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Thermo Gravimetric Analysis (TGA) analysis was employed to investigate activation energy (Ea) for the process of degrading of poly(o-toluidine) (POT) applying Horwitz & Metzger, Coats & Redfern and Chan et al., methods. POT was synthesized by chemical oxidative polymerization method using Ammonium per Sulphate (APS) as an oxidant while Dodecylbenzene Sulphonic Acid (DBSA) and sulfuric acid as co-dopants. Different samples, synthesized by variations in the reactions parameters, were evaluated in order to choose the one with the highest activation energy of degradation. Additional characterization of the polymer was carried out through different techniques such as Scanning Electron Microscopy (SEM), UltraViolet Visible spectroscopy (UV-Vis) and X-Ray Diffraction (XRD) analysis.