Precise Determination of Plutonium by Potentiometric Titration

Amperometric Titration of Plutonium(VI) with Iron(II).

“…More recently several new highprecision analytical methods for plutonium have been reported (11,IS,14) in which the interference of iron has been either eliminated completely or significantly reduced. Scoot and Peekema (11) and Shults (IS) used controlled potential coulometry to titrate plutonium(III) to (IV).…”

“…Waterbury and Metz (14) and Shults (IS) found fuming perchloric acid to be a satisfactory oxidant when the reaction was carried out under closely controlled conditions. The authors of the present work, however, were unable to obtain reproducible results with this reagent.…”

Volumetric Assay Method for Plutonium Using Spectrophotometric End Point Detection.

“…titrimetric (1,10,15), coulometric (8,18), and spectrophotometric (9) methods have been described but do not meet the need for a simple rapid assay procedure having the required precision.…”

“…Previous titrimetric procedures have, for the most part, used plutonium samples of 20 mg. or less (1,15). By increasing the sample size, an increase in precision could be expected.…”

“…By increasing the sample size, an increase in precision could be expected. Such an increase in sample size was one of the essential elements in the precise titrimetric plutonium procedures developed by Waterbury and Metz (15), and Pietri and Baglio (10). Although in theory it should be possible to obtain more satisfactory precison by modifying one of the microvolumetric procedures to use larger samples, the difficulties associated with the use of a potentiometric end point indicated that another approach was advisable.…”