The sorption characteristics of insolubilized humic acid (IHA) were investigated for Ni (II) in a column arrangement. The sodium form of the IHA (INaA) was used as a solid phase. Column operations were performed with five steps and all of them were monitored continuously by a flowthrough cell-adapted UV-Vis spectrophotometer. Thus, all solid-phase extraction (SPE) steps were visualized by breakthrough curves and analyses progress were evaluated. However, all calculations and evaluations were focused on the atomic absorption spectrophotometric (AAS) analyses of the solutions collected during the stripping steps. There was a high correlation (r2, 0.972) between peak area and AAS data of stripping steps. The effect of concentration and pH of the loading solution onto sorption of Ni (II) by INaA was investigated. Sorption characteristics were evaluated by using Freundlich, Langmuir, and Dubinin-Radushkevich (D-R) adsorption isotherms, as well as by Scatchard plot analysis. Multilayer sorption was found to be agreeable for Ni (II). From the D-R isotherm the mean free energy of sorption (E) was calculated (6.65 kJ mol-1) and attributed to the multilayer sorption. Finally, the sorption characteristic of the INaA-Ni (II) system was compared with that of the INaA-Cu (II) system, and possible separation of two ions in a binary mixture system is discussed. © 2005 Elsevier Inc. All rights reserved.