The synthesis of polyaniline (PAni) powder was carried out from 0.15M of aniline and 1M of HCl in distilled water at room temperature in a single compartment electrochemical cell. The PAni was again synthesized chemically keeping the composition and temperature same as electrochemical process but adding equimolar amount of ammonium peroxydisulfate as an oxidizing agent. Then the PAni obtained from these two methods were characterized by the conductivity, solubility, X-ray, FTIR, TGA, UV, and SEM, and compared. Result shows that the electrochemically synthesized PAni (ECS-PAni) has somewhat lower conductivity, higher solubility, more benzenoid rings than quinoid rings, lower crystallinity, higher band energy, and higher particle size than that of chemically synthesized PAni (CS-PAni). © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 1900–1904, 2007
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