Aniline/acrylonitrile nanocomposites were prepared in aqueous media by using a mixture of K2Cr2O7/K2S2O8 as an oxidant in the presence of various surfactants such as poly(vinyl alcohol), hydroxypropylcellulose, and surfactive dopant sodium dodecylbenzenesulfonate. The products were characterized in terms of conductivity, morphology, particle size and chemical structure. The results indicate that the type of surfactant influences the electrical conductivity, size and homogeneity of particles. The FTIR spectra show that the intensity of peaks is related to the type of surfactant.