Electroactive copolymers of m-toluidine (MT) and o-phenylenediamine (OPD) were prepared electrochemically in aqueous sulfuric acid by potential cycling and characterized with cyclic voltametry, in situ conductivity measurements and FT-IR spectroscopy. The voltammograms of the copolymers exhibit different behavior for different concentrations of OPD in the comonomer feed. At optimum conditions the resulting poly(OPD-co-MT) shows an extended useful potential range of the redox activity as compared to the corresponding homopolymers. The effect of scan rate and pH on the electrochemical activity was studied. The copolymer was electrochemically active even at pH 8.0. The stability of the copolymer film was also tested. The copolymer has a potential region of maximum conductivity different from that of PMT and POPD. The conductivity of the copolymer is between the conductivity of the homopolymers. The vibrational bands at 3122/3450 and 2922/875cm−1 in the FT-IR spectra of the copolymer indicate the presence of both OPD and MT units, respectively, in the copolymer backbone.