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Title: Transmission and fluorescence X-ray absorption spectroscopy cell/flow reactor for powder samples under vacuum or in reactive atmospheres

Abstract

X-ray absorption spectroscopy is an element-specific technique for probing the local atomic-scale environment around an absorber atom. It is widely used to investigate the structures of liquids and solids, being especially valuable for characterization of solid-supported catalysts. Reported cell designs are limited in capabilities—to fluorescence or transmission and to static or flowing atmospheres, or to vacuum. Our goal was to design a robust and widely applicable cell for catalyst characterizations under all these conditions—to allow tracking of changes during genesis and during operation, both under vacuum and in reactive atmospheres. Herein, we report the design of such a cell and a demonstration of its operation both with a sample under dynamic vacuum and in the presence of gases flowing at temperatures up to 300 °C, showing data obtained with both fluorescence and transmission detection. The cell allows more flexibility in catalyst characterization than any reported.

Authors:
; ;  [1]; ; ;  [2];  [3]
  1. Department of Chemical Engineering, University of California at Davis, Davis, California 95616 (United States)
  2. KAUST Catalysis Center (KCC), King Abdullah University of Science and Technology (KAUST), 23955-6900 Thuwal (Saudi Arabia)
  3. SLAC National Accelerator Laboratory, SSRL, Menlo Park, California 94025 (United States)
Publication Date:
OSTI Identifier:
22597799
Resource Type:
Journal Article
Resource Relation:
Journal Name: Review of Scientific Instruments; Journal Volume: 87; Journal Issue: 7; Other Information: (c) 2016 Author(s); Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY; 75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; ABSORPTION; ABSORPTION SPECTROSCOPY; ATMOSPHERES; CATALYSTS; DESIGN; FLEXIBILITY; FLUORESCENCE; GASES; LIQUIDS; POWDERS; TEMPERATURE RANGE 0400-1000 K; TRANSMISSION; X RADIATION; X-RAY SPECTROSCOPY

Citation Formats

Hoffman, A. S., Debefve, L. M., Gates, B. C., E-mail: bcgates@ucdavis.edu, Bendjeriou-Sedjerari, A., Ouldchikh, S., Basset, J.-M., and Bare, Simon R.. Transmission and fluorescence X-ray absorption spectroscopy cell/flow reactor for powder samples under vacuum or in reactive atmospheres. United States: N. p., 2016. Web. doi:10.1063/1.4958824.
Hoffman, A. S., Debefve, L. M., Gates, B. C., E-mail: bcgates@ucdavis.edu, Bendjeriou-Sedjerari, A., Ouldchikh, S., Basset, J.-M., & Bare, Simon R.. Transmission and fluorescence X-ray absorption spectroscopy cell/flow reactor for powder samples under vacuum or in reactive atmospheres. United States. doi:10.1063/1.4958824.
Hoffman, A. S., Debefve, L. M., Gates, B. C., E-mail: bcgates@ucdavis.edu, Bendjeriou-Sedjerari, A., Ouldchikh, S., Basset, J.-M., and Bare, Simon R.. Fri . "Transmission and fluorescence X-ray absorption spectroscopy cell/flow reactor for powder samples under vacuum or in reactive atmospheres". United States. doi:10.1063/1.4958824.
@article{osti_22597799,
title = {Transmission and fluorescence X-ray absorption spectroscopy cell/flow reactor for powder samples under vacuum or in reactive atmospheres},
author = {Hoffman, A. S. and Debefve, L. M. and Gates, B. C., E-mail: bcgates@ucdavis.edu and Bendjeriou-Sedjerari, A. and Ouldchikh, S. and Basset, J.-M. and Bare, Simon R.},
abstractNote = {X-ray absorption spectroscopy is an element-specific technique for probing the local atomic-scale environment around an absorber atom. It is widely used to investigate the structures of liquids and solids, being especially valuable for characterization of solid-supported catalysts. Reported cell designs are limited in capabilities—to fluorescence or transmission and to static or flowing atmospheres, or to vacuum. Our goal was to design a robust and widely applicable cell for catalyst characterizations under all these conditions—to allow tracking of changes during genesis and during operation, both under vacuum and in reactive atmospheres. Herein, we report the design of such a cell and a demonstration of its operation both with a sample under dynamic vacuum and in the presence of gases flowing at temperatures up to 300 °C, showing data obtained with both fluorescence and transmission detection. The cell allows more flexibility in catalyst characterization than any reported.},
doi = {10.1063/1.4958824},
journal = {Review of Scientific Instruments},
number = 7,
volume = 87,
place = {United States},
year = {Fri Jul 15 00:00:00 EDT 2016},
month = {Fri Jul 15 00:00:00 EDT 2016}
}