Copolymer nanocomposites were prepared by the oxidative polymerization of Aniline, O-Toluidine/ M-Toluidine with PDS as an initiator and AS2O3 as nano material in aqueous medium under various experimental conditions such as different time, different concentration of monomers and different percentage weight of AS2O3. The properties of the nanocomposites were characterized with Fourier transform infrared (FTIR), conductivity measurements, thermo gravimetric analysis and HRTEM. Using FTIR spectroscopy the relative intensity of Benzenoid structure and Quinonoid structure were quantitatively calculated from which the order of structural formation was determined. TGA confirmed that the thermal stability is increased with the increase of percentage weight of AS2O3. HRTEM was used to confirm the nanosize of metal oxides and the intercalation of PNA chains into the basal spacing of metal oxides.