Original Paper

Topics in Catalysis

, Volume 56, Issue 11, pp 896-904

First online:

Characterization of Metal-Oxide Catalysts in Operando Conditions by Combining X-ray Absorption and Raman Spectroscopies in the Same Experiment

  • A. PatlollaAffiliated withPhysics Department, Yeshiva University
  • , P. BaumannAffiliated withPhysics Department, Yeshiva UniversityUniversity of Applied Sciences of Northwestern Switzerland
  • , W. XuAffiliated withDepartment of Chemistry, Brookhaven National Laboratory
  • , S. D. SenanayakeAffiliated withDepartment of Chemistry, Brookhaven National Laboratory
  • , J. A. RodriguezAffiliated withDepartment of Chemistry, Brookhaven National Laboratory
  • , A. I. FrenkelAffiliated withPhysics Department, Yeshiva University Email author 

Rent the article at a discount

Rent now

* Final gross prices may vary according to local VAT.

Get Access


We have developed a new instrumental setup that combines simultaneous X-ray absorption spectroscopy, Raman spectroscopy and online mass spectrometry for operando studies of catalytic reactions. The importance of combining these techniques in the same experiment is demonstrated with the example of CO oxidation over nanoscale copper oxide catalysts supported on high surface area titanium oxide. X-ray absorption near edge structure (XANES) spectroscopy provides information on the charge state and local geometry of the catalytically active atoms. Extended X-ray absorption fine-structure (EXAFS) technique adds information about their local coordination environment. Raman spectroscopy adds sensitivity to crystallographic phase and long range order that both XANES and EXAFS are lacking. Together, these measurements enable simultaneous studies of the structural and electronic properties of all components present in metal-oxide catalysts. Coupled with online reactant and product analysis, this new setup allows one to elucidate the synergy between different components of a catalytic system and shed light on its catalytic activity and selectivity.


Multi-technique characterization Operando studies Metal Oxide catalysts Oxygen reservoir