The corrosion behavior of pure Ni and 65Ni-24Cr-10Mo alloy in HCl and H2SO4 solutions were investigated using weight-loss and electrochemical methods. The effects of temperature and acidic media were studied to define the main differences in the corrosion behavior of these materials. The results of both techniques revealed lower values of corrosion rates for the 65Ni-24Cr-10Mo alloy compared to pure Ni. Generally, the corrosion rates for both materials increase with increasing temperature in both acids with higher rates in HCl compared to H2SO4 at all conditions. Results of weight-loss and potentiodynamic tests were in a good agreement and indicated that the alloy 65Ni-24Cr-10Mo is a high resistance to corrosion in HCl and H2SO4 acidic solutions than pure Ni. The activation energies (𝐸𝑎) of the dissolution process of Ni and alloy have calculated. The activation energy of Ni in HCl is 18 kJ/mole and in H2SO4 is 20 kJ/mole where for the alloy in HCl is 18 kJ/mole and in H2SO4 is 32 kJ/mole.