Improvements in Resolution of ¹H NMR of solids.

IF 0.6 1区 历史学 0 ARCHAEOLOGY JOURNAL OF NEAR EASTERN STUDIES Pub Date : 2023-04-26 DOI:10.2533/chimia.2023.212
Bruno Simões de Almeida, Lyndon Emsley
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Abstract

Magic angle spinning (MAS) in 1H NMR has allowed progress from featureless spectra in static samples to linewidths of a few hundreds of Hertz for powdered solids at the fastest spinning rates available today (100-150 kHz). While this is a remarkable improvement, this level of resolution is still limiting to the widespread use of 1H NMR for complex systems. This review will discuss two recent alternative strategies that have significantly improved 1H resolution, when combined with fast MAS. The first is based on anti-z-COSY, a 2D experiment originally used for J decoupling in liquids, which removes residual broadening due to splittings caused by imperfect coherent averaging of MAS. The second strategy is to obtain pure isotropic proton (PIP) spectra in solids, by parametrically mapping any residual broadening due to imperfect averaging into a second dimension of a multidimensional correlation spectrum.

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固体¹H NMR分辨率的改进。
1H NMR中的魔角旋转(MAS)使静态样品的无特征光谱在目前可用的最快旋转速率(100-150 kHz)下,发展到粉末固体的几百赫兹线宽。虽然这是一个显着的改进,但这种分辨率水平仍然限制了1H NMR在复杂系统中的广泛使用。这篇综述将讨论两种最近的替代策略,当与快速MAS结合时,它们显著提高了1H分辨率。第一个是基于反z- cosy,这是一种最初用于液体中J去耦的二维实验,它消除了由于MAS的不完全相干平均引起的分裂而产生的剩余展宽。第二种策略是在固体中获得纯各向同性质子(PIP)光谱,通过参数化映射任何由于不完全平均而导致的剩余展宽到多维相关光谱的第二维。
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来源期刊
CiteScore
1.20
自引率
0.00%
发文量
55
期刊介绍: Devoted to an examination of the civilizations of the Near East, the Journal of Near Eastern Studies has for 125 years published contributions from scholars of international reputation on the archaeology, art, history, languages, literatures, and religions of the Near East. Founded in 1884 as Hebraica, the journal was renamed twice over the course of the following century, each name change reflecting the growth and expansion of the fields covered by the publication. In 1895 it became the American Journal of Semitic Languages and Literatures, and in 1942 it received its present designation, the Journal of Near Eastern Studies. From an original emphasis on Old Testament studies in the nineteenth century.
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