title: Reconstruction and characterization of a polymer-based monolithic stationary phase using serial block-face scanning electron microscopy.
abstract: 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-divinylbenzene) monolith in capillary column format from a sample volume of 60.5 × 60.5 × 19.9 μm(3) 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 μm, 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.
authors.affiliation: Department of Chemistry, Philipps-Universität Marburg, Hans Meerwein Strasse, 35032 Marburg, Germany.
authors.forename: Tibor
authors.initials: T
authors.lastname: Müllner
authors.forename: Armin
authors.initials: A
authors.lastname: Zankel
authors.forename: Claudia
authors.initials: C
authors.lastname: Mayrhofer
authors.forename: Herbert
authors.initials: H
authors.lastname: Reingruber
authors.forename: Alexandra
authors.initials: A
authors.lastname: Höltzel
authors.forename: Yongqin
authors.initials: Y
authors.lastname: Lv
authors.forename: Frantisek
authors.initials: F
authors.lastname: Svec
authors.forename: Ulrich
authors.initials: U
authors.lastname: Tallarek