Oxidative polymerization of aniline along with NiO nanoparticles using APS as oxidant and DBSA as dopant as well as surfactant at 0ºC yielded water soluble NiO-polyaniline composite. Spectral analysis like FTIR, XRD and SEM confirms the formation of the composite. Potentiality against corrosion is tested by gravimetric method, open circuit potential measurement, potentiodynamic polarization and electrochemical impedance spectroscopy. Effectiveness to give protection up to eight hours with slight changes in efficiency is observed in weight loss method. The results expose that the materials synthesized could give safe working environment in industrial maintenance work.