The U.S. Bureau of Mines developed an alkaline oxidative pretreatment leaching procedure to increase the recovery of gold from arsenopyrite (feass) ores. The best solution compositions for arsenopyrite dissolution were determined using cyclic voltammetry and chronocoulometry. Initial arsenopyrite dissolution occurred at - 0.20 V versus standard hydrogen electrode (she) in a sodium hydroxide (naoh) solution. Leaching of a high-grade arsenopyritic ore containing, in percent, 28.2 As, 25.3 Fe, 19.9 Total s, and 1.0 Sb and, in troy ounces per short ton, 1.6 Au and 5.5 Ag resulted in > 90 pct as extraction at 100 deg c, 40 psig o2, 4 h, and 2 m naoh solution in a 2-l autoclave. Cyanidation of the leach residues resulted in 90 to 93 pct au and 60 to 80 pct ag extractions, compared with only 5 and 15 pct, respectively, without the pretreatment. The procedure was further tested by leaching a low- grade gold ore and a bulk sulfide flotation concentrate prepared from it. Cyanidation of the leach residues resulted in 70 pct au and 31 pct ag extraction. The naoh leachate was partially regenerated by precipitating the arsenate as calcium arsenate [ca3(aso4)2] and the sulfate as barium sulfate (baso4).