Determination of plutonium and uranium in mixed nuclear fuel by means of potentiostatic and amperostatic coulometry

Product solution occurs in HClO4 + HNO3 mixing. In prepared plutonium (6) and uranium (6) perchloric acid solution Cl and Cr (6), Mn (7,6,3) foreign oxidizers are selectively reduced with formic and malonic acids. Potentiostatic variant of method is based on successive reduction of Pu(6) to Pu(3) and U(6) to U(4) in 4.5M HCl, containing 5x10-4 M bismuth (3). In using amperostatic variant of method plutonium and uranium are determined separately. In sulfur-phosphoric acid media plutonium (6) is titrated to Pu(4) with continuously generated iron (2) ions. Uranium (6) in phosphoric acid media is initially reduced to U(4) with Fe(2), and then after Fe(2) excess reduction with nitric acid it is titrated to uranium (6) with continuously electrogenerated manganese (3) ions or vanadium (5). To obtain equivalent point in plutonium (6) and uranium (4) titration amperometric method is used. Coefficient of variation is 0.2-0.3 % rel