Abstract
Standard nitric acid solutions containing up to 400 g/L plutonium and/or uranium were prepared and these provide a way of rigorously testing methods for the determination of free acid in concentrated plutonium solutions. These standard solutions were prepared from uranyl nitrate hexahydrate and crystalline plutonium(IV) nitrate which was in turn obtained by vacuum evaporation of nitric acid solutions of Pu(IV). Three methods of free acid determination in plutonium solutions were tested, and the widely accepted iodate precipitation methods was shown to give markedly erroneous results at high plutonium concentrations. An improved oxalate complexing procedure was developed which gives accurate results (bias less than the standard deviation of 0.02 M) up to at least 400 g/L plutonium. 27 references, 2 figures, 2 tables.
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