A method for treating process distillate heavies produced during uranium fluoride purification is described. The heavies contain primarily uranium hexafluoride, UF6, and molybdenum oxytetrafluoride, MoOF4. The uranium hexafluoride is removed via distillation at reduced pressure leaving essentially MoOF4 containing <0.1% of residual uranium hexafluoride. This mixture is hydrolyzed in water, then treated with a solution of sodium hydroxide until a pH of at least 7.5 is reached. The precipitated sodium diuranate and sodium fluoride are removed by filtration. The filtrate is reacted with calcium chloride to precipitate the molybdenum values as calcium molybdate containing trace quantities of calcium fluoride.