A new chelating resin, Xylenol Orange coated Amberlite XAD-7, was prepared and used for preconcentration of Cd(II), Co(II), Cu(II), Fe(III), Ni(II) and Zn(II) prior to their determination by flame atomic absorption spectrophotometry. The optimum pH values for quantitative sorption of Cd(II), Co(II), Cu(II), Fe(III), Ni(II) and Zn(II) are 4.5-5.0, 4.5, 4.0-5.0, 4.0, 5.0 and 5.0-7.0, respectively, and their desorptions by 2 mol L(-1) HCl are instantaneous. The sorption capacity of the resin has been found to be 2.0, 2.6, 1.6, 1.6, 2.6 and 1.8 mg g(-1) of resin for Cd, Co, Cu, Fe, Ni and Zn, respectively. The tolerance limits of electrolytes, NaCl, NaF, NaI, NaNO3, Na2SO4 and of cations, Mg2+ and Ca2+ in the sorption of the six metal ions are reported. The preconcentration factor was between 50 and 200. The t1/2 values for sorption are found to be 5.3, 2.9, 3.2, 3.3, 2.5 and 2.6 min for the six metals, respectively. The recoveries are between 96.0 and 100.0% for the different metals at preconcentration limits between 10 to 40 ng mL(-1). The preconcentration method has been applied to determine the six metal ions in river water samples after destroying the organic matter (if present in very large amount) with concentrated nitric acid (RSD < or = 8%, except for Cd for which it is upto 12.6%) and cobalt content of vitamin tablets with RSD of approximately 3.0%.