Abstract: Hydrometallurgical process is a well established technology to separate and recover of nickel ions, from Ni-Cd spent batteries and deposit Nickel powder with high purity and low energy requirements. This study preform to explain the effect of H2SO4 concentration (1, 1.5, 2) N on the deposited weight and percentage purity of Ni when the electrodeposition parameters such as 24 hr time deposition, 4 cm distance between electrodes, 1.5 applied potential, 8 cm2 area of cathode are constant. The results shown that the weight deposited decrease when the solution concentration increase is found to be 150 mg in 2 N concentration and the percentage purity of Ni deposited increase when the solution concentration increase is found to be 93% in same concentration. Ni-Cd spent batteries are used to deposit Ni.