旋转固体中化学等效核的一维核磁共振交换实验

V. Gérardy-Montouillout , C. Malveau , P. Tekely , Z. Olender , Z. Luz
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引用次数: 66

摘要

提出了一种新的一维核磁共振交换实验,在旋转固体的慢动作状态下,化学等效核表现出四极耦合或化学位移各向异性。它由通常用于二维交换光谱的三脉冲序列组成,P1-t1-P2 - τm - p3 - t采集,但演化时间固定为半旋转周期,t1= TR/2,混合时间等于其整数倍,τm= GTR。与各种自旋侧带相关的磁极化在混合时间开始时在交替方向上极化。在τm期间的动态过程重新分配极化,导致在检测时间t期间修改边带模式。给出了碳-13和氘在二甲基砜中发生分子重定向的实验结果。结果与考虑定向和纵向松弛影响的模拟结果进行了比较。
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ODESSA, a New 1D NMR Exchange Experiment for Chemically Equivalent Nuclei in Rotating Solids

A new 1D NMR exchange experiment in the slow-motion regime of spinning solids, with chemically equivalent nuclei exhibiting quadrupole coupling or chemical-shift anisotropy, is proposed. It consists of the usual three-pulse sequence for 2D exchange spectroscopy,P1—t1P2—τmP3—t—acquisition, but with the evolution time fixed at one-half a spinning period,t1= TR/2, and a mixing time equal to an integer multiple thereof, τm= GTR. The magnetic polarizations associated with the various spinning sidebands are then polarized in alternate directions at the beginning of the mixing time. Dynamic processes during τmredistribute the polarizations, resulting in modified sideband patterns during the detection time,t. Experimental results are presented for carbon-13 and deuterium in dimethyl sulfone, which undergoes molecular reorientation in the solid state. The results are compared with simulations which include the effect of reorientation and longitudinal relaxation.

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