色谱

色谱 ›› 2025, Vol. 43 ›› Issue (6): 705-709.DOI: 10.3724/SP.J.1123.2024.05018

• 教学研究 • 上一篇    

磁性共价有机骨架的制备及应用——仪器分析开放性实验教学实践

江丹丹1, 贾琼2,*()   

  1. 1.内蒙古民族大学化学与材料学院，内蒙古 通辽 028000
    2.吉林大学化学学院，吉林 长春 130012
  • 收稿日期:2024-08-02 出版日期:2025-06-08 发布日期:2025-05-21
  • 通讯作者: * Tel：（0431）85168436，E-mail：jiaqiong@jlu.edu.cn.
  • 基金资助:
    内蒙古民族大学博士科研启动基金(BS516);内蒙古民族大学校级教育教学研究课题(QN2024003)

Preparation and application of magnetic covalent organic framework： open experimental teaching practice of instrumental analysis

JIANG Dandan1, JIA Qiong2,*()   

  1. 1. College of Chemistry and Materials Science，Inner Mongolia Minzu University，Tongliao 028000，China
    2. College of Chemistry，Jilin University，Changchun 130012，China
  • Received:2024-08-02 Online:2025-06-08 Published:2025-05-21
  • Supported by:
    Inner Mongolia Minzu University Doctoral Research Startup Fund Project(BS516);Education and Teaching Research Project of Inner Mongolia Minzu University(QN2024003)

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摘要：

针对当前有机合成实验在性质研究方面的不足以及仪器分析实验方法相对独立、缺乏整合性的现状，我们设计了一个本科生开放性实验。本实验将有机合成与仪器分析实验进行结合，构建了一个包含材料合成与表征、羟基多氯联苯的吸附性能及检测方法探究的本科生创新实验。首先，采用正硅酸四乙酯对Fe3O4进行处理，引入3-氨基丙基三甲氧基硅烷制备氨基改性的Fe3O4。随后，加入三甲酰氯和对苯二胺单体用于制备磁性共价有机骨架（MCOF）。本实验利用红外光谱仪和热重分析仪对MCOF的表面基团和热稳定性进行了表征。最后，将MCOF应用于辽河水样中羟基多氯联苯的吸附，并结合液相色谱法进行检测。在实验过程中，学生不仅能够掌握羟基多氯联苯的分离和检测方法，而且能够对羟基多氯联苯在辽河水样品中的含量情况有所了解。通过实验结果的分析和讨论，使学生深刻地认识到仪器分析实验在环境监测中的重要地位。这一系统的实验流程，不仅能够提高学生综合运用无机化学、有机化学和仪器分析基础知识的能力，而且有助于提高学生分析问题、解决问题的能力及实践操作能力。同时，这一开放性实验的开展有助于提高实验室仪器设备的利用率，充分发挥实验室现有资源的作用。

关键词: 开放性实验, 仪器分析, 磁性共价有机骨架, 羟基多氯联苯, 液相色谱

Abstract:

Organic synthesis experiments are often deficient and involve relatively independent experimental instrumental-analysis methods that lack integration. Accordingly， an open-instrument-analysis experiment was designed to address these shortcomings； this experiment combines organic synthesis with instrumental analysis to deliver an innovative undergraduate experiment that includes material preparation and characterization， investigating the adsorption performance of hydroxylated polychlorinated biphenyl， and exploring detection methods. First， Fe3O4 was treated with tetraethyl orthosilicate， after which 3-aminopropyltrimethoxysilane was introduced to prepare amino-modified Fe3O4. Trimesoyl chloride and p-phenylenediamine are then added as monomers to synthesize a magnetic covalent organic framework （MCOF）. The surface groups and thermal stability of the MCOF were then characterized using Fourier-transform infrared spectroscopy and thermogravimetric analysis， after which the MCOF was used to determine hydroxylated polychlorinated biphenyl in Liaohe River water samples using liquid chromatography. During this experiment， students master separation and detection methods for hydroxylated polychlorinated biphenyl， while also learning about its levels in the Liaohe River. Students will recognize the important role that instrumental analysis plays in environmental monitoring by analyzing and discussing the experimental results； they will also improve their abilities to comprehensively apply basic inorganic chemistry， organic chemistry， and instrumental-analysis knowledge， while also improving their abilities to operate， analyze， and solve problems. Implementing this open experiment will help to improve the use of laboratory equipment and fully utilize existing laboratory resources.

Key words: open experiment, instrumental analysis, magnetic covalent organic framework, hydroxylated polychlorinated biphenyl, liquid chromatography

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