Copolymerization of o-anisidine and o-toluidine was achieved electrochemically in aqueous solution containing H 2 SO 4 as supporting electrolyte. The copolymer compositions can be altered by varying the monomer feed ratios during electrosynthesis. The films were electropolymerized in solution containing monomers in various ratio (0.025-0.1 M) and 1 M sulphuric acid as electrolyte by applying sequential linear potential scan rate 50 mV/s between -0.2 to 1.0 V. versus Ag/AgCl electrode. The copolymers were characterized by cyclic voltammetric, conductivity measurement, UV-Visible spectroscopy, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA).