Copolymerization of o-anisidine and o-toluidine was achieved electrochemically in aqueous solution containing H2SO4 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). (c) 2005 Springer Science + Business Media, Inc.