Tocopherols are the major components of deodorizer distillate, and one of the most important byproducts of soybean oil from the deodorization step of the soybean refining process. In the past, tocopherols were removed conventionally from the soybean deodorizer distillate using solvent extraction and molecular and vacuum distillation. Recently, supercritical carbon dioxide was tested as an alternative solvent for the separation processing of tocopherols. A separation process for a binary-component model mixture composed of a-tocopherol and squalene was developed using the pressure swing adsorption concept in supercritical. carbon dioxide. In the present study, the pressure swing operation between the adsorption step at a lower pressure, and the desorption step at a higher pressure was performed with octadecylsilica (ODS) as adsorbent. The objective of the current work was to experimentally measure the effect of operating parameters such as half-cycle time, pressure ratio, and flow-rate ratio on the product purity, yield, and recovery. Alpha-tocopherol was satisfactorily concentrated from 20 wt % of tocopherol in feed mixture to 60 wt % in product in the desorption step, and squalene was also concentrated from 80 wt % in feed mixture up to 98 wt % in product in the adsorption step. Optimal values for product purity, yield, and recovery were determined from these operating parameters. Model calculations were in rough agreement with experimental results.