Gold, silver and palladium may be separated from the other base metals and sulphur contained in copper sulphide precipitates derived from the Sherritt-Gordon nickel process using a process involving an oxidation roast, a reduction roast and a Cu(II)/acetonitrile leach. Sulphur is removed as SO, in an oxidation roast and the hot calcine is reduced with carbon, or with carbon plus cuprous chloride. The resulting product contains metallic copper which is readily dissolved with cupric ions in aqueous acetonitrile solution. Copper powder is recovered by thermal disproportionation. The residue contains the bulk of the iron and precious metals and may be treated by a number of methods, including direct cyanidation or melting with suitable fluxes. Melting the residue will produce a copper alloy containing the precious metals and remove the iron as a slag. The alloy can be recycled to the copper leaching stage or sent for toll refining depending on the precious metal content. Impurities from the leaching circuit are controlled by a bleed circuit which in one approach utilizes the SO, from the calciner to produce Chevreul's salt and separates copper from the soluble cobalt and nickel. Alternatively, the bleed may be directed back to the main refinery copper boil stage or oxydrolysis stage.