Reconstruction and characterization of a polymer-based monolithic stationary phase using serial block-face scanning electron microscopy

Langmuir

Volumn 28, Issue 49, 2012, Pages 16733-16737

  Müllner, Tibor ^a   Zankel, Armin ^b   Mayrhofer, Claudia ^b   Reingruber, Herbert ^b   Höltzel, Alexandra ^a   Lv, Yongqin ^c   Svec, Frantisek ^c   Tallarek, Ulrich ^a  

^a PHILIPPS UNIVERSITY MARBURG   (Germany)

^b GRAZ UNIVERSITY OF TECHNOLOGY   (Austria)

^c LAWRENCE BERKELEY NATIONAL LABORATORY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

CAPILLARY COLUMNS; CHARACTERISTIC LENGTH; CHORD LENGTH DISTRIBUTION; FORMATION PROCESS; FUSED-SILICA CAPILLARIES; MACRO PORES; MACRO-POROSITY; MICROSCOPIC IMAGING; POLYMER-BASED MATERIALS; SAMPLE VOLUME; SEPARATION SCIENCE; SOFT MATTER; STATIONARY PHASE; STATIONARY PHASIS; STYRENE-DIVINYLBENZENE; VOID SPACE;

FUSED SILICA; MICROSCOPIC EXAMINATION; MONOLITHIC INTEGRATED CIRCUITS; MORPHOLOGY; POLYMERS; RESINS; SCANNING ELECTRON MICROSCOPY; STYRENE;

FILLED POLYMERS;

EID: 84870923811     PISSN: 07437463     EISSN: 15205827     Source Type: Journal    
DOI: 10.1021/la3038395     Document Type: Article

References (31)

