Metallic zinc production from sulfide zinc ore is comprised by the stages of ore concentration, roasting, leaching, liquor purification, electrolysis and melting. During the leaching stage with sulfuric acid, other metals present in the ore in addition to zinc are also leached. The sulfuric liquor obtained in the leaching step is purified through impurities cementation. This step produces a residue with a high content of zinc, cadmium and copper, in addition to lead, cobalt and nickel. This paper describes the study of selective dissolution of zinc and cadmium present in the residue, followed by the segregation of those metals by cementation. The actual sulfuric solution, depleted from the electrolysis stage of metallic zinc production, was used as leaching agent. Once the leaching process variables were optimized, a liquor containing 141 g/L Zn, 53 g/L Cd, 0.002 g/L Cu, 0.01 g/L Co and 0.003 g/L Ni was obtained from a residue containing 30 wt.% Zn, 26 wt.% Cd, 7 wt.% Cu, 0.35 wt.% Co and 0.32 wt.% Ni. The residue mass reduction exceeded 80 wt.%. Cementation studies investigated the influence of temperature, reaction time, zinc concentration in feeding solution, pH of feeding solution and metallic zinc excess. After that such variables were optimized, more than 99.9% of cadmium present in liquor was recovered in the form of metallic cadmium with 97 wt.% purity. A filtrate (ZnSO4 Solution) containing 150 g/L Zn and 0.005 g/L Cd capable of feeding the electrolysis zinc stage was also obtained. (c) 2007 Elsevier Ltd. All rights reserved.