A process was developed based on the thermal hydrolysis and precipitation of iron from solutions resulting from the leaching of zinc plant residue. A study was made of the hydrolysis of iron, at temperatures in the range 140-220C, in both pure solutions of ferrie sulphate and in leach solutions derived from plant spent electrolyte.At 200C hydrolysis of pure ferric sulphate solutions results in the precipitation of ferric oxide, Fe2O3, at low acid. concentrations, and a basic salt, Fe2O3.2S03.H20, at hIgher acid concentrations. At 180C ferric oxide is precipitated at low acid concentrations, but at higher acidities. carphosiderite, 3Fe203.4SO.3.9H20, is the stable phase. Frequently a mIxture of ferric oxide and carphosldente IS produced at 180C, the ratio of phases being dependent on the non-equilibrium experimental conditions.With solutions derived from plant spent electrolyte hydrolysIS at elevated temperatures results in the precipitation of jarosite compounds of the type NaFe3(S04)2(OH)6 The precipitation of natrojarosite jarosite, and ammonio-jarosite was studied in detail. Temperature, free acidity, and the concentration of sodium potassium, and ammonium ions are critical factors which affect the extent of precipitation.A process based on ammonio-jarosite precipitation was tested in a pilot plant.An alternative method of iron removal based on the addition of zinc oxide calcine, to neutralize excess acidity, and the precipitation of ferric oxide was also tested in the pilot plant. Both processes appear economically favourable...