X-ray absorption spectroscopy and heterogeneous catalysis: Performances at the SOLEIL's SAMBA beamline

New plug-flow cells suitable for the X-ray absorption spectroscopy (XAS) study of heterogeneous catalysts by transmission and fluorescence detection modes are described. These cells are also suitable for combination with Raman spectroscopy providing valuable complementary information on the state of the catalyst in working conditions. On-line product analysis is obtained either by mass spectrometry or Raman spectroscopy providing a full description of the activity of the catalyst. These tools are successfully used for time-resolved investigations of heterogeneous catalysts in working conditions using the capability of the Quick-XAS monochromators installed at the SAMBA-SOLEIL beamline. The performances of the full set-up including spectrometers and reaction cells are illustrated by a study of the calcination step of a bimetallic hydrodesulphurisation catalyst and of the activation/reaction processes of a Fischer–Tropsch catalyst.

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► New plug-flow cells developed on the SAMBA beamline are presented.
► These studies combined Quick-XAS/XRD or Quick-XAS/Raman.
► Raman spectroscopy is used for monitoring the gas products during operando study.
► For the calcination of HDS NiMo catalyst, MoO42− is formed by depolymerisation.
► During the Fischer–Tropsch synthesis, a further reduction of Co is observed.