Two sublimation techniques have been developed to separate Tc from Mo to support accelerator production of Mo-99/Tc-99m. After bombardment, the metal target is dissolved in nitric acid, the solution is evaporated, and the precipitated solids are calcined to MoO3. In the first technique, MoO3 is melted to a 0.8 mm layer and oxygen is swept over the 835 degrees C sample at 30 std cm(3)/min. Small amounts of MoO3 vapors transported from the 835 degrees C sample are deposited above 550 degrees C onto the walls of a quartz tube in a temperature gradient of 4 degrees C/cm. Greater than 95% of released technetium oxide is collected in a 5 mL condenser at temperatures between 300 and 25 degrees C. In the second process, technetium oxide deposited on the surface of fine needle crystals of MoO3 is quantitatively released in an oxygen stream at 650 degrees C. The crystals are regenerated between milkings by dissolving in NH4OH, evaporating, and drying. In this initial work, greater than 90% product recovery is achieved by both processes during multiple milkings of 14 g Mo samples and a high-purity Tc-99m product results at a concentration exceeding 500 mCi/mL in an isotonic saline solution.