A method for the recovery of metal values from a metal value-bearing material containing arsenic and/or antimony and a source of sulphate ions such as sulphide ore or concentrate is disclosed. In one form the method comprises the steps of: (a) providing a feed stream comprising a metal value-bearing material containing arsenic and/or antimony and a source of sulphate ions; (b) subjecting the feed stream to oxidative conditions under elevated temperature and pressure conditions in the presence of at least one component selected to decrease the effective concentration of free acid generated during the pressure oxidation step and promote the formation of pH-stable iron (III) sulphate products, thereby forming a slurry comprising a metal value-containing leach solution and a solid leach residue containing pH-stable iron (III) sulphate products and environmentally stable iron-arsenic and/or iron-antimony products; (c) separating the metal value-containing leach solution from the solid leach residue; (d) recovering the metal value (s) from the metal value-containing leach solution; and (e) recovering precious metal values, if present, in the solid leach residue by cyanide leaching.