficiency of 81.3% was obtained with Al-Al electrodes at the current density of 0.187 A.cm(-2) and pH 3 for an electrolysis time of 2 h.