The concentration breakthrough curves were examined to predict mass transfer conefficients of nitrogen and oxygen in adsorption column for design data of PSA process. Experimental breakthrough curves for bulk gas flow were compared with theoretical simulation results. For quantitative analysis of the adsorption, coupled Langmuir isotherm was considered and LDF model was used to describe the mass transfer effect. In the experimental and theoretical results, it was found that mass transfer coefficient was not affected by flow rate but strongly affected by pressure. As a result of this tendency, mass transfer resistance in this system was proved to belong to the macropore diffusion controlling region and the mass transfer coefficients could be expressed by exponential functions of pressure change. The mass transfer coefficients for one component, nitrogen or oxygen, were successfully applied to breakthrough curves for bulk mixed gases. The experimental curves were reasonably in consistent with the theoretical curves and the error time was less than 5 percent.