Abstract: Radioxenon isotopes in atmosphere are the important monitoring component of Comprehensive Nuclear-Test-Ban Treaty. In order to improve the radioactive detection sensitivity of xenon samples, it is necessary to purify the sample, remove radon and transfer it to container before measurement. The key technologies in process of efficient purification and preparation of xenon samples were researched. The adsorption and desorption behaviors of xenon on three stage adsorption columns were studied. The effects of xenon sample volume and chromatographic parameters on the peak width were investigated, and the purification and preparation process parameters were determined. The recovery of pure xenon for purification and preparation process is more than 90% by tested with xenon samples, and the radon decontaminate coefficient is more than 10⁴. The efficient purification and preparation of radioxenon samples is realized.