Lynch, B,Muller, GH,Healy, LO,Glennon, JD,Pursch, M,Albert, K;

2003

January

Analytical and Bioanalytical Chemistry

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

Validated

()

solid-state NMR spectroscopy liquid chromatography preparation of bonded silica phases hydrosilation on hydride silica LIQUID-CHROMATOGRAPHY CROSS-POLARIZATION MONO-OL SPECTROSCOPY INTERMEDIATE BUTYLPHENYL SI-29

377

1014

1019

Si-29 and C-13 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 (M-H) 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.

DOI 10.1007/s00216-003-2198-1