A method to recover copper and elemental sulfur from chalcopyrite concentrate, using a ferric chloride leach, cufes2 + 3fecl3 -> cucl + 4fecl2 + 2s, was reported by the federal Bureau of Mines in 1971 (report of investigations 7474). Additional work has been done to improve the recovery of sulfur from the leach residue, the recovery of copper and iron from the leach solution, and the regeneration of the leach solution. Over 99 pct of the elemental sulfur in the leach residue could be extracted at ambient temperature with an ammonium sulfide solution. Heating the pregnant solution precipitated crystals of rhombic sulfur (99.5 pct purity) and liberated ammonia and hydrogen sulfide for recycle. Copper with a purity in excess of 99 pct was obtained from the leach solution by electrolysis, using a diaphragm cell, with an energy requirement of less than 0.7 Kw-hr/lb. Metal was deposited as a weakly adherent powder that could be easily dislodged from the cathode and withdrawn continuously from the cell in the form of a slurry. During electrolysis, part of the fe(II) was oxidized to fe(III) at the anode so there was no chlorine evolution. The leach solution was regenerated by direct oxidation of the spent electrolyte with air or oxygen in a turboaerator at 80 deg c. This precipitated the iron dissolved during leaching in an easily filterable form, fe2o3.Xh2o, and converted the remaining fe(II) to fe(III).