This paper evaluates the application of several biosorbents for Ni removal from aqueous solutions in the absence and in the presence of EDTA. Fixed bed experiments were performed (Ni influent concentration, 2mgdm(-3); EDTA doses, 0, 5, and 10mgdm(-3); pH=7) to study the process feasibility as refining after conventional physicochemical treatment. In absence of EDTA, uptake capacity followed the order peat > Posidonia oceanica > chitosan chitin >> Scharlau AC. Maximum uptakes of 8.95mgg(-1) and 5.10mgg(-1) were found for peat and Posidonia oceanica, respectively. In the presence of EDTA, removal capacity decreased for all biosorbents; Ni was detected in the effluent from the beginning of the operation, indicating low ability to retain Ni EDTA-complexes. Activated carbon presented the ability to remove complexed Ni. Peat exhibited the best performance for the treatment of an industrial spill from a metal-finishing facility, with effluent Ni concentration lower than 0.2mgdm(-3) for more than two weeks of treatment (3500 pore volumes of treated wastewater).