29-Silicon NMR evidence for the improved chromatographic siloxane bond stability of bulky alkylsilane ligands on a silica surface

A.B. Scholten; J.W. Haan, de; H.A. Claessens; L.J.M. Ven, van de; C.A. Cramers

doi:10.1016/0021-9673(94)00928-7

29-Silicon NMR evidence for the improved chromatographic siloxane bond stability of bulky alkylsilane ligands on a silica surface

A.B. Scholten, J.W. Haan, de, H.A. Claessens, L.J.M. Ven, van de, C.A. Cramers

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Abstract

A stable bond stationary phase for reversed-phase HPLC, with a diisobutyl-n-octadecylsilane derivatized surface, was studied using 29Si CPMAS NMR. Fumed silica surfaces (Aerosil), trimethylsilylated to different extents, were used to illustrate the effect of ligand surface loading on the hydrogen bonding contribution to the ligand silane CPMAS NMR signal. Spectral comparison of the diisobutyl-n-octadecylsilane derivatized silica with the conventional dimethyl-n-octadecylsilane derivatized silica revealed significantly decreased hydrogen bonding of residual silanols to the ligand siloxane bond in the diisobutyl-n-octadecyl phase. This illustrates the increased steric protection of the ligand siloxane bond by the bulky alkyl substituents, which is assumed to be the reason for the improved hydrolytic stability at low pH of this phase

Original language	English
Pages (from-to)	25-29
Journal	Journal of Chromatography, A
Volume	688
Issue number	1-2
DOIs	https://doi.org/10.1016/0021-9673(94)00928-7
Publication status	Published - 1994

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title = "29-Silicon NMR evidence for the improved chromatographic siloxane bond stability of bulky alkylsilane ligands on a silica surface",

abstract = "A stable bond stationary phase for reversed-phase HPLC, with a diisobutyl-n-octadecylsilane derivatized surface, was studied using 29Si CPMAS NMR. Fumed silica surfaces (Aerosil), trimethylsilylated to different extents, were used to illustrate the effect of ligand surface loading on the hydrogen bonding contribution to the ligand silane CPMAS NMR signal. Spectral comparison of the diisobutyl-n-octadecylsilane derivatized silica with the conventional dimethyl-n-octadecylsilane derivatized silica revealed significantly decreased hydrogen bonding of residual silanols to the ligand siloxane bond in the diisobutyl-n-octadecyl phase. This illustrates the increased steric protection of the ligand siloxane bond by the bulky alkyl substituents, which is assumed to be the reason for the improved hydrolytic stability at low pH of this phase",

author = "A.B. Scholten and \{Haan, de\}, J.W. and H.A. Claessens and \{Ven, van de\}, L.J.M. and C.A. Cramers",

year = "1994",

doi = "10.1016/0021-9673(94)00928-7",

language = "English",

volume = "688",

pages = "25--29",

journal = "Journal of Chromatography, A",

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publisher = "Elsevier B.V.",

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TY - JOUR

T1 - 29-Silicon NMR evidence for the improved chromatographic siloxane bond stability of bulky alkylsilane ligands on a silica surface

AU - Scholten, A.B.

AU - Haan, de, J.W.

AU - Claessens, H.A.

AU - Ven, van de, L.J.M.

AU - Cramers, C.A.

PY - 1994

Y1 - 1994

N2 - A stable bond stationary phase for reversed-phase HPLC, with a diisobutyl-n-octadecylsilane derivatized surface, was studied using 29Si CPMAS NMR. Fumed silica surfaces (Aerosil), trimethylsilylated to different extents, were used to illustrate the effect of ligand surface loading on the hydrogen bonding contribution to the ligand silane CPMAS NMR signal. Spectral comparison of the diisobutyl-n-octadecylsilane derivatized silica with the conventional dimethyl-n-octadecylsilane derivatized silica revealed significantly decreased hydrogen bonding of residual silanols to the ligand siloxane bond in the diisobutyl-n-octadecyl phase. This illustrates the increased steric protection of the ligand siloxane bond by the bulky alkyl substituents, which is assumed to be the reason for the improved hydrolytic stability at low pH of this phase

AB - A stable bond stationary phase for reversed-phase HPLC, with a diisobutyl-n-octadecylsilane derivatized surface, was studied using 29Si CPMAS NMR. Fumed silica surfaces (Aerosil), trimethylsilylated to different extents, were used to illustrate the effect of ligand surface loading on the hydrogen bonding contribution to the ligand silane CPMAS NMR signal. Spectral comparison of the diisobutyl-n-octadecylsilane derivatized silica with the conventional dimethyl-n-octadecylsilane derivatized silica revealed significantly decreased hydrogen bonding of residual silanols to the ligand siloxane bond in the diisobutyl-n-octadecyl phase. This illustrates the increased steric protection of the ligand siloxane bond by the bulky alkyl substituents, which is assumed to be the reason for the improved hydrolytic stability at low pH of this phase

U2 - 10.1016/0021-9673(94)00928-7

DO - 10.1016/0021-9673(94)00928-7

M3 - Article

SN - 0021-9673

VL - 688

SP - 25

EP - 29

JO - Journal of Chromatography, A

JF - Journal of Chromatography, A

IS - 1-2

ER -

29-Silicon NMR evidence for the improved chromatographic siloxane bond stability of bulky alkylsilane ligands on a silica surface

Abstract

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