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A measured amount of acidic hydrometallurgical leach liquor is first treated with hydrogen peroxide to oxidize Fe(II) to Fe(III), then with potassium pyrophosphate solution to mask interference from Fe(III) and other metal ions. Ammonium acetate solution is then added as a pH modifier, before being titrated with standardized disodium dimethylglyoximate to an exothermic endpoint.

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