The present invention is directed to adsorptive separation of nitrogen with active adsorbent phases with high N.sub.2 capacity and high heats of adsorption when diluted with inert material at levels ranging from 5% to 80%. The presence of diluent reduces the temperature swings in the adsorbent bed, which increases the utilizable effective N.sub.2 working capacity and decreases the relative amount of O.sub.2 left unrecovered on the active adsorbent phase. The net result is equal or better process performance allowing utilization of a lower amount of active adsorbent phase. Use of a diluent having a higher heat capacity than that of the active adsorbent phase increases these benefits, but dilution effects are beneficial even for diluents with heat capacities equal to or lower than that of the active adsorbent phase.