Polyaniline/Polystyrene nanocomposite was prepared in aqueous media by polymerization styrene and aniline by using ammonium peroxy disulfate ((NH4)2S2O8) and potassium iodate (KIO3) as oxidants in the presence of hydroxypropylcellulose (HPC) as surfectant. The composite was characterized in terms of morphology, particle size, chemical structure. The results indicate that the morphology, particle size, chemical structure of products are dependent on the surfactant. The chemical structure, morphology of product were studied by fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM).