The Thermal Cycling Absorption Process (TCAP), is a semicontinuous gas chromatographic process for hydrogen isotope separation by which the experiment for hydrogen-deuterium separation has been carried out. The main operating parameters for optimum separation were obtained. On manual operation conditions the concentrations of product and raffmate gas were batter than 99.5% simultaneously at a feed rate of 12.0% for a 1:1 hydrogen-deuterium mixture. Besides, TCAP is a good process for trace heavier isotope enriching from hydrogen. The concentration of deuterium can be reduced from 0.5% to less than 50ppm in hydrogen in ten cycles.