Interdigitated metal electrodes for high-resolution in situ electrochemical NMR

• An interdigitated metal (Au) electrode system was developed.
• The cylindrically symmetric system is simple to build and easy-to-use.
• The system enables high-resolution NMR spectra to be recorded in situ electrochemically with sensitivity comparable to unmodified NMR systems.

Despite being among the most widely used spectroscopic methods, high-resolution NMR has not yet been applied routinely to electrochemistry and (organic) electrosynthesis, due largely to the incompatibility between NMR detection and electrical conduction of electrochemistry. Here, we introduce a straightforward, easy-to-construct system that incorporates high-resolution (HR) in situ NMR spectroscopy with electrochemistry by using cylindrically symmetric interdigitated metal (Au) electrodes. The constructed system is simple to build, inexpensive, and robust. It requires with minimal setup time and can be used with conventional commercial probes without the need of any modifications to them. To demonstrate the feasibility and performance of the system, we used 1H NMR to monitor the reversible redox reaction of ferrocene and 13C NMR to follow the electro-oxidation reaction of methanol on a commercial ptru electrocatalyst.

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