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An inverted emulsion process was adopted to synthesize conducting copolymers of aniline and acrylonitrile using benzoyl peroxide (BPO) as a novel oxidizing agent. The influence of polyacrylonitrile (PAN) ratio on the properties of conducting copolymers is reported. The chemical structures of the copolymers were characterized spectroscopically by UV-Vis, FT-IR, FT-Raman and EPR. The solubility of polyaniline (PAni) and PAni–PAN copolymers in dimethyl sulphoxide (DMSO) was confirmed by electronic absorption spectra. The conductivity of these copolymers lie in the range (1.26–4.20)×10⁻²S/cm. TGA thermogram of copolymers showed multi-step thermal degradation behaviour. X-ray scattering studies reflected that the copolymers are semicrystalline and showed two crystalline peaks at 17 and 25 (2θ).