A new realization of periodic cycled gas/liquid separation is presented. Separation factors and column efficiencies are compared for a column stripping ammonia from water with air, using three different sets of internals: conventional sieve trays, Sulzer BX gauze packings, and periodically cycled trays. The proposed new periodic trays are shown to be advantageous compared to their continuous alternatives. It is demonstrated experimentally that periodic tray efficiencies of up to 300% are achievable. With the proposed new tray design, a new operation form is also introduced in which the trays are drained sequentially rather than simultaneously, such that the vapor flow is not interrupted during the liquid drainage. For different ratios of counter-current vapor/liquid flow rates, column efficiencies for periodically cycled columns are shown experimentally to be two times greater than those for columns with sieve trays.