Jiang Dan-Dan, Jia Qiong
College of Chemistry and Materials Science,Inner Mongolia Minzu University,Tongliao 028000,China.
College of Chemistry,Jilin University,Changchun 130012,China.
Se Pu. 2025 Jun;43(6):705-709. doi: 10.3724/SP.J.1123.2024.05018.
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, FeO was treated with tetraethyl orthosilicate, after which 3-aminopropyltrimethoxysilane was introduced to prepare amino-modified FeO. Trimesoyl chloride and -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.
有机合成实验往往存在不足,且涉及相对独立的实验仪器分析方法,缺乏整合性。因此,设计了一个开放式仪器分析实验来解决这些缺点;该实验将有机合成与仪器分析相结合,提供了一个创新的本科实验,包括材料制备与表征、研究羟基化多氯联苯的吸附性能以及探索检测方法。首先,用正硅酸乙酯处理FeO,然后引入3-氨丙基三甲氧基硅烷制备氨基改性的FeO。接着加入均苯三甲酰氯和对苯二胺作为单体合成磁性共价有机骨架(MCOF)。然后使用傅里叶变换红外光谱和热重分析对MCOF的表面基团和热稳定性进行表征,之后使用MCOF通过液相色谱法测定辽河水样中的羟基化多氯联苯。在这个实验过程中,学生掌握了羟基化多氯联苯的分离和检测方法,同时也了解了其在辽河中的含量水平。通过分析和讨论实验结果,学生将认识到仪器分析在环境监测中所起的重要作用;他们还将提高综合应用基础无机化学、有机化学和仪器分析知识的能力,同时提高操作、分析和解决问题的能力。实施这个开放实验将有助于提高实验室设备的利用率,并充分利用现有的实验室资源。