Advanced Electrochemical NMR with Interdigitated Electrodes for High-Resolution In-Situ Analysis

OVERVIEW

Georgetown University researchers developed a system combining electrochemical methods with Nuclear Magnetic Resonance (NMR) spectroscopy to study chemical reactions during processes like electrolysis. The system uses interdigitated electrodes in a comb-like arrangement, minimizing NMR-electrochemical coupling and maximizing electrode surface area in the NMR tube. This design boosts sensitivity and allows detailed analysis of electrochemical processes. Unlike traditional methods, this system enables real-time assessment within commercial NMR tubes, preserving spectra quality for accurate reaction monitoring. It minimizes setup complexities and accommodates various sample types and sizes. The electrodes can be coated with electro-catalysts, allowing studies of diverse catalysts and reactions. This feature provides insights into reaction kinetics and efficiency, expanding the device's utility for complex chemical systems. The system's design enhances accessibility across research disciplines and versatility in scientific applications, from small molecules to complex compounds.

BACKGROUND

The invention combines electrochemistry and Nuclear Magnetic Resonance (NMR) spectroscopy, essential techniques in chemical research. Electrochemistry studies electron movement in processes like batteries, while NMR spectroscopy analyzes molecular structure and dynamics. Traditionally, combining these methods required removing samples from electrochemical cells for NMR analysis, disrupting reactions and causing inaccuracies. Georgetown University researchers developed a system integrating electrochemical methods with NMR spectroscopy for real-time, high-resolution analysis within the NMR tube. This preserves NMR spectra integrity and allows continuous reaction monitoring. The system minimizes setup complexities, accommodates various sample types, and enhances research efficiency and accuracy, benefiting both academic and industrial applications.

Benefit

• The system allows for real-time, in-situ analysis of electrochemical processes and chemical reactions directly within the NMR tube.
• It reduces the need for multiple instruments and simplifies experimental setups. This efficiency helps in saving costs associated with equipment and resources.
• Accommodates various sample types and sizes commonly used in NMR experiments, making it versatile for different research applications.

Market Application

• Enables real-time analysis of electrochemical reactions and reduces time and resources required for development.
• Provides detailed insights into catalyst activity and selectivity during chemical reactions, supporting the pharmaceutical industry with fast and reliable analytical methods.
• Offers real-time characterization of material structures and properties during synthesis, guiding the design of new materials with enhanced functionalities and optimizing production processes.

Publications

• Sorte, E. G.; Tong, Y. J. Interdigitated Metal Electrodes for High-Resolution in Situ Electrochemical NMR. J Electroanal Chem
  2016, 769, 1–4. https://doi.org/10.1016/j.jelechem.2016.03.003.
• Sorte, E. G.; Jilani, S.; Tong, Y. J. Methanol and Ethanol Electrooxidation on PtRu and PtNiCu as Studied by High-Resolution In Situ Electrochemical NMR Spectroscopy with Interdigitated Electrodes. Electrocatalysis
  2017, 8 (2), 95–102. https://doi.org/10.1007/s12678-016-0344-8.
• Tong, Y. J. In Situ Electrochemical Nuclear Magnetic Resonance Spectroscopy for Electrocatalysis: Challenges and Prospects. Curr Opin Electrochem
  2017, 4 (1), 60–68. https://doi.org/10.1016/j.coelec.2017.09.017.
• US Patent No. 10,948,441