Synthesis of Chelating Agent Free-Solid Phase Extractor (CAF-SPE) Based on New SiO2/Al2O3/SnO2 Ternary Oxide and Application for Online Preconcentration of Pb2+ Coupled with FAAS

摘要

A new online solid phase preconcentration method using the new SiO2/Al2O3/SnO2 ternary oxide (designated as SiAlSn) as chelating agent free-solid phase extractor (CAF-SPE) coupled to flame atomic absorption spectrometry (FAAS) for Pb2+ determination at trace levels in different kind of samples is proposed. The solid adsorbent has been characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron miscroscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray fluorescence spectroscopy (XRF) and textural data. The method involves the preconcentration using time-based sampling of Pb2+ solution at pH 4.3 through 100.0 mg of packed adsorbed into a mini-column under flow rate of 4.0 mL min-1 during 5 min. The elution step was accomplished by using 1.0 mol L-1 HCl. A wide range of analytical curve (5.0-400.0 ?μg L-1), high enrichment factor (40.5), low consumption index (0.5 mL) and low limits of quantification and detection, 5.0 and 1.5 ?μg L-1, respectively, were obtained with the developed method. Practical application of method was tested on water samples, chocolate powder, Ginkgo biloba and sediment (certified reference material). On the basis of the results, the SiAlSn can be considered an effective adsorbent belonging to the class of CAF-SPE for Pb2+ determination from different matrices.