Abstract: The experimental apparatus for the separation of oxygen and argon was established based on the kinetic adsorption of carbon molecular sieves. The effects of PSA cycle, rinse-ratio and adsorption duration on the performance of adsorption processes were investigated. The experimental results show that to incorporate the rinse step can increase greatly the concentration of oxygen in desorbed gas. For producing high purity oxygen, the optimum values of the rinse-ratio and adsorption duration should be about 0.4 and 60 s respectively. Under this condition, the oxygen purity up to 99.4% is obtained for the 42% recovery with the feed gas mixture of 95% oxygen and 5% argon.