Reconstruction and Characterization of a Polymer-Based Monolithic Stationary phase using Serial Block-Face Scanning Electron Microscopy

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• 作者：Tibor M眉llner ; Armin Zankel ; Claudia Mayrhofer ; Herbert Reingruber ; Alexandra H枚ltzel ; Yongqin Lv ; Frantisek Svec ; Ulrich Tallarek
• 刊名：Langmuir
• 出版年：2012
• 出版时间：December 11, 2012
• 年：2012
• 卷：28
• 期：49
• 页码：16733-16737
• 全文大小：352K
• 年卷期：v.28,no.49(December 11, 2012)
• ISSN：1520-5827

文摘

Porous, polymer-based materials are increasingly used as stationary phases in separation science and catalysis, yet their morphology remains largely unknown. The main difficulty lies in reconciling their soft matter nature with the demands of microscopic imaging techniques. We analyze the morphology of a hyper-cross-linked poly(styrene鈥揹ivinylbenzene) monolith in capillary column format from a sample volume of 60.5 脳 60.5 脳 19.9 渭m³ reconstructed by serial block-face scanning electron microscopy. To obtain a suitable specimen, the polymer skeleton was stained with tetraphenyllead and the void space filled with resin before the whole monolith was resin-embedded after removing the fused-silica capillary. Chord length distribution analysis revealed characteristic lengths of 7.32 and 0.73 渭m, corresponding to two distinct macropore types. The macroporosity (77% on average) was found to increase systematically from the wall to the center. Our results provide valuable insights into the formation process of the monolith and its stationary-phase properties.