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摘要毛细管电色谱（CEC）是具有高效液相色谱（HPLC）和毛细管电泳（CE）的混合动力技术，它在复杂混合物的分析中有望达到高分离效率。而找到一种合适的材料作为毛细管中固定相是制备填充柱关键的一步。本论文将石墨烯应用于电色谱分离，研究工作主要有：将氨基化的SiO2与氧化石墨烯反应，再将反应物还原得到石墨烯修饰的二氧化硅微球，将其作为毛细管电色谱的固定相。采用匀浆法在高压下制备石墨烯毛细管填充柱，以硫脲和苯系物作为分离样品来评价填充柱的性能，研究了流动相比例在石墨烯填充柱分离稠环芳烃混合物的影响。在最佳条件下，石墨烯填充柱可以将苯系物成功分离，且对硫脲的最优柱效可以达到12,678块/m。47590
Abstract: Capillary electrochromatography（CEC）is a promising technology which has both advantages of high-performance liquid chromatography (HPLC) and capillary electrophoresis(CE), and hence high efficiency in the seperation of complex mixture is anticipated. It is essential to select a favorable material as the stationary phase for the fabrication of packed columns. In this thesis, we used the silica modified by graphene as the stationary phase. Our research work mainly focused on: we reducted silica particles modified by graphene oxide to give graphene-modified silica particles, then the silica modified by graphene was used as the stationary phase. We produced graphene coated capillary packed column under high pressure. To evaluate the analytical performance of the packed column, thiourea and benzene deriatives were used as the analytes. Effects of the proportion of the mobile phase on electrochromatographic separation were investigated. The experimental results showed that:benzene, naphthalene and fluorene could be baseline separated using the graphene coated capillary packed column, and the theoretical plate number up to 12,678 was achieved.
毕业论文关键词：毛细管电色谱； 毛细管填充柱； 石墨烯； 稠环芳烃； 分离
KeyWord: capillary electrochromatography; capillary packed column; graphene; polycyclic aromatic hydrocarbons; separation.
目 录 4
1 引言 5
1.1 毛细管电色谱 5
1.1.1毛细管电色谱的研究背景 5
1.1.2 毛细管电色谱原理 6
1.1.3 毛细管填充柱 6
1.1.4 加压电色谱仪器 7
1.2 毛细管电色谱固定相 8
1.3 石墨烯 9
1.3.1 石墨烯性质及应用 9
1.3.2 石墨烯的制备方法 9
2 实验部分 10
2.1 主要实验试剂 10
2.2 主要实验仪器 11
2.3 实验过程 13
2.3.1 石墨烯的制备 13
2.3.2 填充柱的制备 13
2.3.3 毛细管柱性能评价 14
2.3.3.1 溶剂准备 14
2.3.3.2 加压电色谱系统准备 14
3 结果讨论 15
3.1 经修饰的SiO2微球的表征 15
3.2 石墨烯填充柱的性能评价 15
3.2.1 石墨烯对填充柱性能的影响