In order to recover tritium from light water, research and development was carried out concerning a tritium separation process based on the principle of hydrogen-water isotopic exchange reaction. The performance and durability of unit operations for the process were studied. A pilot plant having a capacity of 1 m3/year (3.6 L/day) was designed and fabricated based on the results of the tests and studies. Using this plant, tritiated water could be concentrated to the order of a magnitude of 104. Furthermore, the effect of the various operating conditions on the tritium concentration factor was calculated by applying a data analysis program for the pilot plant. This study offered the prospect of a practical application of the process by the hydrogen vapor isotopic exchange reaction to recovery of tritium from light water.