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2 H QUOSY 2D-NMR Experiments in Weakly Aligning Systems: From the Conventional to the Ultrafast Approach.
ChemPhysChem ( IF 2.3 ) Pub Date : 2020-07-07 , DOI: 10.1002/cphc.202000336
Boris Gouilleux 1 , Abdelkrim Meddour 1 , Philippe Lesot 1
Affiliation  

We describe three anisotropic ultrafast (UF) QUadrupolar Ordered SpectroscopY (QUOSY) 2D‐NMR experiments (referred to as ADUF 2D NMR spectroscopy) designed for recording the 2H homonuclear 2D spectra of weakly aligned (deuterated) solutes in sub‐second experiment times. These new ADUF 2D experiments derive from the Q‐COSY, Q‐resolved and Q‐DQ 2D pulse sequences (J. Am. Chem. Soc. 1999, 121, 5249) and allow the correlation between the two components of each quadrupolar doublet, and then their assignment on the basis of 2H chemical shifts. The UF 2D pulse sequences are analyzed by using the Cartesian spin‐operator formalism for spin I=1 nuclei with a small quadrupolar moment. The optimal experimental/practical conditions as well as the resolution, sensitivity and quantification issues of these ADUF 2D experiments are discussed on comparison to their conventional 2D counterparts and their analytical potentialities. Illustrative ADUF 2D experiments using deuterated achiral/prochiral/chiral solutes in poly‐γ‐benzyl‐L‐glutamate based chiral liquid crystals are presented, as well as the first examples of natural abundance deuterium (ANADUF) 2D spectrum using 14.1 T magnetic field and a basic gradient unit (53 G.cm−1) in oriented solvents.

中文翻译:

弱对准系统中的2 H QUOSY 2D-NMR实验:从传统方法到超快方法。

我们描述了三个各向异性超快(UF)四极有序光谱学(QUOSY)2D-NMR实验(称为ADUF 2D NMR光谱学),旨在记录亚秒级实验中弱排列(氘化)的溶质的2 H同核2D光谱。这些新的ADUF二维实验从导出Q -COSY,Q分辨和Q -DQ 2D脉冲序列(J.化学会会志1999121,5249),并允许每个四极双合的两个分量之间的相关性,然后根据2 H化学位移进行分配 UF 2D脉冲序列通过使用笛卡尔自旋算符形式化进行自旋分析I = 1具有小四极矩的核。这些ADUF 2D实验的最佳实验/实践条件以及分辨率,灵敏度和定量问题,通过与常规2D对应物的比较和分析潜力进行了讨论。介绍了使用基于聚γ-苄基-L-谷氨酸的手性液晶中的氘代非手性/手性/手性溶质进行的ADUF 2D实验,以及使用14.1 T磁场和14.1 T磁场的自然丰度氘(ANADUF)2D光谱的第一个示例定向溶剂中的基本梯度单位(53 G.cm -1)。
更新日期:2020-07-07
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