A comprehensive undergraduate experiment: preparation and chromatographic evaluation of a core-shell stationary phase based on a covalent organic framework

doi:10.3724/SP.J.1123.2024.03003

Abstract

Abstract:

Continuously promoting new curriculum standards is a key aim of the Ministry of Education of China. With this in mind, this paper introduces a comprehensive teaching experiment for undergraduate instrumental analysis courses that aims to improve students’ material-preparation and instrumental-analysis skills through practice. Herein, a covalent organic framework-based core-shell stationary phase material (SiO₂@COF_TTA-DHTA) is prepared via a one-pot method and characterized in detail, after which its chromatographic properties are evaluated by high performance liquid chromatography (HPLC). The experimental process includes material synthesis and characterization, as well as studying the chromatographic-retention behavior and chromatographic-separation performance of the material. By the combining theoretical science and experimental teaching, this experiment not only deepens students’ understanding of the properties of functional materials and their applications, but also improves their experimental-design and critical-thinking skills. This experiment not only cultivates students’ interests in scientific research, but also exercises their experimental, operational, innovative-thinking, and practical abilities, while concurrently enhancing their sense of social responsibility and historical mission, thereby delivering the all-round educational goals of experimental teaching.

Key words: comprehensive experiment, covalent organic framework, chromatographic stationary phase, core-shell structure

CLC Number:

O658

LIU Jin, TIAN Wenchang, WU Fan, ZHANG Qiuting, ZHONG Yanhui, LIN Zian. A comprehensive undergraduate experiment: preparation and chromatographic evaluation of a core-shell stationary phase based on a covalent organic framework[J]. Chinese Journal of Chromatography, 2024, 42(10): 1006-1012.

Figures/Tables 6

Fig. 1 Scheme for the preparation of the SiO2@ COFTTA-DHTA packed column COF: covalent organic framework; TTA: 1,3,5-tris-(4-aminophenyl)triazine; DHTA: 2,5-dihydroxy-1,4-benzenedicarboxaldehyde.

Fig. 2 (a) FT-IR spectra of SiO2-NH2, SiO2@COFTTA-DHTA and COFTTA-DHTA; (b) powder X-ray diffraction (PXRD) patterns of COFTTA-DHTA and SiO2@COFTTA-DHTA; SEM images of (c) SiO2-NH2 and (d) SiO2@COFTTA-DHTA; and TEM images of (e) SiO2-NH2 and (f) SiO2@COFTTA-DHTA

Fig. 3 Effect of ACN content in mobile phase on separation of alkyl benzenes

Fig. 4 Chromatograms of polycyclic aromatic hydrocar- bons on the SiO2@COFTTA-DHTA and SiO2-NH2 packed columns Analytes: 1. benzene; 2. naphthalene; 3. fluorene; 4. phenanthrene; 5. biphenyl; 6. acenaphthene; 7. p-terphenyl; 8. triphenyl.

Fig. 5 Chromatograms of aniline compounds on the SiO2@COFTTA-DHTA and SiO2-NH2 packed columns Analytes: 1. aniline; 2. tetravinylaniline; 3. naphthylamine; 4. diphenylamine.

Fig. 6 Chromatograms of PM2.5 sample, standard solution of quinones and PM2.5 spiked sample on the SiO2@COFTTA-DHTA packed column Analytes: 1. 1,4-naphthoquinone; 2. acenaphthene quinone; 3. phenquinone; 4. anthraquinone; 5. 2- methylanthraquinone.

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