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自旋9/2四极核一维固态核磁共振谱中的分辨率增强

Resolution enhancement in 1D solid-state NMR spectra of spin-9/2 quadrupolar nuclei.

作者信息

Amoureux Jean-Paul, Trébosc Julien

机构信息

UCCS, CNRS-8181, University of Lille-1, C7-ENSCL, 59652 Villeneuve d'Ascq, France.

出版信息

J Magn Reson. 2006 Jun;180(2):311-6. doi: 10.1016/j.jmr.2006.02.018. Epub 2006 Mar 22.

DOI:10.1016/j.jmr.2006.02.018
PMID:16554179
Abstract

NMR is an insensitive spectroscopy, which often requires numerous accumulations, especially for 2D high-resolution methods (MQMAS and STMAS) for quadrupolar nuclei in solids. This may be a very important limitation for the case of insensitive nuclei, where a 1D spectrum with better resolution than the central-transition is then highly desirable. This problem has been addressed for the case of spin-5/2 nuclei by the Double-Quantum Filtered Satellite Transition Spectroscopy: DQF-SATRAS-ST(1). We extend this concept to the spin-9/2 nuclei with the SATRAS-ST(2) method. This method allows the observation of 1D spectra with a much better resolution than that observed in the isotropic projection of 2D MQ/ST(1)-MAS spectra. This enhanced resolution results from the much smaller homogeneous broadening that occurs on the SATRAS-ST(2) method as compared to MQ/ST(1)-MAS spectra. The main interest in this method is for well-crystallized samples.

摘要

核磁共振(NMR)是一种灵敏度较低的光谱技术,通常需要进行多次累加,对于固体中四极核的二维高分辨率方法(MQMAS和STMAS)而言尤其如此。对于灵敏度较低的核来说,这可能是一个非常重要的限制,在这种情况下,人们非常希望获得分辨率比中心跃迁更好的一维谱。对于自旋5/2核的情况,通过双量子滤波卫星跃迁光谱法(DQF-SATRAS-ST(1))解决了这个问题。我们通过SATRAS-ST(2)方法将这一概念扩展到自旋9/2核。该方法能够观测到分辨率比二维MQ/ST(1)-MAS谱的各向同性投影更好的一维谱。与MQ/ST(1)-MAS谱相比,SATRAS-ST(2)方法产生的均匀展宽要小得多,从而带来了这种更高的分辨率。这种方法的主要优势在于适用于结晶良好的样品。

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