A lead-zinc-pyrite flotation middling was pressure oxidised to give residues containing iron hydroxy sulphates (a mixture of basic iron sulphate (BIS) and a hydrated iron sulphate (HIS)) and lead sulphate. Direct thiourea leaching of this residue gave over 90 per cent extraction of gold and silver, but thiourea consumption was high (56 kg/t) because of soluble iron(M) in the residue. Attempts were made to decrease the thiourea consumption by removing the water-soluble iron(M) or reducing it to iron(II). Water washing of the pressure oxidation residue removed most of the hydrated iron sulphate but little of the basic iron sulphate. Iron removal was only 12-20 per cent, depending on the number of washes, from one sample which was low in HIS, and 40-45 per cent in another which was high in HIS. Iron extraction was not appreciably increased by using dilute sulphuric acid (with or without additions of sodium sulphite), dilute phosphoric acid, or sodium chloride solution (150 g/L NaCI). Direct thiourea leaching of the water-washed residue gave over 90 per cent extraction of gold but only 49 per cent of silver, with a thiourea consumption of 27 kg/t. However, the application of a water wash followed by reduction of dissolved iron(III) with sodium sulphite in the presence of thiourea, and then thiourea leaching resulted in over 98 per cent extraction of gold and silver for a thiourea consumption of 26 kg/t.