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Dynamics in electrochemical organic oxidation reactions from in situ and operando techniques

Nature Reviews Chemistry volume 9, pages 766–789 (2025)Cite this article

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A Publisher Correction to this article was published on 10 November 2025

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Abstract

Electrochemical organic oxidation reactions (OORs) play a pivotal role in various industrial processes and sustainable chemical production, transforming small molecules into value-added products. Understanding electrode surface dynamics, catalyst structures, reaction intermediates and product selectivity during OOR is crucial for both fundamental knowledge and the design of high-performance electrocatalysts and economically valuable reactions. The advancement of in situ and operando techniques, especially X-ray absorption and Raman and infrared spectroscopies, as well as differential electrochemical mass spectrometry, provide powerful tools for studying OORs. In situ methods reveal catalyst structural changes under applied bias and reaction-relevant conditions, whereas operando techniques simultaneously monitor both structure and activity in real operating conditions. This Review addresses the achievements towards closing the knowledge gap between fundamental, lab-scale studies and industrial, large-scale applications using in situ and operando techniques to uncover bulk catalyst structures, catalyst–surface–electrolyte dynamics and local transient product formation during anodic OORs. It also highlights the underlying principles of these techniques, offering perspectives on future prospects and challenges for advancing OOR applications, particularly in discovering next-generation efficient catalysts.

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Fig. 1: In situ and operando probing of electrochemical organic oxidation reactions (OORs).
Fig. 2: In situ and operando techniques used to investigate organic oxidation reactions.
Fig. 3: Overview of the organic oxidation reactions (OORs) explored in hybrid water electrolysers.
Fig. 4: Application of X-ray diffraction and X-ray absorption spectroscopies for electrochemical organic oxidation reactions.
Fig. 5: Application of X-ray photoelectron spectroscopy, ultraviolet–visible (UV–Vis) spectroscopy and electrochemical impedance spectroscopy (EIS) for electrochemical organic oxidation reactions.
Fig. 6: Application of Raman spectroscopy for electrochemical organic oxidation reactions.
Fig. 7: Application of infrared spectroscopy for electrochemical organic oxidation reactions.
Fig. 8: Application of sum frequency generation (SFG) for electrochemical organic oxidation reactions.
Fig. 9: Application of differential electrochemical mass spectrometry (DEMS) for electrochemical organic oxidation reactions.
Fig. 10: Application of NMR, cyclic voltammetry (CV) and inductively coupled plasma mass spectrometry (ICP-MS) for electrochemical organic oxidation reactions.
Fig. 11: Future outlook of in situ and operando techniques for electrochemical organic oxidation reactions.

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Acknowledgements

This work is funded by the German Federal Ministry of Education and Research (BMBF) in the framework of the project Catlab (03EW0015A/B) and the project PrometH2eus (03HY105C). The authors also acknowledge support from the Deutsche Forschungsgemeinschaft (DFG; German Research Foundation) under Germany’s Excellence Strategy – EXC 2008/1 – 390540038 – UniSysCat.

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  1. These authors contributed equally: Basundhara Dasgupta, Debabrata Bagchi.

Authors and Affiliations

  1. Department of Chemistry, Metalorganics and Inorganic Materials, Technische Universität Berlin, Berlin, Germany

    Basundhara Dasgupta, Matthias Driess & Prashanth W. Menezes

  2. Department of Materials Chemistry for Catalysis, Helmholtz-Zentrum Berlin für Materialien und Energie, Berlin, Germany

    Debabrata Bagchi & Prashanth W. Menezes

  3. Strategy Department of Energy and Information, Helmholtz-Zentrum Berlin für Materialien und Energie, Berlin, Germany

    Tobias Sontheimer

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P.W.M. conceived the idea, proposed the topic and designed the Review structure. B.D. and D.B. collaboratively planned, organized and co-authored the initial draft. T.S., M.D. and P.W.M. were involved in reviewing, discussing and supervising the Review.

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Dasgupta, B., Bagchi, D., Sontheimer, T. et al. Dynamics in electrochemical organic oxidation reactions from in situ and operando techniques. Nat Rev Chem 9, 766–789 (2025). https://doi.org/10.1038/s41570-025-00767-7

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