Abstract
A new cell for in situ combined X-ray absorption, diffuse reflectance IR Fourier transform and mass spectroscopies (XAS-DRIFTS-MS) is presented. The cell stands out among others for its achievements and flexibility. It is possible to perform XAS measurements in transmission or fluorescence modes, and the cell is compatible with external devices like UV-light and Raman probes. It includes different sample holders compatible with the different XAS detection modes, different sample forms (free powder or self-supporting pellet) and different sample loading/total absorption. Additionally, it has a small dead volume and can operate over a wide range of temperature (up to 600°C) and pressure (up to 5 bar). Three research examples will be shown to illustrate the versatility of the cell. This cell covers a wider range of applications than any other cell currently known for this type of study.
Highlights
Heterogeneous catalysis is one of the most important branches of applied chemistry (Friend & Xu, 2017)
Catalysts often constitute dilute materials on top of a heavy matrix, where XAS measurements have to be conducted in fluorescence mode. To overcome these limitations we have improved the design of this cell (Agostini et al, 2018) to perform coupled experiments using XAS, DRIFTS and MS, on highly dilute materials and/or heavy matrices where XAS measurements in fluorescence mode are necessary
The combined XAS–DRIFTS system is composed of a commercial Varian 680 FT–IR instrument, a set of Au-coated mirrors and a diffuse reflectance sphere provided by OMT Solutions
Summary
Heterogeneous catalysis is one of the most important branches of applied chemistry (Friend & Xu, 2017). The multi-technique approach is an attempt to overcome this drawback In this sense, the combination of X-ray absorption, diffuse reflectance IR Fourier transform and mass spectroscopies (XAS, DRIFTS and MS) covers a significant range of properties and behaviours of interest in the solid–gas-phase heterogeneous catalytic cycle. More than ten years ago, Newton and co-workers (Newton et al, 2004, 2007) designed a combined XAS, DRIFTS and MS experiment on beamline ID24 at the ESRF With this cell, fast gas switching was possible, but the temperature was limited (400C) and the cell presented a bypass of the gas feed in the catalytic bed. To overcome these limitations we have improved the design of this cell (Agostini et al, 2018) to perform coupled experiments using XAS, DRIFTS and MS, on highly dilute materials and/or heavy matrices where XAS measurements in fluorescence mode are necessary
Sign-in/Register to view highlights & summary Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a callDisclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.
