A method for separation-preconcentration of Pb(II), Cr(III), Cu(II), Ni(Il) and Cd(II) ions by membrane filtration has been described. The method based on the collection of analyte metal ions on a cellulose nitrate membrane filter and determination of analytes by flame atomic absorption spectrometry (FAAS). The method was optimized for several parameters including of pH, matrix effects and sample volume. The recoveries of analytes were generally in the range of 93-100%. The detection limits by 3 sigma for analyte ions were 0.02 mu L-1 for Pb(II), 0.3 mu g L-1 for Cr(III), 3.1 mu gL(-1) for Cu(II), 7.8 mu g L-1 for Ni(II) and 0.9 mu gL(-1) for Cd(II). The proposed method was applied to the determination of lead, chromium, copper, nickel and cadmium in tap waters and RM 8704 Buffalo River Sediment standard reference material with satisfactory results. The relative standard deviations of the determinations were below 10%. (c) 2006 Elsevier B.V. All rights reserved.