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Updated: May 29, 2026

05:21
A Scalable Balz-Schiemann Reaction Protocol in a Continuous Flow Reactor
Published on: February 10, 2023
HERFD XAS/ATR-FTIR batch reactor cell.
Martin Makosch1, Christiane Kartusch, Jacinto Sá
1Institute for Chemical and Bioengineering ETH Zurich, Wolfgang-Pauli Strasse, 8093 Zurich, Switzerland.
Physical Chemistry Chemical Physics : PCCP
|September 13, 2011
Summary
A novel reactor setup enables simultaneous X-ray absorption and infrared spectroscopy for in-situ catalyst analysis. This allows researchers to link catalyst structure changes to reaction activity and species during liquid-phase reactions.
Area of Science:
- Catalysis
- Materials Science
- Spectroscopy
Background:
- In situ characterization is crucial for understanding catalytic mechanisms.
- Simultaneous measurements of electronic structure and reaction species are challenging.
Purpose of the Study:
- To develop a versatile operando cell for combined HERFD XAS and ATR-FTIR spectroscopy.
- To enable simultaneous monitoring of catalyst structure and reaction dynamics.
Main Methods:
- Modification of an autoclave reactor for dual spectroscopy.
- High energy resolution fluorescence detected X-ray absorption spectroscopy (HERFD XAS).
- Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy.
Main Results:
- The developed cell allows simultaneous HERFD XAS and ATR-FTIR measurements without reactor redesign.
- Demonstrated catalyst precursor reduction in different solvents.
- Identified Au(0) as the primary species during nitrobenzene hydrogenation over Au/CeO(2).
Conclusions:
- The combined operando spectroscopy technique provides a powerful tool for in situ catalyst studies.
- This method facilitates the correlation of catalyst structural evolution with reaction performance.
- The system is applicable to various liquid-phase catalytic reactions.
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