The modification of gold electrodes with 4-carboxyphenyl diazonium salts to form stable layers for sensing applications is reported. Electrochemical reduction of 4-carboxyphenyl diazonium salts on gold electrodes yielded more stable layers than alkanethiol self-assembled monolayers in terms of extremes of electrode potential, sonication and with time. The application of the 4-carboxyphenyl modified electrodes for electrochemical sensing, which typically requires short chain alkanethiols on gold electrodes, is demonstrated via the covalent attachment of oligopeptides for the selective detection of Cu2+, Cd2+ and Pb2+. The diazonium salt/peptide modified gold electrodes not only had greater stability but also performed with lowest detected concentration to alkanethiol/peptide modified electrodes and with far greater sensitivity than the metal ion sensors when diazonium salt/peptide modified similar glassy carbon electrodes were employed. (c) 2006 Elsevier B.V. All rights reserved.