In order to study the adsorption mechanism of silver ions onto adsorbents prepared from grapefruit pee' functionalized with urea and melamine, carbon paste electrodes (CPE) were prepared and cyclic voltammetr studies were carried out. The electrochemical results showed that for the case of CPE containing the adsorber functionalized with urea, there is one oxidation signal at 0.0 V vs. MSE attributable to the oxidation of silver thi was adsorbed onto the amino groups present on its surface. On the other hand, in the CPE that contained th adsorbent functionalized with melamine, two oxidation signals were observed at 0.0 V and 0.1 V vs. MS attributable to silver adsorbed to the surface, but indicating the presence of two different energy adsorption site: The first of them associated with amino groups and the second with carboxyl groups. The results were con plemented with infrared spectroscopy techniques, X-ray photoemission spectroscopy, and dispersive energ spectroscopy and immersion microcalorimetry. From the results obtained it was possible to define the nu chanism of adsorption of the metal on each of the adsorbents studied. The electrochemical study has provide valuable information to elucidate the mechanism of adsorption, adequately complemented with conventions spectroscopic techniques has achieved a broad characterization of the amino-functionalized organic matrix, s that this analytical technique is shown as a new alternative to study superficial chemical changes in functic nalized materials.