A measured amount of acidic hydrometallurgical leach liquor is treated first with a complexing agent (sodium gluconate). It is then basified to ~pH 10.5 with a NH3 /NH4Cl buffer, prior to the addition of KCN solution to mask Fe(III). Caution! Do not add KCN to solutions of pH below 9! The Fe(III) is then reduced to Fe(II) by additon of ascorbic acid, prior to titrating the Mg content with standard Na4EDTA solution.