Abstract: Technetium is separated from radio-contaminated metal in a three-step process. The contaminated metal is dissolved in an acid solution; the technetium, present in the resultant solution as pertechnetate ions, is quantitatively reduced to its metallic state through a metal displacement (cementation) reaction with a base metal of lower reduction potential; and the desired metal is electrolytically recovered from the solution, substantially free from technetium contamination.