A new solid phase extractor, nano-scale diboron trioxide/titanium dioxide composite material, was synthesized and used for separation and/or preconcentration of trace cadmium ion from various samples. The characterization of the synthesized material was performed by scanning electron microscope (SEM), transmission electron microscope (TEM) and X-ray diffractometer methods (XRD). The specific surface area of the material was also determined and found as 3.4ml/g. Analytical parameters including pH of sample solution, sample volume, flow rate of sample solution, volume and concentration of eluent for the column solid phase extraction (SPE) procedure were examined. The effect of common matrix ions on the recovery of the cadmium has also been investigated and found that they did not interfere on cadmium preconcentration. Under the optimum experimental conditions, preconcentration factor and analytical detection limit were determined as 50 and 1.44 mu g/L, respectively. The reusability (stabile up to 100 run) and adsorption capacity (49 mg/g) of the sorbent were excellent. The accuracy of the method was confirmed by analyzing certified reference materials (Tea leaves GBW-07605). The results demonstrated good agreement with the certified values (relative error <10%). The precision of the method was also satisfactory. The recovery of cadmium under the optimum conditions was found to be 96 +/- 3% at 95% confidence level. The method was applied for the determination of cadmium in tap water and tea leaves. (C) 2008 Elsevier B.V. All rights reserved.