The disintegration of 6 different Nb-Zr-Fe alloys and their hydrogen storage properties due to hydrogenation have been investigated. The hydrogenation was performed in a 0.1MPa hydrogen pressure held at room temperature in arc melting chamber without exposure to air atmosphere. The thermal stability of hydrogen dissolved in disintegrated powder was measured in the temperature range from room temperature to 600°C by using the thermal analysis equipment. Hydrogen contents in alloys were evaluated from the mass difference of TG curve and chemical determinations for hydrogen gas analysis. The values of hydrogen content are in accordance with both chemical and mass difference methods. The hydrogen contents of disintegrated alloys synthesized were in the range of 1.2-2.0 wt% which depend on the composition of alloys.