新型纳米TiO2/SiO2表面离子印迹材料的制备及在固相萃取中的应用

With the nanometer TiO2/SiO2 composite material as carrier, the ions imprinted polymers for Pb, Cd, Hg, Cr, Zn, Ni, Mn, Tl and As were obtained by a surface imprinting technique. Their adsorption efficiency and mechanism toward metal ions were investigated by static and dynamic methods. Solid phase extraction column combined with AAS interface device was designed. The sparation/preconcentration method for Pb, Cd, Hg, Cr, Zn, Ni, Mn, Tl and As was required to determine heavy metals. The developed method was analysied to the determination of trace Pb, Cd, Hg, Cr, Zn, Ni, Mn, Tl and As for the Qinghai lake water samples, gymnocypris przewalskii, yak cheese, soil and forage of the Qilian mountains, as well as Qinghai Lake region and the Qingnani regions. To test the possibility of the new method, morphological analysis method for Cr(III) and Cr(VI) was developed to the determination of Cr(III) and Cr(VI) for the around area of Qinghai xinghuo Chrome salt factory soil, underground water and Huangshui River. The regional and seasonal characteristics of the heavy metal pollution were reflected. The scientific evidence was provided for the prevention and the control of the heavy metal pollution in biological and environmental samples in Qinghai.

本项目以纳米TiO2/SiO2复合材料为载体，分别以铅、镉、汞、铬、铜、锌、镍、锰、铊和砷离子为印迹离子，应用离子表面印迹技术，制备纳米TiO2/SiO2表面铅、镉、汞、铬、铜、锌、镍、锰、铊和砷离子印迹吸附剂。采用静态与动态两种方法，系统研究此材料对这些离子的吸附性能和机理。设计出这些离子的印迹聚合物作为固相萃取富集柱与AAS联用的接口装置。建立铅、镉、汞、三价铬、铜、锌、镍、锰、铊和砷离子痕量测定及Cr(III)和Cr(VI)的形态分析方法。用此方法研究不同季节青海湖水；青海湖内特有的青海裸鲤；青海湖区牦牛奶酪；祁连山系、环湖及青南地区的土壤和牧草中的痕量铅、镉、汞、铬、铜、锌、镍、锰、铊和砷离子及青海星火铬盐厂周围的土壤、地下水和湟水河中六价铬和三价铬的含量进行检测，验证建立新方法的可行性，反应这些重金属污染的季节动态和区域特征，为防治青海环境和生物样品中重金属的污染提供科学依据。

本项目采用溶胶凝胶法制备了纳米TiO2/SiO2复合材料，并用红外光谱、X-射线衍射、扫描电子显微镜、透射电子显微镜等手段表征纳米TiO2/SiO2的结构、形貌以及表面性质。以纳米TiO2/SiO2为载体，采用表面印迹技术，以铅、镉、汞、铬、铜、锌、镍、锰、铊和砷离子为模板离子，以3－氨基丙基－三乙氧基硅烷为功能单体，在纳米TiO2/SiO2表面聚合形成了铅、镉、汞、铬、铜、锌、镍、锰、铊和砷离子印迹聚合物。采用静态与动态两种方法，系统研究离子印迹聚合物材料对这些离子的吸附性能和机理，并设计出了这些离子的印迹聚合物作为固相萃取富集柱与AAS联用的接口装置。借助ICP-AES研究这些离子印迹聚合物对待测离子的定量富集酸度、吸附速率、吸附容量、洗脱条件、抗酸碱性、共存离子干扰、再生使用和选择吸附性能等理化指标，并研究其热力学与动力学性能；通过红外光谱、X-射线衍射等研究其结构及对待测元素的吸附机理，探讨其规律，为实际应用提供理论依据；建立铅、镉、汞、三价铬、铜、锌、镍、锰、铊和砷离子痕量测定及Cr(III)和Cr(VI)的形态分析方法。用此方法研究不同季节青海湖水；青海湖内特有的青海裸鲤；青海湖区牦牛奶酪；祁连山系、环湖及青南地区的土壤和牧草中的痕量铅、镉、汞、铬、铜、锌、镍、锰、铊和砷离子及青海星火铬盐厂周围的土壤、地下水和湟水河中六价铬和三价铬的含量进行检测，验证建立新方法的可行性，反应这些重金属污染的季节动态和区域特征，为防治青海环境和生物样品中重金属的污染提供科学依据。