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ABSTRACT
A SiO2/Al2O3/Sb2O5 mixed oxide was synthesized via a sol-gel method and applied to the on-line preconcentration of Ni(II) with determination by flame atomic absorption spectrometry. The mixed oxide was characterized by infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray fluorescence, thermogravimetric analysis, and the specific surface area. Analysis was performed by percolating 20.0 mL of sample at pH 7.1 through 100 mg of SiO2/Al2O3/Sb2O5 packed into a mini-column at 9.5 mL min−1. Under the optimum conditions, a preconcentration factor of 77.5-fold, linear dynamic range from 5.0 to 270.0 µg L−1, and limits of detection and quantification of 0.48 and 1.61 µg L−1 were obtained. The effects of several concomitant ions were evaluated and no interferences were observed. The method was employed for the analysis of water with good recoveries (92.9–100.6%) and the accuracy was verified by using a marine sediment certified reference material (MESS-3).