1. Guiochon, G. Monolithic columns in high-performance liquid chromatography J. Chromatogr., A 2007, 1168, 101-168
2. Moulijn, J. A.; Kreutzer, M. T.; Nijhuis, T. A.; Kapteijn, F. Monolithic catalysts and reactors: high precision with low energy consumption Adv. Catal. 2011, 54, 249-327
3. Anderson, E. B.; Buchmeiser, M. R. Catalysts immobilized on organic polymeric monolithic supports: from molecular heterogeneous catalysis to biocatalysis ChemCatChem 2012, 4, 30-44
4. Tariq, F.; Lee, P. D.; Haswell, R.; McComb, D. W. The influence of nanoscale microstructural variations on the pellet scale flow properties of hierarchical porous catalytic structures using multiscale 3D imaging Chem. Eng. Sci. 2011, 66, 5804-5812
5. Gostovic, D.; Vito, N. J.; O'Hara, K. A.; Jones, K. S.; Wachsman, E. D. Microstructure and connectivity quantification of complex composite solid oxide fuel cell electrode three-dimensional networks J. Am. Ceram. Soc. 2011, 94, 620-627
6. Sahimi, M. Flow and Transport in Porous Media and Fractured Rock: From Classical Methods to Modern Approaches; VCH: Weinheim, Germany, 1995.
7. Sederman, A. J.; Alexander, P.; Gladden, L. F. Structure of packed beds probed by magnetic resonance imaging Powder Technol. 2001, 117, 255-269
8. Jinnai, H.; Nakanishi, K.; Nishikawa, Y.; Yamanaka, J.; Hashimoto, T. Three-dimensional structure of a sintered macroporous silica gel Langmuir 2001, 17, 619-625
9. Yao, Y.; Czymmek, K. J.; Pazhianur, R.; Lenhoff, A. M. Three-dimensional pore structure of chromatographic adsorbents from electron tomography Langmuir 2006, 22, 11148-11157
10. Dong, H.; Blunt, M. J. Pore-network extraction from micro-computerized- tomography images Phys. Rev. E 2009, 80, 036307
11. Bruns, S.; Müllner, T.; Kollmann, M.; Schachtner, J.; Höltzel, A.; Tallarek, U. Confocal laser scanning microscopy method for quantitative characterization of silica monolith morphology Anal. Chem. 2010, 82, 6569-6575
12. Koku, H.; Maier, R. S.; Czymmek, K. J.; Schure, M. R.; Lenhoff, A. M. Modeling of flow in a polymeric chromatographic monolith J. Chromatogr., A 2011, 1218, 3466-3475
13. Koku, H.; Maier, R. S.; Schure, M. R.; Lenhoff, A. M. Modeling of dispersion in a polymeric chromatographic monolith J. Chromatogr., A 2012, 1237, 55-63
14. Leighton, S. B. SEM images of block faces, cut by a miniature microtome within the SEM: a technical note Scan. Electron Microsc. 1981, 2, 73-76
15. Denk, W.; Horstmann, H. Serial block-face scanning electron microscopy to reconstruct three-dimensional tissue nanostructure PLoS Biol. 2004, 2, e329
16. Svec, F.; Germain, J.; Fréchet, J. M. J. Nanoporous polymers for hydrogen storage Small 2009, 5, 1098-1111
17. Urban, J.; Svec, F.; Fréchet, J. M. J. Hypercrosslinking: new approach to porous polymer monolithic capillary columns with large surface area for the highly efficient separation of small molecules J. Chromatogr., A 2010, 1217, 8212-8221
18. Zankel, A.; Kraus, B.; Poelt, P.; Schaffer, M.; Ingolic, E. Ultramicrotomy in the ESEM, a versatile method for materials and life sciences J. Microsc. 2009, 233, 140-148
19. Courtois, J.; Szumski, M.; Georgsson, F.; Irgum, K. Assessing the macroporous structure of monolithic columns by transmission electron microscopy Anal. Chem. 2007, 79, 335-344
20. Torquato, S. Random Heterogeneous Materials: Microstructure and Macroscopic Properties; Springer: New York, 2002.
21. Nguyen, A. M.; Dinh, N. P.; Cam, Q. M.; Sparrman, T.; Irgum, K. Preparation and characterization of sizable macroporous epoxy resin-based monolithic supports for flow-through systems J. Sep. Sci. 2009, 32, 2608-2618
22. Nischang, I.; Teasdale, I.; Brüggemann, O. Porous polymer monoliths for small molecule separations: advancements and limitations Anal. Bioanal. Chem. 2011, 400, 2289-2304
23. Aggarwal, P.; Tolley, H. D.; Lee, M. L. Monolithic bed structure for capillary liquid chromatography J. Chromatogr., A 2012, 1219, 1-14
24. Diamond, S. Mercury porosimetry: an inappropriate method for the measurement of pore size distributions in cement-based materials Cem. Concr. Res. 2000, 30, 1517-1525
25. Aoki, H.; Kubo, T.; Ikegami, T.; Tanaka, N.; Hosoya, K.; Tokuda, D.; Ishizuka, N. Preparation of glycerol dimethacrylate-based polymer monolith with unusual porous properties achieved via viscoelastic phase separation induced by monodisperse ultrahigh molecular weight poly(styrene) as a porogen J. Chromatogr., A 2006, 1119, 66-79
26. Vlakh, E. G.; Tennikova, T. B. Preparation of methacrylate monoliths J. Sep. Sci. 2007, 30, 2801-2813
27. Urban, J.; Jandera, P. Polymethacrylate monolithic columns for capillary liquid chromatography J. Sep. Sci. 2008, 31, 2521-2540
28. Hlushkou, D.; Bruns, S.; Seidel-Morgenstern, A.; Tallarek, U. Morphology-transport relationships for silica monoliths: from physical reconstruction to pore-scale simulations J. Sep. Sci. 2011, 34, 2026-2037
29. Bruns, S.; Hara, T.; Smarsly, B. M.; Tallarek, U. Morphological analysis of physically reconstructed capillary hybrid silica monoliths and correlation with separation efficiency J. Chromatogr., A 2011, 1218, 5187-5194
30. Viklund, C.; Svec, F.; Fréchet, J. M. J.; Irgum, K. Monolithic, "molded", porous materials with high flow characteristics for separations, catalysis, or solid-phase chemistry: control of porous properties during polymerization Chem. Mater. 1996, 8, 744-750
31. Nischang, I.; Svec, F.; Fréchet, J. M. J. Downscaling limits and confinement effects in the miniaturization of porous polymer monoliths in narrow bore capillaries Anal. Chem. 2009, 81, 7390-7396