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样品旋转引起的场调制效应:在高分辨率魔角旋转核磁共振中的应用

Field modulation effects induced by sample spinning: application to high-resolution magic angle spinning NMR.

作者信息

Elbayed Karim, Dillmann Baudouin, Raya Jésus, Piotto Martial, Engelke Frank

机构信息

Institut de Chimie, FRE 2446, Université Louis Pasteur, Strasbourg, France.

出版信息

J Magn Reson. 2005 May;174(1):2-26. doi: 10.1016/j.jmr.2004.11.017.

Abstract

High-resolution magic angle spinning (HRMAS) has become an extremely versatile tool to study heterogeneous systems. HRMAS relies on magic angle spinning of the sample and on pulse sequences originally developed for liquid state NMR. In most cases the outcome of the experiment is conform to what is expected from high-resolution liquid state NMR spectroscopy. However in some instances, experiments run under MAS can produce some very puzzling results. After reviewing the basic hardware which is at the heart of HRMAS spectroscopy, we show that the origin of this behavior lies in the natural time-dependence of some physical quantities imparted by the rotation. We focus in particular on the effects of B1 inhomogeneities on the nutation, the (90 degrees)+x-t-(90 degrees )-x and the MLEV16 experiments. Different models of radiofrequency distribution of B1 fields in a solenoidal coil are derived from simple geometrical considerations. These models are shown by NMR spin dynamics calculations to reproduce the experimental NMR results. They are also consistent with electromagnetic simulations of the B1 field distribution inside a solenoidal coil.

摘要

高分辨率魔角旋转(HRMAS)已成为研究异质系统的一种极其通用的工具。HRMAS依赖于样品的魔角旋转以及最初为液态核磁共振开发的脉冲序列。在大多数情况下,实验结果与高分辨率液态核磁共振光谱所预期的结果相符。然而,在某些情况下,在魔角旋转(MAS)下进行的实验可能会产生一些非常令人困惑的结果。在回顾了HRMAS光谱核心的基本硬件之后,我们表明这种行为的根源在于旋转赋予的一些物理量的自然时间依赖性。我们特别关注B1不均匀性对章动、(90度)+x - t -(90度)- x以及MLEV16实验的影响。从简单的几何考虑推导出了螺线管线圈中B1场的不同射频分布模型。通过核磁共振自旋动力学计算表明,这些模型能够重现实验核磁共振结果。它们也与螺线管线圈内部B1场分布的电磁模拟结果一致。

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