The Electromagnetic Isotope" Separations Program of the Oak Ridge National Laboratory has been involved in the separation, chemical recovery, and refinement of the stable isotopes of cadmium and zinc since 1946. Traditionally, the chemical refinement procedures for these elements consisted of ion exchange separations using anion exchange resins followed by pH-controlled hydrogen sulfide precipitations. The procedures were quite time-consuming and made it difficult to remove trace quantities of sulfur which interferes in subsequent attempts to prepare rolled metal foils. As demands for 113 Cd and 68 Zn (a precursor for the production of the radiopharmaceutical 67 Ga) increased, it became evident that a quicker, more efficient refinement procedure was needed. Details of an improved method, which employs concurrent hydrogen reduction and distillation in the recovery and refinement of isotopically enriched zinc, are described. Modifications of the procedure suitable for the refinement of cadmium isotopes are also described.