Cathode material from spent Ni-Cd cells was dissolved in aq. H(2)SO(4) and oxidized with H(2)O(2) to remove Fe completely as Fe(OH)(3) ppt. after neutralization with NaOH or NH(3) solns. (pH 4.5-5). The Fe-free soln. was electrolyzed at 0.3-1 A to sep. Cd and Co as brittle coatings on the steel cathode. The final concns. of remaining Cd and Co in soln. after electrolysis (20 mA/cm(2)) were 24 and 350 mg/L, resp. After addnl. 3-step extn. of the solutions with Cyanex 272 in Exxol(R)D80, the concs. decreased down to 3.5 and 0.3 mg/L, resp.