Electrochemical and chemical oxidation methods are the two common methods used for the preparation of poly(pyrrole). The two methods have been acknowledged greatly and extensively studied because of their feasibility in manipulating the properties of poly(pyrrole) according to the desired application. However, chemical oxidation method is considered the best method for the preparation of poly(pyrrole) in larger quantities. There are other methods through which poly(pyrrole) can be synthesized such as plasma polymerization and photopolymerization, which have so far received less attention in the literature. For this paper, chemical oxidation was used to prepare poly(pyrrole) by oxidizing pyrrole with CuCl 2 under different emulsifying conditions. The surfactants used were sodium dodecyl sulfate and/or p-toluenesulfonic acid. Additionally, photopolymerization was also exploited to prepare poly(pyrrole) under similar emulsifying conditions. In this method, poly(pyrrole) was synthesized with the oxidizing ability of AgNO 3 under UV radiation. All samples were investigated by Fourier Transform-Infrared Spectroscopy (FT-IR), X-ray Photoelectron Spectroscopy (XPS), and Powder X-ray Diffraction (XRD). Scanning electron microscope was used to compare the morphological differences, which occurred due to different experimental conditions. The thermal stability was studied using thermogravimetric analysis (TGA).