A sensitive and simple separation-enrichment technique for the determination of trace amounts of some metal ions was described. By the passage of aqueous samples including Fe(III), Cu(II), Ni(II) and Co(II) ions-4-(2-thiazolylazo) resorcinol (TAR) chelates through Diaion SP-850 column, metal chelates adsorb quantitatively and almost all matrix elements were passed through the column to drain. Quantitative recoveries for analyte ions were obtained at pH 6 at 3 ml/min flow rate of sample solution in 0.5 g Diaion SP-850 filled glass column. The investigations were also carried out on the interferences from other concomitant ions in the sorption process. After optimization, a preconcentration factor of 60 and a recovery values as % higher than 95 were achieved. The detection limit (N = 10, 3 sigma) for Fe(III), Cu(II), Ni(II) and Co(II) were found as 3.6, 1.1, 2.8 and 2.3 mu g l(-1), respectively. The applications to the determination of iron, copper, nickel and cobalt in real samples and the validation of the analytical methodology employing NIST SRM 1549 milk powder, NIST RM 8433 Corn Bran and BCR 144R Sewage sludge of domestic origin as certified reference materials were performed. (C) 2010 Elsevier B.V. All rights reserved.