The sorption characteristics of Cu(II) in an insolubilized humic acid (IHA) mediated column system were investigated at various experimental conditions using a solid phase extraction (SPE) technique. Sodium form of the IHA (INaA) was used as solid phase and sorption behaviors were evaluated by using common adsorption isotherms as well as Scatchard plot analysis. Regeneration, loading, washing and stripping steps of SPE were carried out consecutively, and their progresses were monitored through breakthrough curves obtained from a continuous flow-through cell adapted UV-vis spectrophotometer. So, the breakthrough curves were used to visualize distribution of Cu(II) concentration between mobile phase and solid phase, and amount of the Cu(II) sorbed by INaA was obtained from AAS analysis of effluents collected during the stripping steps of particular run. Thus, from the obtained results, the sorption characteristics and usability of IHA as a solid phase for SPE of metal ions was evaluated in detail. © 2007 Elsevier B.V. All rights reserved.