Separated quadrupole and shift interactions of 2H NMR spectra in paramagnetic solids by asymmetric pulse sequences

IF 1.8 3区化学 Q4 CHEMISTRY, PHYSICAL

Solid state nuclear magnetic resonance Pub Date : 2021-04-01 DOI:10.1016/j.ssnmr.2020.101709

Takahiro Iijima , Shinobu Ohki , Masataka Tansho

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引用次数: 2

Abstract

Separated pure-quadrupole (PQ) and -shift (PS) spectra of ²H nuclear magnetic resonance (NMR) of paramagnetic solids are obtained and correlated by simple pulse sequences that can acquire the full magnetization under ideal conditions. Two-dimensional NMR signals obtained using an asymmetric π-pulse-inserted quadrupole-echo (APIQE) sequence yielded separated spectra through the skew operation of an affine transform (AT) before a Fourier transform. Modified APIQE sequences that acquire whole echo signals were fabricated, and separated PQ and PS spectra were obtained by applying a combination of AT, such as rotation and skew operations, to the signal data. These methods were demonstrated for diamagnetic Zn(CD₃CO₂)₂⋅2H₂O and paramagnetic Nd(CD₃CO₂)₃⋅1.5H₂O. Further, the dynamics of the D₂O molecule and [Co(D₂O)₆]²⁺ ion in paramagnetic CoSiF₆⋅6D₂O was analyzed based on the temperature dependence of the separated spectra.

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非对称脉冲序列对顺磁固体中2H核磁共振谱分离四极和位移相互作用的研究

分离pure-quadrupole (PQ)和转移(PS)的2 h核磁共振光谱(NMR)顺得到固体和关联的简单的脉冲序列,可以获得理想的条件下充分磁化。利用非对称π-脉冲插入四极回波(APIQE)序列得到的二维核磁共振信号，在进行傅里叶变换前先进行仿射变换(AT)的偏置运算，得到分离谱。制备了获取完整回波信号的改进APIQE序列，并对信号数据进行旋转和倾斜等AT组合处理，得到分离的PQ和PS谱。这些方法分别对抗磁性Zn(CD3CO2)2⋅2H2O和顺磁性Nd(CD3CO2)3⋅1.5H2O进行了验证。基于分离光谱的温度依赖性，分析了顺磁CoSiF6⋅6D2O中D2O分子和[Co(D2O)6]2+离子的动力学。

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来源期刊

Solid state nuclear magnetic resonance 物理-光谱学

CiteScore

5.30

自引率

9.40%

发文量

审稿时长

72 days

期刊介绍： The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.