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Keywords:

  • X-ray diffraction;
  • diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy;
  • reaction cells;
  • multitechnique approaches;
  • calcium oxalate thermal decomposition;
  • in operando and in situ characterization

In heterogeneous catalysis, chemical reactions take place at the surface of the material and can be influenced by its structure. To understand better the impact of the material surface and structure on catalytic properties, it is important to characterize them simultaneously. The association of X-ray diffraction and diffuse reflectance infrared Fourier transform spectroscopy, combined in a single dedicated high-temperature and high-pressure reaction cell with an online gas chromatograph, could be the answer to this challenge. For the first time, such an analytical tool has been developed for laboratory applications. The use of this device is illustrated, and it is validated through the in situ study of the thermal decomposition of calcium oxalate.