New nano hybrid material (ZrO2/B2O3) was synthesized and applied as a sorbent for the separation and/or preconcentration of Co(II). Cu(II) and Cd(II) in water and tea leaves prior to their determination by flame atomic absorption spectrometry. Synthesized nano material was characterized by scanning electron microscope, transmission electron microscope and X-ray diffraction. The optimum conditions for the quantitative recovery of the analytes, including pH, eluent type and volume, flow rate of sample solution were examined. The effect of interfering ions was also investigated. Under the optimum conditions, adsorption isotherms and adsorption capacities have been examined. The recoveries of Co(II), Cu(II) and Cd(II) were 96 +/- 3%, 95 +/- 3%, 98 +/- 4% at 95% confidence level, respectively. The analytical detection limits for Co(II), Cu(II), and Cd(II) were 3.8, 3.3, and 3.1 mu g L-1, respectively. The reusability and adsorption capacities (32.2 mg g(-1) for Co, 46.5 mg g(-1) for Cu and 109.9 mgg(-1) for Cd) of the sorbent were found as satisfactory. The accuracy of the method was confirmed by analyzing certified reference material (GBW-07605 Tea leaves) and spiked real samples. The method was applied for the determination of analytes in tap water and tea leaves. (C) 2011 Elsevier B.V. All rights reserved.