有机-无机杂化溶胶-凝胶涂层对不锈钢毛细管色谱柱的脱活作用研究  

Study of the Deactivation of the Organic-Inorganic Hybrid Sol-Gel Coatings on Stainless Steel Tubes

作　　者：韩江华[1] 杨海鹰[1] 

机构地区：[1]中国石油化工股份有限公司石油化工科学研究院,北京100083

出　　处：《色谱》2002年第2期121-124,共4页Chinese Journal of Chromatography

摘　　要：用甲基三乙氧基硅烷和四乙氧基硅烷水解缩合后形成的有机 无机杂化溶胶 凝胶 (sol gel)涂层对国产气相色谱用不锈钢毛细管柱进行脱活。通过气相色谱法研究了不同老化温度下所得脱活涂层的色谱行为。结果表明这种涂层不但对不锈钢柱内壁活性点有很好的遮盖作用 ,而且本身具有相当的分离能力。在 2 5 0℃下老化的涂层可使碳原子数在 12以下的正构烷烃达到基线分离 ,与未用涂层的不锈钢裸柱相比 ,吸附活性大大降低 ;但随着老化温度的升高 ,涂层在缩聚老化过程中产生不均匀微孔 ,对被分离物的作用力加强。该脱活方法所用设备简单、操作容易、脱活层的耐温性能好 ,是一种简单而有效的脱活方法。The organic-inorganic hybrid sol-gel coatings used as deactivating substance for stainless steel tubes in gas chromatography have been prepared by dynamic processing of the sol-gel solution produced by hydrolysis and polycondensation of methyltriethoxysilane and tetraethoxysilane under acidic conditions. The chromatographic behavior of the coatings was studied by GC at different aging temperatures. The experimental results indicate that the active sites on the inner surface of the stainless steel tubes have been shielded effectively by the coatings and the coatings also have the ability to separate hydrocarbons. If the coatings were aged only at 250 ℃, the hydrocarbons with the number of carbon under 12 can be separated with perfect baseline. Compared with the results obtained from the untreated stainless steel tubes the adsorbent activation of the treated stainless steel tubes has decreased greatly. It is also found that when the aging temperature was increased, the action between the coatings and the samples was enhanced, mainly produced by the porous structure of the coatings. This phenomenon is also discussed using the tailing factors.

关 键 词：气相色谱法 不锈钢柱管 溶胶-凝胶涂层 脱活作用 有机-无机杂化涂层 毛细管色谱柱 

分 类 号：O657.71[理学—分析化学]