Hydrogen storage materials are increasingly being used as reversible batteries and it is necessary to understand and characterize the role of hydrogen in the reversible two-phase region. LaNi₅ (rare earth transition metal) has been studied in this investigation because it has been well characterized as a potential material for rechargeable metal-hydride batteries and hydrogen storage devices. Hydrogen storage capabilities of LaNi₅ intermetallic compounds have been characterized through the combination of thermoelectric power, Beeghly Ester-Halogen digestion, and Leco hydrogen determination. Thermoelectric power has been demonstrated as a rapid hydrogen assessment technique and can achieve the equivalent of the pressure-composition-temperature (activity) diagram. A thorough assessment of the content of each phase and the two-phase region has been performed to optimize performance of the hydrogen storage materials. The combination of these three analytical practices for rapid characterization of LaNi₅ intermetallic alloys will also be discussed.