This study reports a simple method for the synthesis of alpha-sulfur-nanoparticles-loaded alumina as a reliable kind of sorbents in solid-phase extraction (SPE) methods for the preconcentration and determination of trace levels of Ni(II) from real samples. The most important advantage of this technique is not using the ligand as a complexing agent and hence the disadvantages of other SPE methods have been avoided. The calibration graph was linear over the range of 0.66-100 mu g/L and the relative standard deviation (RSD) of 1.98% at 50 mu g/L was obtained. The limit of detection (LOD) and preconcentration factor (PF) were obtained as 0.22 mu g/L and 250, respectively. The maximum adsorption capacity of the adsorbent was found to be 18 mg/g for Ni(II).