A measured amount of acidic hydrometallurgical leach liquor is pH modified with a small amount of glacial acetic acid, and the Fe(III) content reduced to Fe(II) with iodide ion. The liberated iodine is titrated with standard thiosulfate solution to an exothermic endpoint. Thus, 1 mol Fe³⁺= 1 mol S₂O₃^2-.

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