A column solid phase extraction method for preconcentration of Fe(III), Cu(II), Mn(II) and Pb(II) on multi-walled carbon nanotubes (MWNTs) has been established. The adsorption was achieved quantitatively on carbon nanotube at pH 9.0, then the retained analyte contents on the column were quantitatively eluted with 1 M HNO3 in acetone. The effects of analytical parameters including pH of the solution, eluent type, sample volume, flow rates of eluent, matrix ions. etc. were investigated for optimization of the presented procedure. The preconcentration factor was calculated as 20. The detection limits for the understudy analyte ions were found in the range of 3.5 mu g/L (Mn)-8.0 mu g/L (Pb). The validation of the presented procedure was checked by the analysis of TMDA 54.4 fortified lake water and HR-1 River Sediment certified reference materials. The method was applied to the determination of analyte ions in environmental samples. (C) 2010 Elsevier Ltd. All rights reserved.