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A new method for the preparation of Tc metal from pertechnetate is described. Metallic technetium was prepared from TcO by initial reduction in dry argon atmosphere at 300 °C followed by a wet argon atmosphere in the presence of carbon between 700 and 910 °C. The higher temperature conditions in the presence of H2O and carbon form H2 and CO, which can drive the reduction of TcO2. This method was applied to the recovery of pertechnetate sorbed on anion-exchange resins resulting in the formation of Tc metal microspheres. The resulting Tc was characterized by XRD analysis and SEM. [ABSTRACT FROM AUTHOR]