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在魔角旋转条件下采用同核偶极去耦方案的质子高分辨率固态核磁共振光谱学。

High-resolution solid-state NMR spectroscopy of protons with homonuclear dipolar decoupling schemes under magic-angle spinning.

作者信息

Madhu P K

机构信息

Department of Chemical Sciences, Tata Institute of Fundamental Research, Homi Bhabha Road, Colaba, Mumbai 400 005, India.

出版信息

Solid State Nucl Magn Reson. 2009 Feb;35(1):2-11. doi: 10.1016/j.ssnmr.2008.11.001. Epub 2008 Nov 25.

DOI:10.1016/j.ssnmr.2008.11.001
PMID:19110404
Abstract

High-resolution NMR spectroscopy of (1)H spins in the solid state is normally rendered difficult due to the strong homonuclear (1)H-(1)H dipolar couplings. Even under very high-speed magic-angle spinning (MAS) at ca. 60-70kHz, these couplings are not completely removed. An appropriate radiofrequency pulse scheme is required to average out the homonuclear dipolar interactions in combination with MAS to get high-resolution (1)H NMR spectrum in solid state. Several schemes have been introduced in the recent past with a variety of applications also envisaged. Development of some of these schemes has been made possible with a clear understanding of the underlying spin physics based on bimodal Floquet theory. The utility of these high-resolution pulse schemes in combination with MAS has been demonstrated for spinning speeds of 10-65kHz in a range of (1)H Larmor frequencies from 300 to 800MHz.

摘要

由于固态中氢核(¹H)自旋之间存在强烈的同核¹H-¹H偶极耦合,¹H自旋的高分辨率核磁共振光谱通常难以实现。即使在约60 - 70kHz的超高速魔角旋转(MAS)条件下,这些耦合也不能完全消除。需要一种合适的射频脉冲序列,结合MAS来平均同核偶极相互作用,从而获得固态¹H核磁共振高分辨率谱。最近已经引入了几种序列,并且还设想了各种应用。基于双峰弗洛凯理论,对潜在的自旋物理有清晰的理解,使得其中一些序列的开发成为可能。这些高分辨率脉冲序列与MAS结合的效用,已在10 - 65kHz的旋转速度以及300至800MHz范围内的一系列¹H拉莫尔频率下得到了证明。

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