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Rationalising heteronuclear decoupling in refocussing applications of solid-state NMR.

机译:在固态NMR重新聚焦应用中合理化异核去耦。

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摘要

Factors affecting the performance of 1H heteronuclear decoupling sequences for magic-angle spinning (MAS) NMR spectroscopy of organic solids are explored, as observed by time constants for the decay of nuclear magnetisation under a spin-echo (math formula ). By using a common protocol over a wide range of experimental conditions, including very high magnetic fields and very high radio-frequency (RF) nutation rates, decoupling performance is observed to degrade consistently with increasing magnetic field. Inhomogeneity of the RF field is found to have a significant impact on math formula values, with differences of about 20 % observed between probes with different coil geometries. Increasing RF nutation rates dramatically improve robustness with respect to RF offset, but the performance of phase-modulated sequences degrades at the very high nutation rates achievable in microcoils as a result of RF transients. The insights gained provide better understanding of the factors limiting decoupling performance under different conditions, and the high values of math formula observed (which generally exceed previous literature values) provide reference points for experiments involving spin magnetisation refocussing, such as 2D correlation spectra and measuring small spin couplings.
机译:通过在自旋回波下(数学公式)通过时间常数观察到的核磁衰变的时间常数,探索了影响有机固体的1H异核去耦序列性能的因素,用于魔角旋转(MAS)NMR光谱学。通过在广泛的实验条件下使用通用协议,包括非常高的磁场和非常高的射频(RF)章动速率,可以观察到去耦性能会随着磁场的增加而持续下降。发现射频场的不均匀性对数学公式值有重大影响,在具有不同线圈几何形状的探头之间观察到约20%的差异。增大RF章动率可以显着提高RF偏移的鲁棒性,但是由于RF瞬变,在微线圈中可以达到的很高章动率下,相位调制序列的性能会降低。所获得的见解可以更好地理解在不同条件下限制去耦性能的因素,并且观察到的高数学公式值(通常超过先前的文献值)为涉及自旋磁化重新聚焦的实验提供了参考点,例如二维相关光谱和测量小自旋联轴器。

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