Pd limited volume electrodes (LVE) were obtained electrochemically from the PdCl 2 aqueous solution. Hydrogen absorption was performed using cyclic voltammetry and chronoamperometry in concentrated (6 M) alkaline solutions (KOH, NaOH, the mixture of 2M LiOH + 4M KOH) and results were compared with 0.5 M H 2 SO 4 . It was found that hydrogen pretreatment procedure is crucial for further examination of hydrogen absorption in Pd electrodes. After many cycles of hydrogen absorption/desorption in Pd, these processes become electrochemically more reversible-faster than in a freshly prepared electrode. Results obtained for Pd electrodes in different concentrated alkaline media subjected to hydrogen pretreatment procedure are comparable with those for an acidic solution (e.g., α→β phase transition potential equals to ca. 0.050 V vs. RHE). The continuous Pd electrode cycling does not affect significantly the amount of absorbed hydrogen (ca. 0.72-0.74). The surface roughness factor in basic solutions decreases after multiple hydrogen sorption as in case of an acidic solution.
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