Determination of plutonium and neptunium in various materials by coulometric titration with amperometric indicating

Coulometric methods of determining Pu and Np in the products of complex composition containing, in addition to Pu and Np, Cr and Nn have been developed. The methods are based on titration of Pusup((6)) and Npsup((6)) to tetravalent state in H2SO4-H3PO4 with iron (2) ions generated continuously. A new variant of amperometric method has been proposed for determining end-point of titration. The methods of preparing Pusup((6)) and Npsup((6)) solutions have been developed. It has been shown that, upon dissolution of PuO2 and NpO2 by boiling with a mixture of nitric and perchloric acids Pusup((4)) and Npsup((4)) are oxidized quantitatively to Pusup((6)) and Npsup((6)) while Cl2, Crsup((6)) and Mnsup((7,4,3)) in the solution obtained are selectively reduced by CHOOH and CH2(COOH)2. In 6-8 M in terms of H2SO4 solution, ammonium bichromate oxidizes Npsup((4)) to Npsup((6)), Pusup((3)) to Pusup((4)), and Mnsup((2)) to Mnsup((3)). Oxidized Mn and excess of Crsup((6)) are selectively reduced by CHOOH and H2C2O4 in 4M in terms of H2SO4 solution