The adsorption behaviors of Cu 2+ and Pb 2+ species at electrochemically activated glassy carbon obtained by different activation methods have been studied. Micropore structures were developed by cyclic polarization while small void space located at the bottom of the large void space was resulted from potentiostatic activation. The adsorption of the adsorbents would depend on the relative sizes of both the adsorbents and the void space created by electrochemical pretreatment. Different quinone derivatives would adsorb to different adsorption sites at the activated electrode, and consequently, affected the uptake of metal ions at the activated electrode incorporated with different quinone derivatives. Electrostatic and hydrophobic interactions between the adsorbents and the graphite oxide film might be involved.