Spectroscopic investigation of the hydrolysis of γ-glycidoxypropylsilane bound to silica surfaces

G. R. Bogart; D. E. Leyden; T. M. Wade; W. Schafer; P. W. Carr

doi:10.1016/S0021-9673(01)93123-1

Spectroscopic investigation of the hydrolysis of γ-glycidoxypropylsilane bound to silica surfaces

G. R. Bogart, D. E. Leyden, T. M. Wade, W. Schafer, P. W. Carr

Chemistry (Twin Cities)

Research output: Contribution to journal › Article › peer-review

29 Scopus citations

Abstract

Chemically modified silica gels were prepared under various conditions with γ-glycidoxypropyltrimethoxysilane in order to investigate the effect of various methods of hydrolyzing the terminal epoxide group. The silylated substrates were then examined by ¹³C solid-state NMR with cross-polarization and magic angle spinning. NMR results were correlated with infrared results obtained by diffuse reflectance Fourier transform infrared spectroscopy. By reaction with a primary alkyl amine the percentage of unopened epoxide may be determined by Fourier transform infrared spectroscopy. Infrared data indicate that as little as 10% epoxide remaining after attempted hydrolysis can influence chromatographic capacity factors.

Original language	English (US)
Pages (from-to)	209-219
Number of pages	11
Journal	Journal of Chromatography A
Volume	483
Issue number	C
DOIs	https://doi.org/10.1016/S0021-9673(01)93123-1
State	Published - 1989

Bibliographical note

Funding Information:
This researchw as supported in part by Research Grant CHE-87 12457f rom the National Science Foundation. T.M.W., W.S. and P.W.C. acknowledge the Center for Bioprocess Technology of the University of Minnesota. G.R.B. and D.E.L. acknowledge the Colorado State University NMR Center, funded by National Science

Funding Information:
Foundation Regional Instrumentation Center Grant CHE-8616437. The Nicolet 60SX FTIR spectrometer was purchased in part from a grant from the National Science Foundation (CHE-8317079).

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@article{2208781056354b37a0a9551f2d9ee04e,

title = "Spectroscopic investigation of the hydrolysis of γ-glycidoxypropylsilane bound to silica surfaces",

abstract = "Chemically modified silica gels were prepared under various conditions with γ-glycidoxypropyltrimethoxysilane in order to investigate the effect of various methods of hydrolyzing the terminal epoxide group. The silylated substrates were then examined by 13C solid-state NMR with cross-polarization and magic angle spinning. NMR results were correlated with infrared results obtained by diffuse reflectance Fourier transform infrared spectroscopy. By reaction with a primary alkyl amine the percentage of unopened epoxide may be determined by Fourier transform infrared spectroscopy. Infrared data indicate that as little as 10% epoxide remaining after attempted hydrolysis can influence chromatographic capacity factors.",

author = "Bogart, {G. R.} and Leyden, {D. E.} and Wade, {T. M.} and W. Schafer and Carr, {P. W.}",

note = "Funding Information: This researchw as supported in part by Research Grant CHE-87 12457f rom the National Science Foundation. T.M.W., W.S. and P.W.C. acknowledge the Center for Bioprocess Technology of the University of Minnesota. G.R.B. and D.E.L. acknowledge the Colorado State University NMR Center, funded by National Science Funding Information: Foundation Regional Instrumentation Center Grant CHE-8616437. The Nicolet 60SX FTIR spectrometer was purchased in part from a grant from the National Science Foundation (CHE-8317079).",

year = "1989",

doi = "10.1016/S0021-9673(01)93123-1",

language = "English (US)",

volume = "483",

pages = "209--219",

journal = "Journal of Chromatography A",

issn = "0021-9673",

number = "C",

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TY - JOUR

T1 - Spectroscopic investigation of the hydrolysis of γ-glycidoxypropylsilane bound to silica surfaces

AU - Bogart, G. R.

AU - Leyden, D. E.

AU - Wade, T. M.

AU - Schafer, W.

AU - Carr, P. W.

N1 - Funding Information: This researchw as supported in part by Research Grant CHE-87 12457f rom the National Science Foundation. T.M.W., W.S. and P.W.C. acknowledge the Center for Bioprocess Technology of the University of Minnesota. G.R.B. and D.E.L. acknowledge the Colorado State University NMR Center, funded by National Science Funding Information: Foundation Regional Instrumentation Center Grant CHE-8616437. The Nicolet 60SX FTIR spectrometer was purchased in part from a grant from the National Science Foundation (CHE-8317079).

PY - 1989

Y1 - 1989

N2 - Chemically modified silica gels were prepared under various conditions with γ-glycidoxypropyltrimethoxysilane in order to investigate the effect of various methods of hydrolyzing the terminal epoxide group. The silylated substrates were then examined by 13C solid-state NMR with cross-polarization and magic angle spinning. NMR results were correlated with infrared results obtained by diffuse reflectance Fourier transform infrared spectroscopy. By reaction with a primary alkyl amine the percentage of unopened epoxide may be determined by Fourier transform infrared spectroscopy. Infrared data indicate that as little as 10% epoxide remaining after attempted hydrolysis can influence chromatographic capacity factors.

AB - Chemically modified silica gels were prepared under various conditions with γ-glycidoxypropyltrimethoxysilane in order to investigate the effect of various methods of hydrolyzing the terminal epoxide group. The silylated substrates were then examined by 13C solid-state NMR with cross-polarization and magic angle spinning. NMR results were correlated with infrared results obtained by diffuse reflectance Fourier transform infrared spectroscopy. By reaction with a primary alkyl amine the percentage of unopened epoxide may be determined by Fourier transform infrared spectroscopy. Infrared data indicate that as little as 10% epoxide remaining after attempted hydrolysis can influence chromatographic capacity factors.

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U2 - 10.1016/S0021-9673(01)93123-1

DO - 10.1016/S0021-9673(01)93123-1

M3 - Article

AN - SCOPUS:0024847634

VL - 483

SP - 209

EP - 219

JO - Journal of Chromatography A

JF - Journal of Chromatography A

SN - 0021-9673

IS - C

ER -

Spectroscopic investigation of the hydrolysis of γ-glycidoxypropylsilane bound to silica surfaces

Abstract

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