Determination of the O/M ratios of polynary uranium oxides by Ce(IV)-Fe(II) back titration after dissolution in mixed sulphuric and phosphoric acids

Uranium (IV) in polynary uranium oxides is determined after the solid has been dissolved in a warm mixed solution of sulphuric and phosphoric acids containing excess Ce(IV). The latter is titrated with a Fe(II) standard solution using ferroin as indicator. This method is especially effective for (mixed) uranium oxides which are difficult to dissolve in hot Ce(IV) sulphuric acid. The standard deviation of the determined x value in polynary oxides is estimated to be below ± 0.004 for samples of 10–30 mg.