Abstract: It is established a procedure which includes MEK extraction Tc from NaOH solution,vaporating MEK with 1 mol/L HNO 3, then measuring 99 Tc with ICP MS. Using this procedure the 99 Tc of varied samples in the low level liquid waste treatment is first measured. In order to compare the γ radionuclides in samples are measured with unti Compton Ge(Li) γ spectrometry and 90 Sr 90 Y with Cerenkov counting.