Hydrogen peroxide reduces on the nickel electrode surface in the acidic medium. On the nickel electrode the passive film layers such as NiS and NiOOH form in the peroxide free solution. However the nickel surface was activated with the addition of the peroxide. The cyclic voltammetry (CV) and impedance (EIS) studies verified the passivation and activation states in peroxide free acidic solution and the acidic peroxide solution. The electrochemical reactions of the sulphuric acid and peroxide at nickel electrode were electrochemically analyzed by cyclic voltammetry (CV) and impedance spectroscopy (EIS)