Tritium resulting from separation processes is being stored in metal hydrides. In time, because of radioactive decay, tritium converts into 3He, which accumulates in the storage vessel. The recovery of 3He is a topic of high interest because of its wide range of applications in health care, security, and advanced research. Currently, at ICSI Râmnicu Vâlcea, a method is under development based on gas chromatography, Pd/Ag membrane permeation, and cryogenic distillation for 3He separation and enrichment having as sources both the cover gas of nuclear reactors and tritium storage containers. This paper reports the investigation of using Pd/Ag membranes for helium separation from hydrogen isotopes by experimental determination of the operating performance of the membrane in view of process integration. Tests have been performed at different temperatures in the domain of 100°C to 350°C for different hydrogen partial pressures in the upstream side of the membrane in the domain of 150 to 300 kPa, while the downstream part was continuously purged with a preliminary vacuum pump. The results for the membrane parameters are in good agreement with previous literature reports and will be utilized for the dimensioning and establishing of operating parameters of the membrane used for intermediate separation of helium isotopes from hydrogen.