Abstract: The performances of 4A molecular sieves column, 5A molecular sieves column, carbon black pellets column, and activated carbon column in separation of xeron and the concurrent gaseous impurities were investigated at different temperature. Based on the measurement results, a preparative chromatographic procedure for separation and purification of Xe from air samples was established, and the technical parameters were ascertained. The procedure was tested with simulated trace Xe-containing samples. The results show that the purity of thus isolated Xe is higher than 98%, and its overall recovery is better than 90%, indicating samples prepared by this procedure can meet the requirement of the radioactive Xe measurement.