通过质子储层的逐渐饱和间接探测到卫星跃迁四极核磁共振

IF 1.8 3区 化学 Q4 CHEMISTRY, PHYSICAL Solid state nuclear magnetic resonance Pub Date : 2023-06-01 DOI:10.1016/j.ssnmr.2023.101862
Tamar Wolf , Anna Eden-Kossoy , Lucio Frydman
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引用次数: 1

摘要

来自半整数四极核的静态卫星跃迁(ST)NMR线形可能非常有用:它们可以提供关于宽时间尺度上局部运动的见解,并可以报告由四极参数变化反映的局部电子环境的微小变化。然而,由于半整数四极核的绝对宽度,卫星跃迁通常是“不可见的”,导致信噪比较低,尤其是对于不可接受的低伽马或稀释四极核。最近,我们介绍了一种提高静止固体中不可接收X核NMR灵敏度的方法,称为质子库的渐渗饱和(PROSPR),该方法通过在更灵敏的1H NMR信号上重复压印频率选择性X驱动的去极化,打开了放大此类自旋信号的可能性。在这里,我们表明PROSPR的功效足以检测35Cl、33S甚至17O等具有挑战性的物种的静态ST NMR——所有这些都处于自然丰度。因此,随后的ST-PROSPR NMR实验为探测超宽线(6-8 MHz宽)光谱开辟了新的途径。这些高度明显的各向异性反过来又可以提供关于固体动态变化的新视角,如这里通过跟踪热驱动事件期间作为温度函数的ST线形状所示。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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Indirectly detected satellite-transition quadrupolar NMR via progressive saturation of the proton reservoir

Static satellite-transitions (ST) NMR line shapes from half-integer quadrupolar nuclei could be very informative: they can deliver insight about local motions over a wide range of timescales, and can report on small changes in the local electronic environments as reflected by variations in the quadrupolar parameters. Satellite transitions, however, are typically “invisible” for half-integer quadrupolar nuclei due to their sheer breadth, leading to low signal-to-noise ratio –especially for unreceptive low-gamma or dilute quadrupolar nuclei. Very recently we have introduced a method for enhancing the NMR sensitivity of unreceptive X nuclei in static solids dubbed PROgressive Saturation of the Proton Reservoir (PROSPR), which opens the possibility of magnifying the signals from such spins by repeatedly imprinting frequency-selective X-driven depolarizations on the much more sensitive 1H NMR signal. Here, we show that PROSPR's efficacy is high enough for enabling the detection of static ST NMR for challenging species like 35Cl, 33S and even 17O –all at natural-abundance. The ensuing ST-PROSPR NMR experiment thus opens new approaches to probe ultra-wideline (6–8 MHz wide) spectra. These highly pronounced anisotropies can in turn deliver new vistas about dynamic changes in solids, as here illustrated by tracking ST line shapes as a function of temperature during thermally-driven events.

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来源期刊
CiteScore
5.30
自引率
9.40%
发文量
42
审稿时长
72 days
期刊介绍: The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.
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