色谱

色谱 ›› 2011, Vol. 29 ›› Issue (05): 426-429.DOI: 10.3724/SP.J.1123.2011.00426

• 研究论文 • 上一篇    下一篇

干凝胶无机整体柱的制备及评价

严逢川, 陈波*   

  1. 湖南师范大学 化学生物学及中药分析教育部重点实验室, 湖南 长沙 410081
  • 收稿日期:2010-11-02 修回日期:2011-03-14 出版日期:2011-05-28 发布日期:2011-05-28
  • 通讯作者: 陈波,教授,主要研究方向为药物与色谱分析. Tel: (0731)88865515
  • 基金资助:

    国家自然科学基金、国家“863”课题及湖南省科技计划课题资助

Preparation and evaluation of silica xerogel monolithic column

YAN Fengchuan, CHEN Bo*   

  1. Key Laboratory of Chemical Biology & Traditional Chinese Medicine Research, Ministry of Education, Hunan Normal University, Changsha 410081, China
  • Received:2010-11-02 Revised:2011-03-14 Online:2011-05-28 Published:2011-05-28

PDF

1530

被引次数

28

摘要： 以硅酸钾为硅源,甲酰胺为催化剂在毛细管内原位聚合形成干凝胶柱,制备了一系列致密度不同的整体柱。该法在柱制备及高温干燥过程中不会发生柱床断裂和塌陷现象,此特点明显优于以烷氧基硅烷为前驱体制备无机整体柱的方法。考察了不同模数硅酸钾对整体柱柱床结构的影响,用扫描电镜(SEM)和氮吸附法对整体柱结构进行了表征,考察了整体柱柱压与流速的关系;对整体柱进行十八烷基修饰后,测定了反相整体柱(C18整体柱)对蒽的柱效,通过考察甲苯在该柱上的突破曲线,获得了其对甲苯的柱容量。结果显示该整体柱柱床刚性好,在高温、高柱压、高流速时柱床能保持其物理结构的稳定性,对蒽的柱效达到41400理论塔板/m,对甲苯的柱容量为61 ng。

关键词: 干凝胶, 硅酸钾, 甲酰胺, 稳定性, 无机整体柱

Abstract: Using potassium silicate as silicon source, formamide as catalyst, a series of silica xerogel monolithic columns with different consistencies were prepared. The column bed would not rupture and collapse during drying at high temperatures. This is the biggest advantage compared with the inorganic monolithic columns using alkoxy silane as precursor. The effect of the modulus of potassium silicate on the physical structure of the monolithic column was investigated. The monolithic silica columns were characterized by scanning electron micrograph (SEM) and nitrogen adsorption. The relationship between column pressure and flow rate was evaluated. The column efficiency for anthracene was tested. The breakthrough curve for toluene was studied. The results showed that the column bed could maintain good stability at high temperatures, high column pressures, and high flow rates. The column efficiency of 41400 plates/m was achieved for anthracene. The column capacity for toluene was 61 ng.