Potentiometric determination of plutonium by argentic oxidation, ferrous reduction and dichromate titration

Abstract

A simple and rapid method is described for the routine determination of plutonium with a coefficient of variation of better than 0.2%. It is directly applicable to nitrate solutions containing a large amount of uranium; moderate amounts of iron, molybdenum, fluoride and phosphate do not interfere. Chromium, cerium and manganese interfere quantitatively, and the procedure may also prove convenient for the determination of these elements. The plutonium is oxidised to the sexivalent state with argentic oxide in nitric acid solution, and the excess of oxidant is destroyed by reaction with sulphamic acid. A weighed small excess of iron(II) solution is then added, and the excess is titrated potentiometrically with standard potassium dichromate solution using polarised gold indicator electrodes. The whole determination is performed in one vessel at room temperature, and takes about 20 min.