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Investigating FAM-N pulses for signal enhancement in MQMAS NMR of quadrupolar nuclei

机译:研究FAM-N脉冲以增强四极核的MQMAS NMR中的信号

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摘要

Although a popular choice for obtaining high-resolution solid-state NMR spectra of quadrupolar nuclei, the inherently low sensitivity of the multiple-quantum magic-angle spinning (MQMAS) experiment has limited its application for nuclei with low receptivity or when the available sample volume is limited. A number of methods have been introduced in the literature to attempt to address this problem. Recently, we have introduced an alternative, automated approach, based on numerical simulations, for generating amplitude-modulated pulses (termed FAM-N pulses) to enhance the efficiency of the triple- to single-quantum conversion step within MQMAS. This results in efficient pulses that can be used without experimental reoptimisation, ensuring that this method is particularly suitable for challenging nuclei and systems. In this work, we investigate the applicability of FAM-N pulses to a wider variety of systems, and their robustness under more challenging experimental conditions. These include experiments performed under fast MAS, nuclei with higher spin quantum numbers, samples with multiple distinct sites, low-γ nuclei and nuclei subject to large quadrupolar interactions.
机译:尽管获得四极核的高分辨率固态NMR光谱的普遍选择,但多量子魔术角旋转(MQMAS)实验固有的低灵敏度,限制了其在具有低接受性或可用样品量的核中的应用。是有限的。文献中已经引入了许多方法来尝试解决这个问题。最近,我们基于数值模拟引入了另一种自动化方法,用于生成调幅脉冲(称为FAM-N脉冲),以增强MQMAS中三重到单量子转换步骤的效率。这样可产生无需进行实验重新优化即可使用的高效脉冲,从而确保该方法特别适用于具有挑战性的原子核和系统。在这项工作中,我们调查了FAM-N脉冲在各种系统中的适用性,以及在更具挑战性的实验条件下的鲁棒性。这些包括在快速MAS,具有更高自旋量子数的核,具有多个不同位点的样品,低γ核和经受大四极相互作用的核下进行的实验。

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