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Title: Design and Operation of a High Pressure Reaction Cell for in situ X-ray Absorption Spectroscopy

Abstract

X-ray absorption spectroscopy measurements of catalytic reactions have been instrumental in advancing the understanding of catalytic processes. These measurements require an in situ catalysis reaction cell with unique properties. Here we describe the design and initial operation of an in situ/operando catalysis reaction cell for transmission X-ray absorption spectroscopy measurements. The cell is designed: to be an ideal catalytic reactor with no mass transfer effects; to give the same conversion and selectivity under similar space velocities as standard laboratory micro-reactors; to be operational temperatures up to 600 {sup o}C and pressures up to 14 bar; to be X-ray transparent allowing XAS measurement to be collected in transmission for all elements with Z {>=} 23 (vanadium K-edge at 5.5 keV); to measure the actual catalyst bed temperature; to not use o-ring seals, or water cooling; to be robust, compact, easy to assemble, and use, and relatively low cost to produce. The heart of the cell is fabricated from an X-ray transparent beryllium tube that forms a plug flow reactor. XAFS data recorded during the reduction of a Re/{gamma}-A{sub 2}O{sub 3} catalyst as a function of hydrogen pressure from 0.05 to 8 bar, and from a Pt-Sn/{gamma}-A{sub 2}O{sub 3} catalyst during n-heptanemore » reforming are given as initial examples of the versatility of the reactor.« less

Authors:
; ; ; ;
Publication Date:
Research Org.:
Brookhaven National Laboratory (BNL) National Synchrotron Light Source
Sponsoring Org.:
Doe - Office Of Science
OSTI Identifier:
929920
Report Number(s):
BNL-80510-2008-JA
Journal ID: ISSN 0920-5861; CATTEA; TRN: US200822%%1093
DOE Contract Number:
DE-AC02-98CH10886
Resource Type:
Journal Article
Resource Relation:
Journal Name: Catalysis Today; Journal Volume: 126
Country of Publication:
United States
Language:
English
Subject:
08 HYDROGEN; ABSORPTION SPECTROSCOPY; BERYLLIUM; CATALYSIS; CATALYSTS; CONVERSION; COOLING; DESIGN; ELEMENTS; GASKETS; HYDROGEN; MASS TRANSFER; OPERATION; PRESSURE RANGE MEGA PA 10-100; REDUCTION; SEALS; TRANSMISSION; TUBES; VANADIUM; X-RAY SPECTROSCOPY; national synchrotron light source

Citation Formats

Bare,S., Yang, N., Kelly, S., Mickelson, G., and Modica, F. Design and Operation of a High Pressure Reaction Cell for in situ X-ray Absorption Spectroscopy. United States: N. p., 2007. Web. doi:10.1016/j.cattod.2006.10.007.
Bare,S., Yang, N., Kelly, S., Mickelson, G., & Modica, F. Design and Operation of a High Pressure Reaction Cell for in situ X-ray Absorption Spectroscopy. United States. doi:10.1016/j.cattod.2006.10.007.
Bare,S., Yang, N., Kelly, S., Mickelson, G., and Modica, F. Mon . "Design and Operation of a High Pressure Reaction Cell for in situ X-ray Absorption Spectroscopy". United States. doi:10.1016/j.cattod.2006.10.007.
@article{osti_929920,
title = {Design and Operation of a High Pressure Reaction Cell for in situ X-ray Absorption Spectroscopy},
author = {Bare,S. and Yang, N. and Kelly, S. and Mickelson, G. and Modica, F.},
abstractNote = {X-ray absorption spectroscopy measurements of catalytic reactions have been instrumental in advancing the understanding of catalytic processes. These measurements require an in situ catalysis reaction cell with unique properties. Here we describe the design and initial operation of an in situ/operando catalysis reaction cell for transmission X-ray absorption spectroscopy measurements. The cell is designed: to be an ideal catalytic reactor with no mass transfer effects; to give the same conversion and selectivity under similar space velocities as standard laboratory micro-reactors; to be operational temperatures up to 600 {sup o}C and pressures up to 14 bar; to be X-ray transparent allowing XAS measurement to be collected in transmission for all elements with Z {>=} 23 (vanadium K-edge at 5.5 keV); to measure the actual catalyst bed temperature; to not use o-ring seals, or water cooling; to be robust, compact, easy to assemble, and use, and relatively low cost to produce. The heart of the cell is fabricated from an X-ray transparent beryllium tube that forms a plug flow reactor. XAFS data recorded during the reduction of a Re/{gamma}-A{sub 2}O{sub 3} catalyst as a function of hydrogen pressure from 0.05 to 8 bar, and from a Pt-Sn/{gamma}-A{sub 2}O{sub 3} catalyst during n-heptane reforming are given as initial examples of the versatility of the reactor.},
doi = {10.1016/j.cattod.2006.10.007},
journal = {Catalysis Today},
number = ,
volume = 126,
place = {United States},
year = {Mon Jan 01 00:00:00 EST 2007},
month = {Mon Jan 01 00:00:00 EST 2007}
}