Zhao Hongyan, Wang Yuanchao, Cheng Heyong, Shen Yili
College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036, China.
College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036, China.
J Chromatogr A. 2016 Jun 24;1452:27-35. doi: 10.1016/j.chroma.2016.05.001. Epub 2016 May 3.
In this work, GO bonded monolith (pAS-GO@PS-DVB) as the stationary phase for capillary electrochromatography was fabricated, which was achieved by a simple one-step in-situ copolymerization of styrene and vinylized GO in the presence of divinylbenzene as a cross-linker. GO functionalization was primarily completed using p-aminostyrene based on condensation reaction between amino and carboxyl groups. The characterization by infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction and scanning electron microscopy proved the covalent bonding of GO on the monolith. The average pore diameter via Barrett-Joyner-Halenda, specific surface area and pore volume via Brunauer-Emmett-Teller equation by nitrogen adsorption/desorption were determined to be 112.4nm, 485.8m(2)g(-1) and 1.4cm(3)g(-1), respectively. The pAS-GO@PS-DVB monolithic column gave effective separation for a wide range of aromatic compounds, which was based on hydrogen bonding and π-π interactions of GO with polar and/or non-polar organic compounds. The reproducibility in terms of the precisions of migration time, peak height and peak area was estimated below 6% using thiourea and other aromatic compounds. Furthermore, the differences of migration time, peak height and peak area between the first-week analysis and the forth-week analysis were less than 19%, indicating good stability of the proposed monolithic column in one month. The applicability of the pAS-GO@PS-DVB monolith was also demonstrated by baseline separation of three phenols and three anilines.
在本工作中,制备了氧化石墨烯键合整体柱(pAS-GO@PS-DVB)作为毛细管电色谱的固定相,该整体柱通过在二乙烯基苯作为交联剂存在的情况下,使苯乙烯和乙烯化氧化石墨烯进行简单的一步原位共聚反应来实现。基于氨基和羧基之间的缩合反应,主要使用对氨基苯乙烯完成氧化石墨烯的功能化。通过红外光谱、X射线光电子能谱、X射线衍射和扫描电子显微镜进行的表征证明了氧化石墨烯在整体柱上的共价键合。通过巴雷特-乔伊纳-哈伦达法测定的平均孔径,以及通过氮吸附/脱附采用布鲁诺尔-埃米特-特勒方程测定的比表面积和孔体积分别为112.4nm、485.8m²/g和1.4cm³/g。pAS-GO@PS-DVB整体柱基于氧化石墨烯与极性和/或非极性有机化合物之间的氢键和π-π相互作用,对多种芳香族化合物实现了有效分离。使用硫脲和其他芳香族化合物,迁移时间、峰高和峰面积精度方面的重现性估计低于6%。此外,第一周分析和第四周分析之间迁移时间、峰高和峰面积的差异小于19%,表明所提出的整体柱在一个月内具有良好的稳定性。三种酚类和三种苯胺类化合物的基线分离也证明了pAS-GO@PS-DVB整体柱的适用性。