A process is disclosed for producing a high purity tantalum precipitate from an impure source by dissolving in a first hydrofluoric acid solution and digested to form a first precipitate of tantalum which dissolved in hydrochloric acid. The resulting solution is heated to form a second precipitate of tantalum which is dissolved in another hydrofluoric acid solution and digested to form a third precipitate of tantalum. The third precipitate of tantalum is then dissolved in an oxalic acid solution with the pH being adjusted to form another tantalum precipitate which is converted to tantalum oxide.