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Title: Small-volume, ultrahigh-vacuum-compatible high-pressure reaction cell for combined kinetic and in situ IR spectroscopic measurements on planar model catalysts

Abstract

We describe the design and performance of a high-pressure reaction cell for simultaneous kinetic and in situ infrared reflection (IR) spectroscopic measurements on model catalysts at elevated pressures, between 10{sup -3} and 10{sup 3} mbars, which can be operated both as batch reactor and as flow reactor with defined gas flow. The cell is attached to an ultrahigh-vacuum (UHV) system, which is used for sample preparation and also contains facilities for sample characterization. Specific for this design is the combination of a small cell volume, which allows kinetic measurements with high sensitivity under batch or continuous flow conditions, the complete isolation of the cell from the UHV part during UHV measurements, continuous temperature control during both UHV and high-pressure operation, and rapid transfer between UHV and high-pressure stage. Gas dosing is performed by a designed gas-handling system, which allows operation as flow reactor with calibrated gas flows at adjustable pressures. To study the kinetics of reactions on the model catalysts, a quadrupole mass spectrometer is connected to the high-pressure cell. IR measurements are possible in situ by polarization-modulation infrared reflection-absorption spectroscopy, which also allows measurements at elevated pressures. The performance of the setup is demonstrated by test measurements on themore » kinetics for CO oxidation and the CO adsorption on a Au/TiO{sub 2}/Ru(0001) model catalyst film at 1-50 mbar total pressure.« less

Authors:
; ; ; ;  [1]
  1. Department Surface Chemistry and Catalysis, University of Ulm, D-89069 Ulm (Germany)
Publication Date:
OSTI Identifier:
20778487
Resource Type:
Journal Article
Resource Relation:
Journal Name: Review of Scientific Instruments; Journal Volume: 76; Journal Issue: 12; Other Information: DOI: 10.1063/1.2140449; (c) 2005 American Institute of Physics; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; ABSORPTION SPECTROSCOPY; ADSORPTION; CATALYSTS; CHEMICAL REACTORS; DESIGN; GAS FLOW; GOLD; MASS SPECTROMETERS; MODULATION; OPERATION; OXIDATION; PERFORMANCE; POLARIZATION; REFLECTION; RUTHENIUM; SAMPLE PREPARATION; SENSITIVITY; TEMPERATURE CONTROL; TITANIUM OXIDES

Citation Formats

Zhao, Z., Diemant, T., Haering, T., Rauscher, H., and Behm, R.J. Small-volume, ultrahigh-vacuum-compatible high-pressure reaction cell for combined kinetic and in situ IR spectroscopic measurements on planar model catalysts. United States: N. p., 2005. Web. doi:10.1063/1.2140449.
Zhao, Z., Diemant, T., Haering, T., Rauscher, H., & Behm, R.J. Small-volume, ultrahigh-vacuum-compatible high-pressure reaction cell for combined kinetic and in situ IR spectroscopic measurements on planar model catalysts. United States. doi:10.1063/1.2140449.
Zhao, Z., Diemant, T., Haering, T., Rauscher, H., and Behm, R.J. Thu . "Small-volume, ultrahigh-vacuum-compatible high-pressure reaction cell for combined kinetic and in situ IR spectroscopic measurements on planar model catalysts". United States. doi:10.1063/1.2140449.
@article{osti_20778487,
title = {Small-volume, ultrahigh-vacuum-compatible high-pressure reaction cell for combined kinetic and in situ IR spectroscopic measurements on planar model catalysts},
author = {Zhao, Z. and Diemant, T. and Haering, T. and Rauscher, H. and Behm, R.J.},
abstractNote = {We describe the design and performance of a high-pressure reaction cell for simultaneous kinetic and in situ infrared reflection (IR) spectroscopic measurements on model catalysts at elevated pressures, between 10{sup -3} and 10{sup 3} mbars, which can be operated both as batch reactor and as flow reactor with defined gas flow. The cell is attached to an ultrahigh-vacuum (UHV) system, which is used for sample preparation and also contains facilities for sample characterization. Specific for this design is the combination of a small cell volume, which allows kinetic measurements with high sensitivity under batch or continuous flow conditions, the complete isolation of the cell from the UHV part during UHV measurements, continuous temperature control during both UHV and high-pressure operation, and rapid transfer between UHV and high-pressure stage. Gas dosing is performed by a designed gas-handling system, which allows operation as flow reactor with calibrated gas flows at adjustable pressures. To study the kinetics of reactions on the model catalysts, a quadrupole mass spectrometer is connected to the high-pressure cell. IR measurements are possible in situ by polarization-modulation infrared reflection-absorption spectroscopy, which also allows measurements at elevated pressures. The performance of the setup is demonstrated by test measurements on the kinetics for CO oxidation and the CO adsorption on a Au/TiO{sub 2}/Ru(0001) model catalyst film at 1-50 mbar total pressure.},
doi = {10.1063/1.2140449},
journal = {Review of Scientific Instruments},
number = 12,
volume = 76,
place = {United States},
year = {Thu Dec 15 00:00:00 EST 2005},
month = {Thu Dec 15 00:00:00 EST 2005}
}