Abstract
An accurate and simple method was described for the determination of U (VI) in uranium dioxide. The method was based on the constant current coulometry using titanium sulfate electrolyte proposed by Kennedy and Lingane (Anal. Chim. Acta, 18, 240, 1958). The sample (0.10.5g) was dissolved readily in a mixture of 2N sulfuric acid and 12 drops of hydrofluoric acid, which was more preferable than the strong phosphoric acid. An aliquot of the solution was added to 3540ml of the electrolyte consisting of 78M sulfuric acid, 0.60.8M titanium sulfate, 10 mg of ferrous ion, 50100 mg of uranium (IV) ion and a few drops of hydrofluoric acid. Uranium (VI) was determined coulometrically using a sensitive amperometric end point procedure.
Satisfactory results were obtained for 131240 μg of uranium(VI) when the indicator circuit potential was chosen at 0.140.16 V vs. S. C. E. Results of stoichiometric analysis of uranium oxides (UO2 and U3O8) were also tabulated.
