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首页> 外文期刊>The journal of physical chemistry, A. Molecules, spectroscopy, kinetics, environment, & general theory >Effects of Finite Rf Pulses and Sample Spinning Speed in Multiple-Quantum Magic-Angle Spinning (MQ-MAS) and Multiple-Quantum Quadrupolar Carr-Purcell-Meiboom-Gill Magic-Angle Spinning (MQ-QCPMG-MAS) Nuclear Magnetic Resonance of Half-Integer Quadrupo
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Effects of Finite Rf Pulses and Sample Spinning Speed in Multiple-Quantum Magic-Angle Spinning (MQ-MAS) and Multiple-Quantum Quadrupolar Carr-Purcell-Meiboom-Gill Magic-Angle Spinning (MQ-QCPMG-MAS) Nuclear Magnetic Resonance of Half-Integer Quadrupo

机译:有限Rf脉冲和样品旋转速度在多量子幻角自旋(MQ-MAS)和多量子四极Carr-Purcell-Meiboom-Gill幻角自旋(MQ-QCPMG-MAS)核磁共振中的影响-整数Quadrupo

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摘要

The multiple-quantum magic-angle spinning (MQ-MAS) solid-state nuclear magnetic resonance (NMR) experiment and a sensitivity-enhanced variant detecting the second-order quadrupolar powder pattern through a train of quadrupolar Carr-Purcell-Meiboom-Gill refocusing pulses (MQ-QCPMG-MAS) are analyzed with respect to the effects of finite radio frequency (rf) pulse irradiation and the MAS frequency. Taking these effects explicitly into account, it is possible to accurately determine optimum conditions for excitation of MQ coherences and reconversion of these into detectable single-quantum coherences as well as simulate the second-order quadrupolar lineshape necessary to extract accurate parameters for quadrupolar coupling interactions and isotropic chemical shifts. This accurate determination is of great importance for the exploitation of MQ-MAS and MQ-QCPMG-MAS NMR experiments for quantitative determination of site populations. The various effects are described analytically and demonstrated by numerical simulations and by ~(87)Rb MQ-MAS and MQ-QCPMG-MAS experiments on RbNO_3.
机译:多量子魔术角旋转(MQ-MAS)固态核磁共振(NMR)实验和灵敏度增强型变量,通过一系列四极Carr-Purcell-Meiboom-Gill重聚焦来检测二阶四极粉末图案针对有限射频(rf)脉冲辐照和MAS频率的影响分析了脉冲(MQ-QCPMG-MAS)。明确考虑到这些影响,可以准确确定激发MQ相干并将其重新转换为可检测的单量子相干的最佳条件,并模拟为提取四极耦合相互作用的准确参数所必需的二阶四极线形。各向同性的化学位移。这种准确的确定对于利用MQ-MAS和MQ-QCPMG-MAS NMR实验定量确定位点种群非常重要。分析地描述了各种影响,并通过数值模拟以及RbNO_3上的〜(87)Rb MQ-MAS和MQ-QCPMG-MAS实验进行了证明。

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