Courtois Julien, Szumski Michal, Byström Emil, Iwasiewicz Agnieszka, Shchukarev Andrei, Irgum Knut
Department of Chemistry, Umeå University, Umeå, Sweden.
J Sep Sci. 2006 Jan;29(1):14-24. doi: 10.1002/jssc.200500294.
Based on a survey of the literature on pretreatment of fused silica capillaries, 3 etching procedures and 11 silanization protocols based on the vinylic silane 3-((trimethoxysilyl)propyl) methacrylate (gamma-MAPS) were found to be most representative as a means of ensuring attachment of in situ prepared vinylic polymers. These techniques were applied to fused silica capillaries and the success in establishing the intended surface modification was assessed. X-ray photoelectron spectroscopy (XPS) was used to characterize the chemical state of the surface, providing information regarding presence of the reagent bound to the capillary. Wetting angles were measured and correlated with the XPS results. An adherence test was done by photopolymerization of a 2 mm long plug of 1,6-butanediol dimethacrylate in the prepared capillaries and evaluation of its ability to withstand applied hydraulic pressure. SEM was also performed in cases where the plug was released or other irregularities were observed. Finally, the roughness of the etched surface, considered to be of importance, was assessed by atomic force microscopy. Alkaline etching at elevated temperature provided a surface roughness promoting adhesion. The commonly used silanization protocols involving water in the silanization or washing steps gave inadequate surface treatment. The best silanization procedure was based on toluene as a solvent.
基于对熔融石英毛细管预处理文献的调查，发现3种蚀刻程序和11种基于乙烯基硅烷甲基丙烯酸3-（三甲氧基硅基）丙酯（γ-MAPS）的硅烷化方案是确保原位制备的乙烯基聚合物附着的最具代表性的方法。这些技术应用于熔融石英毛细管，并评估了实现预期表面改性的成功率。使用X射线光电子能谱（XPS）表征表面的化学状态，提供有关与毛细管结合的试剂存在的信息。测量接触角并将其与XPS结果相关联。通过在制备的毛细管中光聚合2 mm长的1,6-丁二醇二甲基丙烯酸酯塞并评估其承受施加的液压的能力来进行粘附测试。在塞子脱落或观察到其他不规则情况时也进行扫描电子显微镜（SEM）检查。最后，通过原子力显微镜评估被认为很重要的蚀刻表面粗糙度。高温碱性蚀刻提供了促进粘附的表面粗糙度。在硅烷化或洗涤步骤中涉及水的常用硅烷化方案表面处理不足。最佳的硅烷化程序是以甲苯为溶剂。
