Revealing the fine details of functionalized silica surfaces 2 by solid-state NMR and adsorption isotherm 3 measurements: the case of fluorinated stationary phases for 4 liquid chromatography (Articolo in rivista)

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  • Revealing the fine details of functionalized silica surfaces 2 by solid-state NMR and adsorption isotherm 3 measurements: the case of fluorinated stationary phases for 4 liquid chromatography (Articolo in rivista) (literal)
Anno
  • 2014-01-01T00:00:00+01:00 (literal)
Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#doi
  • 10.1002/chem.201304330 (literal)
Alternative label
  • A. Ciogli, P. Simone, C. Villani, F. Gasparrini, A. Lagana, D. Capitani, N. Marchetti, L. Pasti, A. Massi, A. Cavazzini (2014)
    Revealing the fine details of functionalized silica surfaces 2 by solid-state NMR and adsorption isotherm 3 measurements: the case of fluorinated stationary phases for 4 liquid chromatography
    in Chemistry - A European Journal; Wiley-VCH Verlag Gmbh, Weinheim (Germania)
    (literal)
Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#autori
  • A. Ciogli, P. Simone, C. Villani, F. Gasparrini, A. Lagana, D. Capitani, N. Marchetti, L. Pasti, A. Massi, A. Cavazzini (literal)
Pagina inizio
  • 8138 (literal)
Pagina fine
  • 8148 (literal)
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  • 20 (literal)
Rivista
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  • 11 (literal)
Note
  • Google Scholar (literal)
  • ISI Web of Science (WOS) (literal)
  • Scopus (literal)
Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#affiliazioni
  • Dipartimento di Chimica e Tecnologia del Farmaco University \"La Sapienza\", Piazzale Aldo Moro 5, 00185 Rome (Italy) University of Rome, \"La Sapienza\", Department of Chemistry Piazzale Aldo Moro 5, 00185 Rome (Italy) Istituto di Metodologie Chimiche CNR University of Ferrara Department of Chemistry and Pharmaceutical Sciences via L. Borsari, 46, 44121 Ferrara (Italy) (literal)
Titolo
  • Revealing the fine details of functionalized silica surfaces 2 by solid-state NMR and adsorption isotherm 3 measurements: the case of fluorinated stationary phases for 4 liquid chromatography (literal)
Abstract
  • The structural and chromatographic characterization of two novel fluorinated mesoporous materials prepared by covalent reaction of 3-(pentafluorophenyl)propyldimethylchlorosilane and perfluorohexylethyltrichlorosilane with 2.5 mm fully porous silica particles is reported. The adsorbents were characterized by solid state 29Si, 13C, and 19F NMR spectroscopy, low-temperature nitrogen adsorption, elemental analysis (C and F), and various chromatographic measurements, including the determination of adsorption isotherms. The structure and abundance of the different organic surface species, as well as the different silanol types, were determined. In particular, the degree of so-called horizontal polymerization, that is, Si-O-Si bridging parallel to the silica surface due to the reaction, under \"quasi-dry\" conditions of trifunctional silanizing agents with the silica surface was quantified. Significant agreement was found between the information provided by solid-state NMR, elemental analysis, and excess isotherms regarding the amount of surface residual silanol groups, on the one hand, and the degree of surface functionalization, on the other. Finally, the kinetic performance of the fluorinated materials as separation media for applications in near-ultrahigh-performance liquid chromatography was evaluated. At reduced velocities of about 5.5 (ca. 600 bar backpressure at room temperature) with 3 mm diameter columns and toluene as test compound, reduced plate heights on the order of 2 were obtained on columns of both adsorbents. (literal)
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