An improved pressure swing adsorption process is disclosed for the recovery of two individual components from a multicomponent gas mixture. The process utilizes a first group of adsorbent beds selective for the secondary component product and a second group of beds selective for tertiary impurities in the mixture. The gas mixture is passed through the first and second beds in series and high purity primary component product is discharged from the second beds. The secondary component product is recovered by desorption from the first beds. Product recovery is improved by recycling depressurization gas from the first beds and by several novel pressure equalization steps. The process can be used to recover high-purity hydrogen and carbon dioxide from a gas mixture containing these components along with minor amounts of methane, carbon monoxide, and nitrogen.