AbstractA process has been studied in which Zircaloy‐uranium alloy is dissolved in a mixture of hydrofluoric acid and potassium fluoride. The uranium can be precipitated with an efficiency of 99.9%, as a complex potassium uranium fluoride, together with some of the zirconium in analogous complexes. These precipitates, when dissolved in a mixture of aluminium nitrate and nitric acid, give stable solutions from which uranium may be recovered by solvent extraction with an overall efficiency of 99.7%.