Carbon dioxide separation and recovery from air-CO2 mixtures were carried out by means of a pressure swing adsorption process consisting of both rectifying and stripping sections. Zeolite MS 13X was used as the adsorbent and parametric studies such as effects of feed inlet position, reflux ratio, gas flow rates, and pressure ratio on the enriched product concentration or recovery as well as lean product concentration were experimentally investigated. The concept of optimal feed inlet position and reflux ratio was discussed from a viewpoint of concentration distributions along each adsorbent bed. It is also found that a reduction of the gas flow rates, which allows longer residence time inside the column, improves sensibly the separation performance.