Abstract
The determination of uranium and plutonium in mixed oxide fuels has been developed by sequential potentiometric titration. A weighed sample of uranium and plutonium oxides is dissolved in a mixture of nitric and hydrofluoric acids and the solution is fumed with sulfuric acid. After the reduction of uranium and plutonium to uranium(IV) and plutonium(III) by chromium(II) sulfate, 5 ml of buffer solution (KClHCl, pH 1.0) is added to the solution. Then the solution is diluted to 30 ml with water and the pH of the solution is adjusted to 1.01.5 with 1 M sodium hydroxide. The solution is stirred until the oxidation of the excess of chromium(II) by air is completed. After the removal of dissolved oxygen by bubbling nitrogen through the solution for 10 minutes, uranium (IV) is titrated with 0.1 N cerium(IV) sulfate. Then, plutonium is titrated by 0.02 N cerium(IV) sulfate. When a mixture of uranium and plutonium is titrated with 0.1 N potassium dichromate potentiometrically, the potential change at the end point of plutonium is very small and the end point of uranium is also unclear when 0.1 N potassium permanganate is used as a titrant. In the present method, nitrate, fluoride and copper(II) interfere with the determination of plutonium and uranium. Iron interferes quantitatively with the determination of plutonium but not of uranium. Results obtained in applying the proposed method to 50 mg of mixtures of plutonium and uranium {(7.550)}% Pu were accurate to within 0.15 mg of each element.
