岩矿测试

文章摘要

申书昌,冷茉含,彭程,吕伟超.二氧化钛表面键合配位体固相萃取填料的制备及其吸附性能研究[J].岩矿测试,2018,37(1):21-29

SHEN Shu-chang,LENG Mo-han,PENG Cheng,LÜ Wei-chao.The Preparation and Performance of SPE Packing of Bonded Ligand on the Surface of Nanometer Titanium Dioxide[J].Rock and Mineral Analysis,2018,37(1):21-29.DOI:10.15898/j.cnki.11-2131/td.201706080096

二氧化钛表面键合配位体固相萃取填料的制备及其吸附性能研究

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The Preparation and Performance of SPE Packing of Bonded Ligand on the Surface of Nanometer Titanium Dioxide

投稿时间：2017-06-08 修订日期：2017-11-07

DOI：10.15898/j.cnki.11-2131/td.201706080096

中文关键词: 纳米二氧化钛键合配位体固相萃取吸附性能重金属

英文关键词: nano-titanium dioxide bond ligand Solid Phase Extraction adsorption property heavy metals

基金项目:黑龙江省教育厅基本科研业务专项（135209221）

作者	单位
申书昌	齐齐哈尔大学分析测试中心, 黑龙江齐齐哈尔 161006
冷茉含	齐齐哈尔大学分析测试中心, 黑龙江齐齐哈尔 161006
彭程	齐齐哈尔大学分析测试中心, 黑龙江齐齐哈尔 161006
吕伟超	齐齐哈尔大学分析测试中心, 黑龙江齐齐哈尔 161006

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中文摘要:

有机配位体/无机纳米复合材料作为固相萃取填料用于重金属离子分离富集是当前分析化学研究的热点课题。本文将含有N、S配位原子的氨基硫脲通过缩合反应接枝于纳米二氧化钛表面，制备了一种新型纳米TiO₂/TSC复合固相萃取填料。通过红外光谱、X射线衍射、X射线光电子能谱和扫描电镜表征，此填料与共混法制备的聚合物包覆纳米二氧化钛复合填料相比，二氧化钛粒子（尺寸200~300 nm）分布更均匀，结构更稳定。用该填料制备的固相萃取小柱静态吸附Sb³⁺、Cd²⁺和Ba²⁺在30℃时饱和吸附量分别为13.9 mg/g、12.9 mg/g和11.2 mg/g，在优化的实验条件下三种金属离子的吸附回收率分别达到97.94%、95.65%和94.04%，实验数据重现性高（RSD<5.5%），吸附性能优于聚苯乙烯-甲基丙烯醛-氨基硫脲包覆纳米二氧化钛和纳米二氧化钛两种填料。本填料结合ICP-MS测定水样中以上三种离子的检出限分别为0.061 μg/L、0.013 μg/L和0.075 μg/L。

英文摘要:

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.

主管单位：	中国科学技术协会
主办单位：	中国地质学会岩矿测试技术专业委员会国家地质实验测试中心