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Analytical and Bioanalytical Chemistry

, Volume 377, Issue 6, pp 1014–1019 | Cite as

Analysis of silica hydride and surface hydrosilation reactions by solid-state NMR in the preparation of p-chlorobenzamide bonded silica phase

  • B. Lynch
  • G. H. Müller
  • L. O. Healy
  • J. D. Glennon
  • M. Pursch
  • K. Albert
Original Paper

Abstract

29Si and 13C CP-MAS NMR spectroscopy was used to follow the conversion of native silica to a p-chlorobenzamide bonded silica material. The benzamide bonded phase was prepared via a hydrosilation reaction of a hydride silica intermediate with p-chloro-N-allylbenzamide. Solid-state NMR was used to show the disappearance of reactive surface hydride species (MH) and to identify newly formed bonded chemical species on the silica surface. DRIFT spectroscopy, elemental analysis, and specific surface-area determinations (BET) of the prepared phases are also reported.

Keywords

Solid-state NMR spectroscopy Liquid chromatography Preparation of bonded silica phases Hydrosilation on hydride silica 

Notes

Acknowledgements

All the specific surface-area measurements were carried out at Mitsui Denman Limited, Little Island, Cork, Ireland.

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Copyright information

© Springer-Verlag 2003

Authors and Affiliations

  • B. Lynch
    • 1
  • G. H. Müller
    • 1
  • L. O. Healy
    • 1
  • J. D. Glennon
    • 1
  • M. Pursch
    • 2
  • K. Albert
    • 2
  1. 1.Department of Chemistry, Analytical and Biological Chemistry Research FacilityUniversity College CorkCorkIreland
  2. 2.Institut fur Organische ChemieUniversität TübingenTübingenGermany

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