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Artefact-free broadband 2D NMR for separation of quadrupolar and paramagnetic shift interactions.
Solid State Nuclear Magnetic Resonance ( IF 1.8 ) Pub Date : 2019-05-09 , DOI: 10.1016/j.ssnmr.2019.05.001
Rihards Aleksis 1 , José P Carvalho 1 , Aleksander Jaworski 1 , Andrew J Pell 1
Affiliation  

Two new two-dimensional, broadband, solid-state NMR experiments for separating and correlating the quadrupolar and shift interactions of spin I=1 nuclei in paramagnetic systems are proposed. The new pulse sequences incorporate the short, high-power adiabatic pulses (SHAPs) into the shifting d-echo experiment of Walder et al. [J. Chem. Phys., 142, 014201 (2015)], in two different ways, giving double and quadruple adiabatic shifting d-echo sequences. These new experiments have the advantage over previous methods of both suppressing spectral artefacts due to pulse imperfections, and exhibiting a broader excitation bandwidth. Both experiments are analysed with theoretical calculations and simulations, and are applied experimentally to the 2H NMR of deuterated CuCl2 ⋅2H2O, and two deuterated samples of the ion conductor oxyhydride BaTiO3−xHy prepared using two different methods. For the CuCl2 ⋅2H2O sample, both new methods obtain very high-quality spectra from which the parameters describing the shift and quadrupolar interaction tensors, and their relative orientation, were extracted. The two BaTiO3−xHy samples exhibited different local hydride environments with different tensor parameters. The 2H spectra of these oxyhydrides exhibit inhomogeneous broadening of the 2H shifts, and so whilst the quadrupolar interaction parameters were easily extracted, the measurement of the shift parameters was more complex. However, effective shift parameters were extracted, which combine the effects of both the paramagnetic shift tensor and the inhomogeneous broadening.



中文翻译:

无伪像的宽带2D NMR用于分离四极和顺磁位移相互作用。

两个新的二维,宽带,固态NMR实验,用于分离和关联自旋的四极和位移相互作用 一世=1个提出了顺磁系统中的原子核。新的脉冲序列将短的高功率绝热脉冲(SHAP)整合到Walder等人的d d回波实验中。[J. 化学 Phys。,142,014201(2015)],以两种不同方式给出了双重和四重绝热移位d回波序列。这些新的实验具有优于以前的方法的优点,既可以抑制由于脉冲缺陷引起的频谱伪影,又可以显示更宽的激励带宽。两个实验中,分析与理论计算和模拟,并且通过实验施加到2氘化的CuCl 1 H NMR 2 ⋅2H 2 O,和两个氘化oxyhydride的BaTiO离子导体样品3-X ħ ÿ使用两种不同的方法制备。为氯化亚铜2 ⋅2H 2 ö样品,这两种新的方法获得非常从该描述位移和四极相互作用张量,以及它们的相对取向的参数,提取高质量的光谱。两个BaTiO 3− x H y样品表现出具有不同张量参数的不同局部氢化物环境。这些氢氧化物的2 H光谱显示2的不均匀加宽H位移,因此尽管很容易提取四极相互作用参数,但位移参数的测量更为复杂。然而,提取了有效的位移参数,其结合了顺磁位移张量和不均匀展宽的效果。

更新日期:2019-05-09
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