A method has been developed for the separation and purification of {sup 99}Tc in nuclear power plant radioactive waste samples. The classical iron hydroxide and carbonate precipitations are followed by solid phase extraction. The pure {sup 99}Tc is quantified using liquid scintillation spectrometry. Technetium-99m is used as an internal radiotracer to determine the radiochemical recovery for the process. The quality of analytical results obtained was within the 15% precision and accuracy criteria established for this technique at the Yankee Atomic Environmental Laboratory (YAEL).