Abstract: A multi-step process for recovering metal values from lead smelter matte. The matte is mixed with sulfuric acid and manganese oxide and leaching is effected at atmospheric pressure to form an aqueous solution including dissolved metal sulfates and a residue containing sulfur and lead sulfate. The sulfur is removable by conventional means and the lead sulfate may be returned to the smelter. The pH of the aqueous sulfate solution is adjusted to 3.5 to 4.5 to precipitate ferric iron and arsenic and pH is readjusted to about 3.0 to redissolve coprecipitated copper. After separation from the precipitate, the aqueous solution is mixed with a sulfiding agent, such as sodium sulfide at a pH of not more than 3 to selectively precipitate copper sulfide. After separating the copper sulfide, the aqueous solution is mixed with further sulfiding agent at a pH of 3 to 4.5 to form a cobalt-nickel sulfide precipitate in which the weight ratio of copper-nickel to sulfur is 1.8.