Yankuang ceshi (Jan 2018)
The Preparation and Performance of SPE Packing of Bonded Ligand on the Surface of Nanometer Titanium Dioxide
Abstract
At present, the solid phase extraction packing of organic ligand/nano inorganic composite material is used to separate and enrich metal ions, which has become a hot research topic in analytical chemistry. A novel nano-TiO2/TSC solid-phase extraction packing was prepared by grafting thiosemicarbazone containing N, S coordination atoms onto the surface of nano-TiO2 by condensation reaction and is described in this paper. The structures and the property of synthesized composite were characterized and analyzed by Infrared Spectroscopy, X-ray Diffraction Scanning, X-ray Photoelectron Spectroscopy, and Electron Microscopy. The composition and size distribution of the packing particle were more uniform (the particle size is 200-300 nm) and more stable than the solid phase extraction packing made by physical blending technology. The saturation adsorption capacities of Sb3+, Cd2+ and Ba2+ on the solid phase extraction column prepared by this method at 30℃ were 13.9 mg/g, 12.9 mg/g, and 11.2 mg/g, respectively. The recoveries of three metal ions were 97.94%, 95.65% and 94.04%, respectively under the optimal experimental conditions. The data has good reproducibility with RSD < 5.5%. Thus, the adsorption property of the new nanometer TiO2/TSC composite solid phase extraction packing is an improvement on the styrene-methyl acrolein-thiosemicarbazide coated nano-titanium dioxide packing and nano-titanium dioxide packing. The contents of Sb3+, Cd2+ and Ba2+ in water samples were determined by Inductively Coupled Plasma-Mass Spectrometry coupled with the TiO2/TSC composite solid phase extraction packing, which yields detection limits of 0.061 μg/L, 0.013 μg/L, and 0.075 μg/L for Sb3+, Cd2+ and Ba2+, respectively.
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