摘要
为了进一步开发气相色谱(gas chromatography, GC)分离的固定相材料,首次对杯[6]芳烃上、下缘改性合成了一种新型杯[6]芳烃材料(C6A-NH2),通过核磁共振氢谱(1H-nuclear magnetic resonance,1H-NMR)、质谱(mass spectrum, MS)和红外光谱(infrared spectroscopy, IR)等手段对所合成的C6A-NH2进行结构确证。结果表明:采用TGA热重分析测得其热稳定温度高达310℃,使用静态涂渍法制柱后,测得C6A-NH2毛细管色谱柱为中等极性,以正十二烷为探针化合物在120℃下测得的柱效为2 600板/m。C6A-NH2柱的分离性能和保留行为研究表明:C6A-NH2柱对Grob试剂、17组分混合物、脂肪族与芳香族分析物、位置和顺反异构体等均具有良好的分离能力,尤其是对17组分混合物的分离,C6A-NH2柱的分离能力优于C6A柱,且表现出了独特的保留行为。
In order to further develop the stationary phases for gas chromatography(GC)separations,a novel calix[6]arene-based derivative(C6A-NH 2)was firstly synthesized by modifying the upper and lower edges of calix[6]arene.The structure of the synthesized C6A-NH 2 was characterized by 1H-NMR,MS and IR.The thermal stability was up to 310℃by carrying out the thermogravimetric analysis(TGA).After static coating,the C6A-NH 2 capillary column showed medium polarity and the column efficiency at 120℃by n-dodecane was 2600 plates/m.The research on the separation performance and retention behavior of C6A-NH 2 column showed that it has good resolving capacity for Grob reagent,the mixture of 17 components,aliphatic and aromatic analytes,position and cis/trans-isomers.Especially for the mixture of 17 components,C6A-NH 2 column exhibited higher resolution than C6A column and showed unique retention behavior.
作者
蔡志强
李伟
章围
帅筱敏
黄秋晨
陈若男
李琼璐
吴澳萍
孙涛
CAI Zhiqiang;LI Wei;ZHANG Wei;SHUAI Xiaomin;HUANG Qiuchen;CHEN Ruonan;LI Qionglu;WU Aoping;SUN Tao(School of Petrochemical Engineering,Liaoning Province Professional and Technical Innovation Center for Fine Chemical Engineering of Aromatics Downstream,Shenyang University of Technology,Liaoyang 111003,China;College of Chemistry and Chemical Engineering,Henan Key Laboratory of Function-Oriented Porous Materials,Luoyang Normal University,Luoyang 471934,China)
出处
《广西大学学报（自然科学版）》
CAS
北大核心
2023年第3期711-719,共9页
Journal of Guangxi University（Natural Science Edition）
基金
国家自然科学基金项目(21705072)
辽宁省自然科学基金项目(20180550016)
辽宁省教育厅科学研究项目(LJGD2020015)。
关键词
杯芳烃
固定相
气相色谱
分离性能
异构体
calix arene
stationary phase
gas chromatography
separation performance
isomer
