This study presents a chelating agent free solid phase extraction method for preconcentration of Al(III) using hybrid nano zirconium dioxide-boron oxide (ZrO2/B2O3) sorbent. This method is based on the sorption of Al(III) ions directly onto nano sorbent, followed by the elution with 10 mL of 4 mol L-1 HNO3 and determination by flame atomic absorption spectrometry (FAAS). Preconcentration parameters, including pH of the sample solution, volume and concentration of the eluent, sample volume, and flow rate of the sample solution, that affect the recovery of the Al(III) ions have been optimized. Under the optimized experimental conditions, analytical parameters such as limit of detection, limit of quantification, linear working range, precision, and accuracy were determined. The analytical limit of detection for Al(III) was found as 7.71 mu g L-1. The reusability and adsorption capacity of the new hybrid sorbent for Al(III) ions were also investigated. Interfering effects of matrix constituent on the recovery of the Al(III) ions were studied. The accuracy of the method was checked by determining Al(III) ions in a certified reference water sample (SPS-WW1 Waste Water). The proposed procedure was applied for the determination of Al(III) ions in dam waters.