[en] Uranium is separated from analytical Group II and Group III metal ions in an aqueous liquor containing uranyl ions. The liquor is extracted with a non-interfering, water-immiscible, organic solvent containing a reagent which will react with the uranyl ions to form a complex soluble in the solvent. If the liquor is acidic, the solvent is washed with water. Then to the solvent is added an aqueous solution containing about 0.5 to 1.0 mole per liter of (NH₄)₂CO₃ or NH₄HCO₃ ions and sufficient sulfide ions to precipitate the metal ions as sulfides. The solvent and the aqueous solution are separated and the sulfides filtered from the aqueous solution. The ammonium-uranyl-tricarbonate in the aqueous solution can then be precipitated by increasing the concentration of (NH₄)₂CO₃ or NH₄HCO₃ ions to about 1.5 to 2.5 moles per liter. The precipitate is filtered and calcined to obtain U₃O₈ or UO₂. 21 claims, 1 figure