In this work, the pitch-based activated carbon fibers (ACFs) were prepared by nitric acid to investigate the multi-metal adsorption in interfacial and textural points of view. N-2/77 K adsorption isotherm characteristics, including the specific surface area and micropore volume, were studied by BET specific surface area and t-plot methods, respectively. As a result, the specific surface area of the almost neutral ACFs in nature significantly decreased with nitric acid treatment, probably due to the widening of micropores. However the total acidity, including the carboxyl groups, on carbon surfaces was extremely induced during the acidic surface treatment. From the adsorptions of Cu2+ and Ni2+, it was revealed that the adsorption capacity of metal ions was mainly influenced by the weakly acidic functional groups such as lactones on the carbon surfaces at pH < pI (isoelectric point), and by the strongly acidic functional groups such as carboxyl groups at pH > pI. (C) 2004 Elsevier Inc. All rights reserved.