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In Situ Infrared Emission Spectroscopy for Quantitative Gas-Phase Measurement Under High Temperature Reaction Conditions: An Analytical Method for Methane by Means of an Innovative Small-Volume Flowing Cell

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Abstract:

We have used infrared emission spectroscopy (IRES) in order to perform in situ studies under flowing gas-phase conditions. When the small-volume cell developed herein is used, we can (1) observe emission spectra from a hot gas-phase sample having an effective volume much less than one milliliter, (2) observe spectra of typical molecular species present, and (3) observe spectra of the more important molecular species down to below 10% and in some cases even as low as 1%. In addition, an analytical method has been derived in order to conduct quantitative studies under typical reaction conditions. We show that simplifications can be made in the data acquisition and handling for a direct linear correlation between band intensity and concentration with only simple background correction. The practical lower limit for methane in the present setup is approximately 0.5–1% v/v depending on the selected temperature. Our data were collected at 500, 600, and 700 °C, respectively. The major features of the present cell design are fairly simple and basically formed by a quartz tube (outer diameter=6 mm, inner diameter=4 mm) inside a metal pipe and two tubular ceramic heaters. This simple setup has advantages and attractive features that have extended the application of IRES to new fields and, in particular, for in situ studies of hydrocarbon reactions at different residence times at high temperature.

Keywords: GAS-PHASE ANALYSIS; HIGH TEMPERATURE; INFRARED EMISSION SPECTROSCOPY; METHANE; SELF-DESIGNED INFRARED EMISSION CELL

Document Type: Research Article

DOI: http://dx.doi.org/10.1366/000370210790619564

Affiliations: 1: SINTEF Materials and Chemistry, Department of Hydrocarbon Process Chemistry, P.O. Box 124 Blindern, N-0314 Oslo, Norway 2: Centre for Theoretical and Computational Chemistry, Department of Chemistry, University of Oslo, P.O. Box 1033 Blindern, N-0315 Oslo, Norway 3: Telemark University College, P.O. Box 203, N-3901 Porsgrunn, Norway 4: SINTEF Materials and Chemistry, Department of Hydrocarbon Process Chemistry, P.O. Box 124 Blindern, N-0314 Oslo, Norway. Email: elisabeth.tangstad@sintef.no

Publication date: February 1, 2010

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