Al2O3-PLOT毛细管色谱柱的溶胶-凝胶法制备

Preparation of Sol-Gel Al_2O_3-PLOT Capillary Column

首次将溶胶－凝胶法用于制备Al2O3-PLOT毛细管色谱柱。采用正硅酸乙酯、稀盐酸以及氧化铝的乙醇悬浮液组成的溶胶体系，高压动态法涂敷石英毛细管，然后通过高温凝胶反应固定Al2O3 涂层，再用无机盐溶液淋洗灭活得到成品。考察制备过程的重复性，表明溶胶一凝胶法制备Al2O3-PLOT色谱柱简单易行，重复性好；对色谱柱性能进行评价，18组分C1～C5烃类标准气完全基线分离，环丙烷和丙烯的分离度为1．55～1．65，甲烷和正丁烷保留时间变化范围分别小于0．5％和1％，色谱柱的耐温性和稳定性显著提高。

A novel method was developed to prepare Al2O3 porous-layer open-tubular（Al2O3-PLOT） column based on the sol - gel chemistry. A cleaned fused silica capillary was prepared by coating with a sol - gel solution comprised of tetraethyl orthosilicate （TEOS）, hydrochloric acid （HC1） and sus- pension of aluminium oxide in ethanol. The Al2O3 coat could be fixed in surface of column by gelation at high temperature, following by an additional modification using inorganic salt. The eolumn performanee was evaluated by using C1 - C5 hydrocarbons sample. The result showed that, comparing with the column made by liquid sediment method, the column prepared by sol - gel method has better separation performance, larger column capacity and higher operation temperature. After using six months, the resolution of eyclopropane and propylene varies between 1.55 and 1.65, the variety ranges of retention time of methane and butane were less than 0. 5% and 1% , respectively. The results indicated that the column also had better stability, and was applied in the separation of hydrocarbons with satisfactory result.