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Operando anomalous X-ray powder diffraction interleaved with X-ray absorption spectroscopy using a scanning 2D imaging detector on the XMaS beamline: design, implementation and performance

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Title: Operando anomalous X-ray powder diffraction interleaved with X-ray absorption spectroscopy using a scanning 2D imaging detector on the XMaS beamline: design, implementation and performance
Authors: Dariusz Wardecki, Paul B. J. Thompson, Kinga Mlekodaj, Mark G. Dowsett, Mieke Adriaens, Amy J. Knorpp, Catherine Dejoie, Kinga Góra-Marek, Jeroen A. van Bokhoven, Mark A. Newton, Przemyslaw Rzepka
Source: Journal of Applied Crystallography. 58:1778-1788
Publisher Information: International Union of Crystallography (IUCr), 2025.
Publication Year: 2025
Description: We present a method for achieving high-quality anomalous X-ray powder diffraction, interleaved with transmission X-ray absorption spectroscopy, using a flat-panel imaging detector scanned over a large angular range. Anomalous X-ray powder diffraction is a technique that enables the highlighting of specific elements within a crystal structure and pinpointing the nature of active (or inactive) sites involved in specific reactions in situ or in an operando manner. This approach enables the collection of a Q range that is not attainable using static flat-panel detectors in the absorption energy regimes used (8.94–17.5 keV). We consider the advantages and limitations of such an approach compared with alternative methods and describe in detail how it is achieved, along with the data processing and workflow required for an accurate restoration of conventional X-ray powder diffraction and anomalous X-ray powder diffraction data from sequentially acquired images. We demonstrate the applicability and capacity of this method for the in situ/operando restoration of the positions and atomic arrangement of copper atoms in the elevated-temperature aerobic activation of a copper-ion-exchanged zeolite, Cu–mazzite.
Document Type: Article
ISSN: 1600-5767
DOI: 10.1107/s1600576725007022
Rights: CC BY
Accession Number: edsair.doi...........cecbfdb3df3acc653129901920e380b2
Database: OpenAIRE
Description
Abstract:We present a method for achieving high-quality anomalous X-ray powder diffraction, interleaved with transmission X-ray absorption spectroscopy, using a flat-panel imaging detector scanned over a large angular range. Anomalous X-ray powder diffraction is a technique that enables the highlighting of specific elements within a crystal structure and pinpointing the nature of active (or inactive) sites involved in specific reactions in situ or in an operando manner. This approach enables the collection of a Q range that is not attainable using static flat-panel detectors in the absorption energy regimes used (8.94–17.5 keV). We consider the advantages and limitations of such an approach compared with alternative methods and describe in detail how it is achieved, along with the data processing and workflow required for an accurate restoration of conventional X-ray powder diffraction and anomalous X-ray powder diffraction data from sequentially acquired images. We demonstrate the applicability and capacity of this method for the in situ/operando restoration of the positions and atomic arrangement of copper atoms in the elevated-temperature aerobic activation of a copper-ion-exchanged zeolite, Cu–mazzite.
ISSN:16005767
DOI:10.1107/s1600576725007022