硅胶整体柱的制备及其能评价

发布时间：2017-12-30 18:10

本文关键词：硅胶整体柱的制备及其能评价　出处：《北京化工大学》2016年硕士论文　论文类型：学位论文

【摘要】：高效液相色谱法(HPLC)以其分离效率高、选择性好、灵敏度高、分析速度快、适用范围广等特点得到广泛应用。色谱柱作为高效液相色谱技术的“心脏”,高性能的色谱填料是色谱发展中最丰富、最具有创造性和挑战性的研究。整体柱与传统填充柱相比,具有柱压低、速度快、可进行速度梯度洗脱等优势,广泛应用于大分子的分离,成为近些年来发展非常快的色谱固定相。本文以单晶硅粉水解生成的二氧化硅水溶胶为硅源,在碱性条件(pH=8-9)下,以聚乙二醇(PEG)为致孔剂,四甲氧基硅烷(TMOS)作交联剂,通过溶胶-凝胶法(sol-gel)制备出高纯、同时具有通孔和中孔的硅胶整体柱,开创了一种新的硅胶整体柱制备方法。采用扫描电镜(SEM)、红外(IR)、固体核磁(NMR)、元素分析和BET氮脱附等手段表征了硅胶整体柱的结构与性能,并对十八烷基硅烷键合前后的硅胶整体柱进行了色谱评价。(1)本实验探讨了烷氧基硅烷试剂的类型、二氧化硅水溶胶的固含量、二氧化硅水溶胶／烷氧基硅烷试剂的比例、PEG分子量、PEG加入量、体系pH、陈化温度、煅烧温度等条件对硅胶整体柱制备的影响,经SEM、BET等分析手段对通孔和比表面积进行了表征；以正己烷作为流动相,对苯酚、苯、甲苯和邻苯二甲酸二丁酯进行了色谱分离,得到了较为满意的分离效果。(2)通过在硅胶整体柱表面键合二甲基十八烷基氯硅烷(C18)合成了反相色谱模式的固定相。经元素分析、IR、NMR等分析手段对键合后的硅胶整体柱固定相进行了表征；以甲醇和水作为流动相,在反相色谱模式下对苯酚、苯、甲苯和邻苯二甲酸二丁酯进行了分离,表现出了整体柱的高渗透性、高速、高效等分离优势,取得了比较满意的效果。
[Abstract]:High performance liquid chromatography (HPLC) is characterized by high separation efficiency, good selectivity, high sensitivity and high analytical speed. The chromatographic column is the "heart" of the high performance liquid chromatography technology, and the high performance chromatographic packing is the most abundant in the development of the chromatography. The most creative and challenging research. Compared with the traditional packed column, the monolithic column has the advantages of low column pressure, high speed, can be eluted by velocity gradient, and widely used in the separation of macromolecules. In this paper, silica hydrosol produced by hydrolysis of monocrystalline silicon powder was used as silicon source under alkaline conditions (pH = 8-9). High purity was prepared by sol-gel method using polyethylene glycol (PEG) as pore-forming agent and tetramethoxysilane (TMOS) as crosslinking agent. A new preparation method of silica gel monolithic column with both through pore and mesopore was developed. Scanning electron microscope (SEM), IR (IR) and solid nuclear magnetic resonance (NMRs) were used to prepare silica gel monolithic column. The structure and properties of silica gel monolithic column were characterized by elemental analysis and BET nitrogen desorption. The type of alkoxy silane reagents and the solid content of silica hydrosol were investigated. The effect of the ratio of silica hydrosol / alkoxy silane reagent on the preparation of silica monolithic column was studied by SEM. The through pore and specific surface area were characterized by BET. Using n-hexane as mobile phase, phenol, benzene, toluene and dibutyl phthalate were separated by chromatography. The stationary phase of reversed phase chromatographic mode was synthesized by bonding dimethyl 18 alkyl chlorosilane C18 on the silica gel monolithic column, and IR was analyzed by elemental analysis. The bonded silica monolithic stationary phase was characterized by NMR. Using methanol and water as mobile phase, phenol, benzene, toluene and dibutyl phthalate were separated in reverse phase chromatography mode, showing the advantages of high permeability, high speed and high efficiency. Satisfactory results have been obtained.
【学位授予单位】：北京化工大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O652.63

【相似文献】