基于磁性金属有机骨架材料的固相萃取电感耦合等离子体质谱法测定环境水中的重金属元素  

Determination of heavy metals in environmental water by magnetic solid phase extraction inductively coupled plasma mass spectrometry based on magnetic metal-organic framework materials

作　　者：王意[1] 邹昊彤 薛涛[1] 刘洋[1] 林奎[1] 李方[2] 邓小娟[1] WANG Yi;ZOU Haotong;XUE Tao;LIU Yang;LIN Kui;LI Fang;DENG Xiaojuan(Analysis and Testing Center,Tianjin University,Tianjin 300072,China;College of Materials Science and Engineering,Tianjin University,Tianjin 300072,China)

机构地区：[1]天津大学分析测试中心,天津300072 [2]天津大学材料学院,天津300072

出　　处：《分析试验室》2024年第4期476-481,共6页Chinese Journal of Analysis Laboratory

基　　金：天津大学实验室建设项目(LAB2021-10);国家自然科学基金(21506147)资助。

摘　　要：利用水热反应,成功合成了一种功能化的金属有机骨架材料,磁性MIL-101(Fe),并将其用作磁性固相萃取(MSPE)吸附剂,与电感耦合等离子体质谱(ICP-MS)联用,实现高效、灵敏的痕量重金属离子测定。利用扫描电子显微镜、透射电子显微镜、 X射线衍射和X射线光电子能谱对磁性MIL-101(Fe)进行了表征,并通过间歇吸附实验优化了溶液pH、吸附时间和解吸时间等萃取参数。结果表明,所合成的MIL-101(Fe)磁性固相萃取剂具有良好的晶体结构和表面功能化纳米颗粒。在优化实验条件下,所建立的MSPE-ICP-MS方法线性范围为0.5~500μg/L, As(Ⅲ), Pb(Ⅱ)和Cu(Ⅱ)的检出限为0.177~0.301μg/L,相对标准偏差为1.7%~3.2%,在连续7次循环使用后回收率仍可达82%。该方法用于环境水样中痕量重金属离子的测定,加标回收率为90.0%~113.2%,可用于环境水样中痕量重金属检测。A functionalized metal-organic framework material,magnetic MIL-101(Fe)composite,was successfully synthesized through hydrothermal reaction.MIL-101(Fe)composite was used as a magnetic solid phase extraction(MSPE)agent,which was coupled with inductively coupled plasma mass spectrometry(ICP-MS)to realize the efficient and sensitive analysis of trace heavy metal ions.The synthesized magnetic MIL-101(Fe)composite was characterized by scanning electron microscopy,transmission electron microscopy,X-ray diffraction and X-ray photoelectron spectroscopy.The extraction parameters including solution pH,adsorption time and desorption time,were optimized by batch adsorption experiments.The experimental results showed that the magnetic solid phase extraction agent had good crystal structure and surface functionalized nanoparticles.Under the optimized experimental conditions,the established MSPEICP-MS method had a linear range of 0.5~500μg/L,the detection limits of As(III),Pb(II)and Cu(II)ions were 0.177-0.301μg/L,and the relative standard deviations were 1.7%-3.2%.The recycled magnetic MIL-101(Fe)composite had good reusability,and the recovery was higher than 82%after seven adsorption-desorption cycles.The method has been applied to the determination of trace heavy metal ions in environmental water samples.The recoveries of arsenic,lead and copper ions in seawater and lake water samples ranged from 90.0%to 113.2%.This method can be used for the determination of trace heavy metals in environmental water samples.

关 键 词：磁性固相萃取 电感耦合等离子体质谱 金属有机骨架材料 重金属离子 

分 类 号：O657.63[理学—分析化学]