Synchrotron beamline setup enabling quasi-simultaneous PXRD and XANES measurements: case study of Fischer–Tropsch catalyst reduction at 60 bar

Powder X-ray diffraction (PXRD) and X-ray absorption near-edge structure (XANES) spectroscopy are complementary techniques for probing cobalt-based (Co-based) Fischer-Tropsch synthesis (FTS) catalyst structures. PXRD reveals crystalline composition, while XANES provides information on coordination geometry and oxidation state. We developed a fast, automated measurement method, based on rapid selection of X-ray beam energy and a dedicated sample environment at beamline ID10 (ESRF), to combine in situ PXRD and XANES in a single experiment. This approach enables simultaneous monitoring of structural and electronic changes in Co-based FTS catalysts under in situ conditions up to 60 bar, offering a comprehensive view of catalyst dynamics.