用于空间选择性电化学核磁共振光谱的平行线探针

IF 2 3区 化学 Q3 BIOCHEMICAL RESEARCH METHODS
Ruipeng Luo, Hans J.W.G. Janssen, Arno P.M. Kentgens, Evan Wenbo Zhao
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引用次数: 0

摘要

原位核磁共振是研究氧化还原液流电池和电催化反应器等电化学装置的重要工具,能够检测反应中间体、蜕变态、过程的时间演化或监测稳定性与电化学条件的函数关系。在此,我们报告了一种用于空间选择性原位电化学核磁共振光谱的平行线探测器。该检测器由 17 根铜线组成,可对 1H/19F 和 X 核进行双重调谐,频率范围从 63Cu (106.1 MHz) 到 7Li (155.5 MHz)。平行线探测器的扁平几何形状允许将其插入高电极表面体积比的电化学流动反应器中,从而实现了探测器在反应器中的设计。这种集成装置被命名为 "eReactor NMR 探针"。结合 B1 选择性脉冲序列,实现了对电极-电解质界面(距离电极表面 800 μm 范围内)原子核的选择性探测。使用两种电解质(LiCl 和 LiBF4 溶液)分别对 7Li 和 19F 核进行了选择性检测。实现了良好的 B1 一致性,810° 到 90°脉冲强度比为 68-72%。我们以金属锂的电化学电镀为模型反应,进一步证明了该探针的操作功能。新的 eReactor NMR 探针为研究流动电化学提供了一种通用方法,我们设想将其广泛应用于与环境相关的能源系统,例如金属锂电池、电化学氨合成、二氧化碳捕获和还原、氧化还原流动电池、燃料电池、海水淡化、木质素氧化等。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

A parallel line probe for spatially selective electrochemical NMR spectroscopy

A parallel line probe for spatially selective electrochemical NMR spectroscopy

In situ NMR is a valuable tool for studying electrochemical devices, including redox flow batteries and electrocatalytic reactors, capable of detecting reaction intermediates, metastable states, time evolution of processes or monitoring stability as a function of electrochemical conditions. Here we report a parallel line detector for spatially selective in situ electrochemical NMR spectroscopy. The detector consists of 17 copper wires and is doubly tuned to 1H/19F and X nuclei ranging from 63Cu (106.1 MHz) to 7Li (155.5 MHz). The flat geometry of the parallel line detector allows its insertion into a high electrode surface-to-volume electrochemical flow reactor, enabling a detector-in-a-reactor design. This integrated device is named “eReactor NMR probe”. Combined with B1-selective pulse sequences, selective detection of the nuclei at the electrode-electrolyte interface, that is within a distance of 800 μm from the electrode surface, has been achieved. The selective detection of 7Li and 19F nuclei is demonstrated using two electrolytes, LiCl and LiBF4 solutions, respectively. A good B1 homogeneity with an 810° to 90° pulse intensity ratio of 68–72 % was achieved. Using electrochemical plating of lithium metal as a model reaction, we further demonstrated the operando functionality of the probe. The new eReactor NMR probe offers a general method for studying flow electrochemistry, and we envision applications in a wide range of environmentally relevant energy systems, for example, Li metal batteries, electrochemical ammonia synthesis, carbon dioxide capture and reduction, redox flow batteries, fuel cells, water desalination, lignin oxidation etc.

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来源期刊
CiteScore
3.80
自引率
13.60%
发文量
150
审稿时长
69 days
期刊介绍: The Journal of Magnetic Resonance presents original technical and scientific papers in all aspects of magnetic resonance, including nuclear magnetic resonance spectroscopy (NMR) of solids and liquids, electron spin/paramagnetic resonance (EPR), in vivo magnetic resonance imaging (MRI) and spectroscopy (MRS), nuclear quadrupole resonance (NQR) and magnetic resonance phenomena at nearly zero fields or in combination with optics. The Journal''s main aims include deepening the physical principles underlying all these spectroscopies, publishing significant theoretical and experimental results leading to spectral and spatial progress in these areas, and opening new MR-based applications in chemistry, biology and medicine. The Journal also seeks descriptions of novel apparatuses, new experimental protocols, and new procedures of data analysis and interpretation - including computational and quantum-mechanical methods - capable of advancing MR spectroscopy and imaging.
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