Nuclear magnetic resonance analysis of silica gel surfaces modified with mixed, amine-containing ligands

  • Bruch M
  • Fatunmbi H
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Abstract

Different approaches for quantitative analysis by29Si and13C CP/MAS nuclear magnetic resonance (NMR) of silica gel chemically modified by a mixture of long and short chain amines, -(O)3Si(CH2)3N(CH3)2(CH2)13CH3and -(O)3Si(CH2)3N(CH3)3, are compared to elemental analysis. Unlike29Si NMR, variable contact time data are necessary for accurate quantitative analysis by13C NMR. Surprisingly, spectral overlap does not interfere with this approach. Surfaces prepared from reaction mixtures that consisted of 67 and 33% (v/v) long chain are found to actually contain 37 and 16% long chain amines, respectively. The mixed phase surfaces have more extensive cross-linking and fewer unreacted hydroxyls than single phase surfaces. © 2003 Elsevier B.V. All rights reserved.

Author-supplied keywords

  • Amine ligands
  • Cross polarization-magic-angle spinning
  • Cross-linking
  • Nuclear magnetic resonance spectroscopy
  • Silica
  • Stationary phases, LC

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Authors

  • Martha D. Bruch

  • Hafeez O. Fatunmbi

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