Volumetric determination of the U/O ratio in uranium oxides

A method is given for determining the general formula UO2+x, of sintered uranium dioxide pellets and uranium dioxide powders. Uranium(VI) is reduced by titration with iron(II) ammonium sulphate, after which the total amount of uranium is oxidized by titration with potassium dichromate. The end-points of both titrations are detected electrometrically. Determination of x in the range 0.0001–1.00 is possible.