Polypyrrole and its nanocomposites were obtained by chemical polymerization by using anhydrous ferric chloride as an oxidant in the presence of dodecylbenzensulfonate and poly(vinyl alchohol) as surfactants and iron (III) oxide nanoparticles in aqueous media. The products were characterized, such as morphology, chemical structure, and crystalline nature, by using analysis by scanning electron microscope, Fouriertransform infrared spectrometry, and X-ray diffraction. The results indicated that sodium dodecylbenzenesulfonate, poly(vinyl alcohol), and Fe 2 O 3 nanoparticles influenced the properties of products. Scanning electron microscope analysis results indicated that when additives were added to the pyrrole matrix, the size of the product decreased and homogeneity increased. Fourier-transform infrared spectrometry confirmed that nanocomposites formed in the presence of surfactant. X-ray diffraction pattern analysis confirmed the presence of Fe 2 O 3 nanoparticles in the nanocomposite matrix. J. VINYL ADDIT. TECHNOL., 22:362-367, 2016. V C 2014 Society of Plastics Engineers EXPERIMENTAL InstrumentationA magnetic mixer, OHAUS, Model PA214, digital scale, IKA, Model RO 10P, scanning electron microscope (SEM), Model KYKY-EM3200, X-ray diffraction (XRD),