Two heavy metals, Cd and Ni, have been separately recovered from spent AA-size Ni–Cd batteries by the potentiostatic electrodeposition and chemical precipitation methods, respectively. Various types and concentrations of HCl, H2SO4, and HNO3 acids had been used as leach extractants. Experimental results indicate that the acid with the best leach capability is 4M HCl. Three complexing reagents of NH3, sodium acetate, sodium citrate have been chosen and tested. The most effective buffer is sodium citrate. The optimum mole ratio of metallic ion to citrate ion is 1:1. The recovery process for Cd metal is conducted by the potentiostatic electrodeposition in a leach electrolyte with a sodium citrate complex. The optimum applied potential for Cd recovery is in the range −1100 to −1120mV (versus saturated calomel electrode (SCE)). The current efficiency for the recovery process is between 70 and 90% and depends strongly on the process parameters, e.g. liquor, concentration, applied potential, temperature, type of complex reagents, mole ratio, mass-transfer rate.