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