【作者】 张静；

【导师】 吴一微；

【作者基本信息】 湖北师范学院 ， 分析化学， 2011， 硕士

【摘要】 自固相萃取(SPE)创立以来,由于其具有有机溶剂耗量少、快速相分离、稳定性强、选择性好、富集倍数高、吸附容量大、可封闭操作(避免引入污染物)、制备方法简单、易于实现自动化、易与其它检测技术结合等优点,成为分离／富集中最重要的技术之一。本论文的研究目的是开发和研制新的磁固相萃取技术和新型固相萃取材料,建立磁固相萃取(MSPE)-火焰原子吸收光谱法(FAAS)联用测定铬元素形态的新方法。主要研究内容如下：(1)建立了以Fe3O4@SiO2-AEAPS作为萃取剂的MSPE-FAAS联用测定环境及生物样品中的痕量铬形态(Cr(Ⅲ)和Cr(Ⅵ)的新方法,系统地考察了影响MSPE的诸因素。在最佳条件下,富集倍数达到100倍,检测限为0.661μg/L。该方法被成功用于环境及生物样品中铬形态的测定。(2)建立了Fe3O4@ZrO2 MSPE-FAAS联用测定环境及生物样品中的铬形态(Cr(Ⅲ)和Cr(Ⅵ)的新方法,系统地考察了影响MSPE的诸因素。在最佳条件下,富集倍数达到25倍,检测限为0.69μg/L。该方法被应用于环境及生物样品中的铬形态的测定,取得了满意结果。(3)建立了Fe3O4@APDC MSPE-FAAS联用测定环境及生物样品中的铬形态(Cr(Ⅲ)和Cr(Ⅵ))的新方法,系统地考察了影响MSPE的诸因素。在最佳条件下,富集倍数达到8.3倍,检测限为3.1μg/L。该方法被成功用于环境及生物样品中的铬形态的测定,说明了此方法的可行性和可靠性。更多还原

【Abstract】 Solid phase extraction (SPE) has become one of the most important techniques used for separation and preconcentration due to its advantages of low organic solvents consumption, rapid phase separation, strong stability, good selectivity, high enrichment factor, high adsorption capacity, closed operation without introducting pollutants, simple preparation method, easy automation, good ability of combination with different determination techniques etc.. The aim of this dissertation is to develop new solid phase extraction materials and new magnetic solid phase extraction technology, to establish new technology of combination flame atomic absorption spectrophotometer (FAAS) with magnetic solid phase extraction (MSPE) and new method of chromium species analysis. The main contents are as follows:(1) A method has been developed for the determination of trace chromium species (Cr(III) and Cr(VI)) in environmental and biological samples by MSPE combined with FAAS using Fe3O4@SiO2-AEAPS as extractant. Various parameters affecting MSPE were optimized systematically. Under the optimized conditions, an enrichment factor 100 and the determination limit 0.66μg/L were found. The proposed method has been successfully applied to the determination of trace chromium species in environmental and biological samples.(2) A method has been developed for the determination of trace chromium species (Cr(Ⅲ) and Cr(Ⅳ)) in environmental and biological samples by MSPE combined with FAAS using Fe3O4@ZrO2 as extractant. Various parameters affecting MSPE were optimized systematically. Under the optimized conditions, an enrichment factor 25 and the determination limit 0.69μg/L were found. The proposed method has been applied to the determination of trace chromium species in environmental and biological samples, and a well result was received.(3) A method has been developed for the determination of trace chromium species (Cr(Ⅲ) and Cr(Ⅵ)) in environmental and biological samples by MSPE combined with FAAS using Fe3O4@APDC as extractant. Various parameters affecting MSPE were optimized systematically. Under the optimized conditions, an enrichment factor 8.3 and the determination limit 3.13μg/L were found. The proposed method has been successfully applied to the determination of trace chromium species in environmental and biological samples, demonstrating the feasibility and reliability of the proposed method.更多还原