Abstract: A super largecapacity hydrogen isotopes separation system, including total plan, unit (including making and purification of gas, three-grade chromatographic columns, gas loop and auto-controll, and carrier recovery) and experimental scheme, had been designed on the basis of a series of hydrogen-deuterium experiments by temperature programmed desorption. The characteristic of the system was that desorption kinetic parameters could be directly calculated from the hydrogen isotope separation desorption spectra information. In other words, the complicated dynamic process of separation could be described by the desorption rate equation, shape parameter and desorption activation energy calculation on the condition of the experimental data and appropriate assumptions (equilibrium and adsorption, uniform surface). In previous work, an experimental series of operation to verify the successive enrichment of D₂ from a H₂-D₂ mixture, the production of the deuterium from natural hydrogen and the recovery of tritium such as from the nuclear heavy-water were carried out using MS5A at 77 K. This work was only conceptual design, so it was necessary to identify the availability of super large capacity system by experiment.