A new method for measuring adsorption of organic molecules at the metal/solution interface as a function of potential is presented. The method is designed primarily for studying the adsorption of C14‐ or S35‐labeled organic compounds but can also be used for the adsorption of tagged inorganic species. The main feature of this method is that the large background usually present in this type of experiment has been eliminated. Any metal, which can be obtained in the form of a thin tape of sufficient tensile strength or which can be plated onto a base of sufficient tensile strength, can be investigated by this technique. Some results of the adsorption of thiourea on nickel are given.