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To obtain an environmentally clean energy source, many experimental methods have been de‐ veloped and used to study the adsorption of hydrogen for the cathodic H2 evolution reaction (HER) and hydroxide for the anodic O2 evolution reaction (OER) at noble and highly corrosionresistant metal and alloy/aqueous solution interfaces [1−7]. The cathodic HER is one of the most extensively studied topics in electrochemistry, electrode kinetics, renewable and sustainable energy, etc. It is well known that underpotentially deposited hydrogen (UPD H) and overpo‐ tentially deposited hydrogen (OPD H) occupy different surface adsorption sites and act as two distinguishable electroadsorbed H species, and that only OPD H can contribute to the cathodic HER [2−7]. Similarly, one can interpret that underpotentially deposited deuterium (UPD D) and overpotentially deposited deuterium (OPD D) occupy different surface adsorption sites and act as two distinguishable electroadsorbed D species, and that only OPD D can contribute to the cathodic D2 evolution reaction (DER). However, there is not much reliable electrode ki‐ netic data for OPD H and OPD D, i.e. the fractional surface coverage, interaction parameter, and equilibrium constant for the Frumkin adsorption isotherm, at the interfaces. Also, a quantita‐ tive relationship between the Temkin and Frumkin or Langmuir adsorption isotherms has not been developed to study the cathodic HER and DER. Thus, there is a technological need for a useful, effective, and reliable method to determine the Frumkin, Langmuir, and Temkin ad‐ sorption isotherms of OPD H and OPD D and related electrode kinetic and thermodynamic pa‐ rameters. In the following discussions, H and D mean OPD H and OPD D, respectively.

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Developments in Electrochemistry: The Phase-Shift Method and Correlation Constants for Determining the Electrochemical Adsorption Isotherms at Noble and Highly Corrosion-Resistant Metal/Solution Interfaces