A solid phase extraction procedure for flame atomic absorption spectrometric determination of Cu(II), Pb(II), Fe(III), Co(II), and Cr(III) is proposed on Chelex-100 resin. The sample solutions at pH 6 were pumped through a micro-column at the rate of 2.0 mL/min by using a peristaltic pump. The elution of the retained analytes on the column was performed with 5 mL of 1 M HNO3 at 2.0 mL/min flow rate. The recoveries of analyte ions were greater than 95%. The relative standard deviations at the 50 mug/L levels of analyte ions were generally lower than 3% (N = 10). Recoveries of spike addition to bottled mineral water and artificial seawater were quantitative (>95%). The proposed preconcentration/separation method has been applied to determinations of the analyte contents of microwave and wet digested black tea and natural water samples. The validation of the developed preconcentration/ separation procedure was carried out by successfully analyzing standard stream sediment (GBW7310) reference material.