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Repetitive sideband-selective double frequency sweeps for sensitivity enhancement of MAS NMR of half-integer quadrupolar nuclei

机译:重复边带选择双频扫描,提高半整数四极核的MAS NMR的灵敏度

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摘要

A sensitivity enhancement scheme aiming at selective adiabatic inversion of a single set of satellite transition sidebands under magic angle spinning has been employed on samples of albite containing a single moderately distorted ~(27)Al site and zoisite containing two highly distorted octahedral ~(27)Al sites. Overall enhancements of ~2.5 for albite and ~3 for the two AlO _6 sites of zoisite are reported by applying this scheme at different spinning speeds reflecting the versatility of this enhancement scheme which achieves significant signal-to-noise enhancements for the systems with moderately high quadrupolar coupling and high quadrupolar coupling. Repeating the sensitivity enhancement scheme and signal readout several times without allowing for spin-lattice relaxation leads to sensitivity enhancements of factors of ~4 for albite and ~5 for zoisite which substantially increases the detectability of the quadrupolar sites. The effectiveness of this scheme at high magnetic field under very fast magic angle spinning has been demonstrated. Finally, the possibility of performing spectral editing by selective enhancement of one of the quadrupolar sites in zoisite whilst keeping the other site unaffected has been explored.
机译:针对在魔角旋转下对一组卫星过渡边带进行选择性绝热反演的灵敏度增强方案,已被用于包含单个畸变的〜(27)Al位点和含两个垂直畸变的八面体〜(27)的硅沸石的样品铝网站。据报道,通过在不同的纺丝速度下应用该方案,钠长石的整体增强程度为〜2.5,钠长石的〜2.5整体增强,两个AlO _6位点的整体增强能力为〜3,反映了该增强方案的多功能性,可为中等偏高的系统实现显着的信噪比增强四极耦合和高四极耦合。在不允许自旋晶格弛豫的情况下,重复进行几次灵敏度增强方案和信号读出操作,可使钠长石的灵敏度提高至〜4,对菱沸石的灵敏度提高至〜5,从而大大提高了四极位点的可检测性。已经证明了该方案在非常快的魔角旋转下在高磁场下的有效性。最终,探索了通过选择性增强黄铁矿中一个四极位点同时保持另一个位点不受影响来执行光谱编辑的可能性。

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