溶胶—凝胶法制备新型毛细管气相色谱柱

【作者】 吴秀红；

【导师】 王东新；

【作者基本信息】 南京师范大学 ， 物理化学， 2005， 硕士

【摘要】 本论文共有4个部分: 1、首先回顾了气相色谱的发展,简单介绍气相色谱仪的基本结构、评价色谱柱性能的方法,简述了目前使用的几类色谱固定相;接着详细的介绍了传统毛细管气相色谱柱的制备过程,并指出了相关步骤的缺陷。 2、第二章节对溶胶-凝胶化学过程作了简要叙述,讨论了毛细管柱材料的内表面结构,着重介绍溶胶凝胶制柱的原理、步骤,并探讨了该制柱过程可能的影响因素。 3、分别把三乙醇胺、端羟基β-氰乙基甲基聚硅氧烷、2,6-二丁基-β-环糊精、单硬脂酸甘油酯、柠檬酸三丁酯作为气相色谱固定相,使用溶胶-凝胶法制备成毛细管气相色谱柱,并进行了柱极性、分离能力、热稳定性、柱效等的考察,获得了较为理想的结果。与传统制柱法制得的毛细管柱相比,溶胶-凝胶柱具有更高的热稳定性,更好的惰性,主要是由于涂层与毛细管内壁之间的化学键合;并对游离的脂肪酸、酚类、醇类、胺类、醛、酮以及二醇具有良好的分离能力。 4、使用自制的溶胶-凝胶端羟基聚硅氧烷毛细管气相色谱柱对某些卫生用品中的樟脑或者中成药中龙脑的含量进行了测定,结果表明,方法具有操作简便、分析速度快、精密度高、准确度高等特点。更多还原

【Abstract】 The thesis includes the following four sections:Section 1: The history about the development of Gas Chromatography is reviewed briefly, and the typical configuration of a Gas Chromatograph is described. Then, conventional capillary column fabrication approach is introduced including surface treatment, deactivation, coating and stationary phase immobilization. Section 2: This section mainly introduces the sol-gel chemistry, the typical method of preparing sol-gel capillary column and the main influence factors in the preparation of the sol-gel capillary column.Section 3: The special methods of preparation of sol-gel capillary columns for GC are introduced with the following as stationary phases: Triethanol Amine, Hydroxy-terminated poly(cyanoethylmethyl)siloxane, Heptakis(2,6-di-O-ethyl)- β -cyclodextrin, Glycerolmon Ostearate and Tributyl Citrate. On these columns the polarity of the stationary phases, the separation power, the column efficiency and the thermal stability are studied. Results show that these columns have excellent thermal stability, high column efficiency, good inertness. Compared with the columns made using conventional approach, the higher thermal stability of the the sol-gel columns is owing to the formation of chemical bonds between the coating layer and the inner wall of the capillary. So is the inertness. The sol-gel columns also provide efficient separations for analytes including free fatty acids, phenolic compounds, amines, aldehydes, ketones, alcohols ,diols etc.Section 4: sol-gel capilliary polydimethylsiloxane column is used for quantitative determination of naphthalene ,camphor and borneol. The experiment results show that the sol-gel columns can provide excellent quantitative determination. The methods are simple , accurate , rapid and useful.更多还原