A process for recovering residual uranium from emptied uranium hexafluoride shipping cylinder during cleaning, including rinsing a uranium hexafluoride shipping cylinder with hydrofluoric acid to dissolve a heel of uranium hexafluoride therein to form a mixture of sediment, precipitates and a uranium solution; separating the uranium solution from the sediment and precipitates; mixing sodium hydroxide with the uranium solution to precipitate sodium diuranate; separating the solid sodium diuranate from the sodium fluoride solution formed; re-dissolving the sodium diuranate in sodium carbonate solution to form uranyl carbonate complex solution; and adjusting the pH of uranyl carbonate complex solution further to precipitate uranyl peroxide with the addition of hydrogen peroxide. Sodium fluoride solution produced is further treated to remove fluoride by percolating it through a calcite limestone bed to form calcium fluoride solid.