A new powerful technique viz inductively coupled plasma-mass spectrometry (ICP-MS) has been utilized for the measurement of99Tc in the environmental samples. In this regard, when using anion exchange column for the separation of99Tc, significant quantities of Mo are also eluted from the resin along with the technetium. Various reagents (i.e., HCl, NaOH and HNO3) have been applied for the separation of Mo from the column prior to the Tc treatment. The result thus obtained are discussed.