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Novel conducting copolymers of N-methylaniline (NMAn) and o-aminophenol (o-APh) were synthesized electrochemically with different feed ratios of the monomers in sulfuric acid solution. The obtained homopolymers and copolymers were characterized with cyclic voltammetry, scanning electron microscopy (SEM), in situ conductivity measurements, in situ UV-Vis., and FT-IR spectroscopy techniques. The influence of applied copolymerization potentials and monomer feed ratio on the optical properties and conductivity of the copolymers were discussed. The in situ UV-Vis. spectroscopy results revealed strong absorption bands at different applied electrode potentials. The conductivity of copolymers increased with increasing the o-APh concentration in feed ratios. The fundamental differences between the structures and morphology of the homo- and copolymers were observed from FT-IR spectroscopy and SEM analysis.