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Hydrogen/methane mixtures draw attention due to the idea of the injection of hydrogen into natural gas networks and biological production of biohythane by one- and two-step anaerobic fermentation/digestion methods. It is hard to extract hydrogen from dilute mixtures with methane by traditional separation processes, since hydrogen is the minor component with low partial pressure. Metal hydrides selectively absorb hydrogen and offer an opportunity to overcome the limitations of traditional separation methods. In the present paper, we present experimental results on the separation of a dilute mixture of hydrogen (10%) with methane in a flow-through metal hydride reactor with inlet mixture pressure of 0.95 MPa by the LaNi 4.8 Mn 0.3 Fe 0.1 intermetallic compound. Hydrogen was separated in one step with roundtrip (absorption/desorption) recovery of 74%. An exergetic analysis of the metal hydride separation of a binary mixture containing hydrogen was implemented and equations for hydrogen recovery and exergy efficiency of separation are obtained. Thermodynamic analysis shows that the exergy efficiency of the metal hydride purification has a clear maximum at hydrogen concentrations around 5–20%. The advantage of metal hydride purification is the absorption of the minor fraction from the feed, thus it is preferable for dilute mixtures and could be feasible for practical applications. With the use of low potential or waste heat to drive the reaction, it is possible to increase the efficiency of hydrogen purification by metal hydrides. The maximum exergy efficiency is 61% for 0.8 MPa outlet pressure, taking into account the quality of involved heat flows. • H 2 (10%)/CH 4 mixture was separated by LaNi 4.8 Mn 0.3 Fe 0.1 with 74% H 2 recovery. • Equations for the exergy efficiency of separation and the hydrogen recovery are obtained. • Exergy efficiency has maximum at H 2 concentration 5–20%. • Metal hydride purification has advantage for dilute H 2 mixtures. [ABSTRACT FROM AUTHOR]