This paper demonstrates the methodology of the investigations on electrochemical behavior of hydrogen-absorbing materials using a Pd-limited volume electrode (LVE) as an example and model system. An experiment for physical chemistry students is described, in which they prepare Pd-LVE by electrodeposition of a thin metal layer on Au matrix and then examine the influence of electrode potential on the amount of hydrogen electrochemically absorbed in Pd from 0.5 M H 2SO 4 solution. The potential ranges corresponding to alpha- and beta-phase existence as well as the alpha-beta phase transition can be easily distinguished. Hysteresis between hydrogen absorption and desorption is illustrated. The comparison between electrochemical behavior of Pd-LVE and bulk Pd electrode is also made, demonstrating the unique advantages of the use of LVE in the electrochemical studies on hydrogen-absorbing materials. Chronoamperometry and cyclic voltammetry are used as experimental techniques together with the application of Faraday law of electrolysis coupled with classical gravimetry. The experiment allows the students to learn on some important topics of solid state chemistry and electrochemistry, i.e. hydrogen absorption in metals, non-stoichiometric compounds, metal deposition, phase transition, thin layer electrodes.