An extraction chromatographic material based on Aliquat-336 anchored on hydrophobized silica gel support was prepared as an ion exchanger. The prepared material appeared to be suitable for the separation of 99Tc from environmental matrices in column application. The properties of the material, sorption characteristic and distribution coefficient of 99mTcO4-in various media were studied. The prepared sorbent was conditioned by washing with nitric acid. The solution containing 99mTcO4- in 0.1M HNO3 was passed through the column. Tc was eluted from the column by 8M HNO3. The flow rate was 0.4 ml/min. The chemical yield of technetium during the separation process was determined using 99mTc tracer and gamma measurement. The sorption recovery of Tc from the prepared sorbent with 0.1M HNO3 solution was more than 98%, and the desorption recovery from the column using 8M HNO3 varied between 92-96%. It was found that the prepared sorbent is suitable for the separation of technetium from environmental matrices and radioactive wastes.