Metrohm Hyphenated EC-Raman for electrocatalysis

Importance of the Topic

Combining electrochemical techniques with in situ Raman spectroscopy is critical for understanding electrocatalytic reactions at the molecular level. Operando measurements reveal real-time structural transformations, adsorbed intermediates and products, enabling rational catalyst design and optimization.

Purpose and Study Overview

This work presents two integrated EC-Raman solutions—Explorer and Starter—tailored for electrocatalysis researchers. Both packages synchronize electrochemical control with Raman data acquisition through a trigger cable and dedicated software, simplifying operando analyses without complex setups.

Methodology

• Synchronize potentiostat/galvanostat and Raman spectrometer using a trigger cable under NOVA software control.
• Perform operando Raman spectroscopy during electrochemical experiments to monitor catalyst structure and adsorbate evolution.
• Apply complementary techniques such as electrochemical impedance spectroscopy (EIS), surface-enhanced Raman spectroscopy (SERS) and Raman microscopy.

Used Instrumentation

• Autolab PGSTAT302N (Explorer) or PGSTAT204 (Starter) potentiostat/galvanostat with built-in EIS module; modular architecture allows addition of bipotentiostat, low-current amplifier and linear scan generator.
• B&W Tek i-Raman Plus 532H spectrometer: 532 nm laser (30 mW), cooled CCD detector, spectral range 65–3400 cm⁻¹, resolution < 3.5 cm⁻¹.
• B&W Tek BAC151 Raman Video Microsampling System with coaxial LED illumination, video camera and interchangeable 20×/50× objectives for macro/micro analysis.

Key Results and Discussion

The EC-Raman Explorer and Starter solutions deliver high-throughput operando data, capturing dynamic changes in catalyst surfaces and adsorbed species. The fiber-optic probe and video microscope facilitate versatile sample interrogation across various electrochemical cells. Modular potentiostat options ensure adaptability as research demands evolve.

Benefits and Practical Applications

• Ready-to-use turnkey system minimizes setup time and training requirements.
• Simultaneous structural and functional data support mechanistic studies in energy conversion, sensor development and materials science.
• Compact and portable configuration (Starter) allows flexible deployment in diverse laboratory environments.
• Scalable instrumentation adapts to evolving research needs through modular add-ons.

Future Trends and Applications

Integration of advanced cell designs and rotating ring-disk electrodes, high-speed scan capabilities and femtoamp-level current resolution will expand operando EC-Raman applications. Coupling with automation, AI-driven spectral analysis and high-throughput platforms promises accelerated catalyst screening and deeper mechanistic insights.

Conclusion

Metrohm’s hyphenated EC-Raman solutions offer streamlined operando measurement capabilities by synchronizing electrochemical control with Raman spectroscopy. These turnkey systems enable detailed mechanistic studies, foster rapid technology development and support flexible adaptation to future research challenges.