In situ studies of electrochemical processes using NMR offer valuable information on reaction mechanisms, kinetics, and species identification, making it a powerful tool in electrochemistry research. In this study, we present the design of an in situ redox-flow NMR cell that allows for a continuous flow of liquid (electrolyte) or gas, application of electrical voltage, and recording of NMR signals. The utility of this setup is demonstrated through two case studies: electrochemical copper deposition on a gold electrode and the electrochemical conversion of carbon dioxide into hydrocarbon products. Specifically, the presence of multicarbon products containing C–C bonds generated during the electrochemical reduction reaction is confirmed in the H NMR spectra in the latter example. These findings highlight the ability of the in situ redox-flow NMR cell to directly monitor reaction intermediates and products, thereby enabling the elucidation of reaction mechanisms for the efficient and selective production of valuable hydrocarbon products through the conversion of CO into value-added chemicals. In contrast to other reported in situ NMR cells, the presented cell is suitable for multiple uses, and allows detecting NMR signals not only from exhaust products but also from those formed on the catalyst surface.

中文翻译：

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通过原位流核磁共振波谱检测电催化和化学过程

使用核磁共振对电化学过程进行原位研究提供了有关反应机制、动力学和物种鉴定的宝贵信息，使其成为电化学研究中的强大工具。在这项研究中，我们提出了原位氧化还原流核磁共振池的设计，该池允许液体（电解质）或气体连续流动、施加电压并记录核磁共振信号。通过两个案例研究证明了该装置的实用性：金电极上的电化学铜沉积和二氧化碳电化学转化为碳氢化合物产品。具体来说，在后一个例子的 1H NMR 谱中证实了电化学还原反应过程中产生的含有 C-C 键的多碳产物的存在。这些发现凸显了原位氧化还原流核磁共振单元直接监测反应中间体和产物的能力，从而能够阐明通过将CO转化为增值化学品来高效、选择性地生产有价值的碳氢化合物产品的反应机制。与其他报道的原位 NMR 电池相比，该电池适用于多种用途，并且不仅可以检测来自废气产物的 NMR 信号，还可以检测催化剂表面形成的 NMR 信号。