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化学修饰硅胶的1H MAS NMR光谱法:一种表征色谱固定相界面的快速方法。

1H MAS NMR spectroscopy of chemically modified silica gels: a fast method to characterize stationary interphases for chromatography.

作者信息

Brindle R, Pursch M, Albert K

机构信息

Institut für Organische Chemie, Universität Tubingen, Germany.

出版信息

Solid State Nucl Magn Reson. 1996 Jun;6(3):251-66. doi: 10.1016/0926-2040(96)01227-1.

Abstract

Chemically modified silica gels used as stationary phases in chromatography have been investigated by means of solid-state 1H magic angle spinning (MAS) NMR spectroscopy. Since the organosilanes are bonded to the surface of the silica gel, their protons are diluted and possess a higher mobility in comparison to protons in pure organic solids. Thereby the usually strong homonuclear dipole-dipole interactions among the protons are reduced and it is possible to obtain well-resolved 1H NMR spectra of the organic interphases with MAS-only techniques. Effects of temperature and magnetic field strength on the resolution of the spectra are examined as well as the dependence of T1 and T1pH relaxation times on temperature and spinning speed.

摘要

已通过固态¹H魔角旋转(MAS)核磁共振光谱法对用作色谱固定相的化学改性硅胶进行了研究。由于有机硅烷键合在硅胶表面,其质子被稀释,与纯有机固体中的质子相比具有更高的迁移率。因此,质子之间通常很强的同核偶极-偶极相互作用被减弱,仅用MAS技术就有可能获得有机界面分辨良好的¹H NMR光谱。研究了温度和磁场强度对光谱分辨率的影响,以及T1和T1pH弛豫时间对温度和旋转速度的依赖性。

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