The dry distillation method was studied for rapid separation of 99mTc from neutron irradiated MoO3. Upon heating, 99mTc produced in MoO3 crystal by the 98Mo(n,r)Mo99m β→ 99mTc process was found to be released by diffusion. From observations made of the deposition temperature, it was concluded that 99mTc was present in the form of 99mTc(IV) in the MoO3 crystal lattice and that it was released in the form of 99mTcO2, which, in air, further oxidized to 99mTc2O7. The release of 99mTc from neutron irradiated MoO3 powder was studied in the temperature range of 480°700°C, and its behavior was found to be in good agreement with the bulk diffusion mechanism based on Fick's law. The diffusion coefficient varied with temperature in compliance with Arrhenius' relation, except in the region of temperatures above 700°C. The separation of 99mTc from MoO3 was performed with a yield higher than 80% upon heating for 30 min at 800°C in air. The decontamination factor for 99Mo was consistently found higher than 105.
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