The separation of argon and oxygen from their gaseous mixture is very difficult to accomplish by the adsorption process using zeolite adsorbents due to the closeness of their molecular properties and adsorption behavior in the zeolites. Strontium exchanged zeolite X (SrX) showed the adsorption selectivity for oxygen over argon at ambient temperature and demonstrated its potential as a column-packing material for the gas chromatographic analysis of argon-oxygen mixtures. The adsorption capacities and Henry's law constants for oxygen and argon increased in SrX compared to NaX at ambient temperature. Activation of the SrX adsorbent is shown to play a highly significant role in the separation of argon-oxygen mixture due to the low hydrothermal stability of SrX.