Conductive polyaniline salts were synthesized by inverted emulsion polymerization method and were characterized by thermogravimetric analysis (TGA), thermogravimetry-mass (TGA-MS) analysis, and X-ray photoelectron spectroscopy (XPS) methods. The various characteristic fragments evolved during the thermal degradation of polyaniline were identified. The weight loss of dopants as well as sodium lauryl sulfate decomposition were identified at different temperatures from TGA-MS analysis. The kinetic analysis of the thermal decomposition processes of polyaniline in doped state was performed. Broiclo, Chang, and Friedman methods were used for the evaluation of kinetic parameters in nitrogen atmosphere. High resolution XPS analysis was used to provide a method of differentiating the presence of nitrogen and carbon associated in the different environments in the polyaniline base and doped-samples. (c) 2006 Wiley Periodicals, Inc.