Abstract:The cyanide residue from a smelter in Xinjiang was treated by the process of “Pellet-Desiccation-Chloridizing roast” for recovery of gold and silver. And the effect of the conditions of chloridizing roast on the metal volatilization rate was studied. The optimum conditions were obtained as follows: the addition of CaCl2: 7%(wt%), the roast temperature: 1100℃ and reaction time: 60min. Under the optimum conditions, the volatilization rates of Au and Ag were 98% and 62%, respectively. The volatilization rates of Cu, Pb and Zn were above 80%. The concentrations of Au and Ag in pellet after roasted decreased to 0.47g/t and 6.12g/t, respectively.