The electrolysis process is essential in the water detritiation subsystem using the combined electrolytic catalytic exchange process. A special experimental program was designed to characterize a modified HOGEN H Series industrial electrolyzer. The tritium amount transferred to hydrogen gas, the water enrichment factor, and the number of hours necessary to attain a steady-state regime were parameters of primary interest in the experiments. To minimize the necessary time for a steady-state regime, the holdup of the water electrolyzer was chosen as the minimum value allowed for safe and constant parameter operation in all experiments. The stationary regime was attained after 120 h, with an enrichment factor near 5, and an amount of 18% to 19% of tritium transferred from tritium-enriched water to hydrogen gas. These parameters were obtained in all three experiments, and the modeling software of isotope separation by electrolysis confirmed the results.