A simple and inexpensive method of separation of 99m Tc from 99 Mo produced by neutron activation of 98 Mo via the 98 Mo(n,γ) 99 Mo nuclear reaction is described. The recovery of 99m Tc was performed by solvent extraction technique followed by column (active alumina) chromatography. The overall radiochemical yield for the complete separation of 99m Tc was 85–95% (n=10). The separated Na[ 99m Tc]TcO 4 was of high radionuclidic, radiochemical, and chemical purities. The method can be adopted for routine use of 99m Tc in hospital radio-pharmacies utilizing low-medium specific activity (n,γ) 99 Mo produced in a research reactor.