Some aspects of the electrodeposition of copper and cobalt from aqueous sulphate solutions containing low concentrations of their ions were studied with a view to heavy metal removal via an electrochemical process. Both metals were deposited on a vitreous carbon rotating disc electrode. Deposits formed under different conditions were studied employing linear sweep voltammetry, scanning electron microscopy and EDAX surface analysis. Constant potential electrolysis was used to simulate recovery in a laboratory batch reactor. Copper can be deposited without cobalt interference at potentials as cathodic as -1.0 V despite high Co concentrations. At more negative potentials, both metals are deposited simultaneously, although the copper proportion in the binary mixture is greater than that corresponding to the solution concentration ratio. Voltammetry studies effected under conditions in which codeposition occurs show only minor changes in copper behaviour. On the other hand, cobalt behaviour exhibits significant modifications. Even though formation of an intermetallic compound is possible, ASVL and microscopy tests indicate cobalt deposition in different crystalline forms as the more probable cause. In turn, cobalt deposition depends on the polarization conditions of the electrode and on the cobalt and copper concentrations.