Effective bulk and surface temperatures of the catalyst bed of FT-IR cells used for in situ and operando studies

The temperature prevailing in the catalyst bed of three different IR spectroscopic reaction cells was assessed by means of thermocouples, an optical pyrometer and reaction rate measurements. One of the cells was a custom-made transmission FT-IR cell for use with thin wafers and the two others were c...

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Veröffentlicht in:Physical chemistry chemical physics : PCCP 2013-01, Vol.15 (19), p.7321-7327
Hauptverfasser: Li, Haoguang, Rivallan, Mickael, Thibault-Starzyk, Frederic, Travert, Arnaud, Meunier, Frederic C
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container_issue 19
container_start_page 7321
container_title Physical chemistry chemical physics : PCCP
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creator Li, Haoguang
Rivallan, Mickael
Thibault-Starzyk, Frederic
Travert, Arnaud
Meunier, Frederic C
description The temperature prevailing in the catalyst bed of three different IR spectroscopic reaction cells was assessed by means of thermocouples, an optical pyrometer and reaction rate measurements. One of the cells was a custom-made transmission FT-IR cell for use with thin wafers and the two others were commercial Harrick and Spectra-Tech diffuse reflectance FT-IR (DRIFTS) cells used for the analysis of powdered samples. The rate of CO methanation measured over a 16 wt% Ni/alumina catalyst was used as a means to derive the effective temperature prevailing in the IR cells from that existing in a traditional (non-spectroscopic) reactor having a well-controlled temperature. The sample bed of these three IR cells exhibited a significantly lower temperature than that of the corresponding measure thermocouple, which was yet located in or close to the sample bed. The comparison of Arrhenius plots enabled us to determine a temperature correction valid over a large temperature range. The use of an optical pyrometer was assessed with a view to determining the temperature of the surface of the powdered beds and that at the centre of the wafer. The optical pyrometer proved useful in the case of the catalyst powder, which behaved as a black non-reflecting body. In contrast, the temperature reading was inaccurate in the case of the pressed wafer, probably due to the shiny surface and minute thickness of the wafer, which led to a significant portion of the IR radiation of the surroundings being reflected by and transmitted through the wafer. The optical pyrometer data showed that the temperature of the surface of the powdered beds was significantly lower than that of the bulk of the bed, and that the total flow rate and composition did not affect this value. This work emphasises that the effective bed temperature in spectroscopic cells can be significantly different from that given by measure thermocouples, even when located in the vicinity of the sample, but that the calibration curves derived from rate measurements can be used to overcome this problem. The bulk and surface temperatures of sample beds of spectroscopic cells can be significantly lower than expected and can be derived from Arrhenius plots of model reactions and optical pyrometry.
doi_str_mv 10.1039/c3cp50442e
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One of the cells was a custom-made transmission FT-IR cell for use with thin wafers and the two others were commercial Harrick and Spectra-Tech diffuse reflectance FT-IR (DRIFTS) cells used for the analysis of powdered samples. The rate of CO methanation measured over a 16 wt% Ni/alumina catalyst was used as a means to derive the effective temperature prevailing in the IR cells from that existing in a traditional (non-spectroscopic) reactor having a well-controlled temperature. The sample bed of these three IR cells exhibited a significantly lower temperature than that of the corresponding measure thermocouple, which was yet located in or close to the sample bed. The comparison of Arrhenius plots enabled us to determine a temperature correction valid over a large temperature range. The use of an optical pyrometer was assessed with a view to determining the temperature of the surface of the powdered beds and that at the centre of the wafer. The optical pyrometer proved useful in the case of the catalyst powder, which behaved as a black non-reflecting body. In contrast, the temperature reading was inaccurate in the case of the pressed wafer, probably due to the shiny surface and minute thickness of the wafer, which led to a significant portion of the IR radiation of the surroundings being reflected by and transmitted through the wafer. The optical pyrometer data showed that the temperature of the surface of the powdered beds was significantly lower than that of the bulk of the bed, and that the total flow rate and composition did not affect this value. This work emphasises that the effective bed temperature in spectroscopic cells can be significantly different from that given by measure thermocouples, even when located in the vicinity of the sample, but that the calibration curves derived from rate measurements can be used to overcome this problem. 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One of the cells was a custom-made transmission FT-IR cell for use with thin wafers and the two others were commercial Harrick and Spectra-Tech diffuse reflectance FT-IR (DRIFTS) cells used for the analysis of powdered samples. The rate of CO methanation measured over a 16 wt% Ni/alumina catalyst was used as a means to derive the effective temperature prevailing in the IR cells from that existing in a traditional (non-spectroscopic) reactor having a well-controlled temperature. The sample bed of these three IR cells exhibited a significantly lower temperature than that of the corresponding measure thermocouple, which was yet located in or close to the sample bed. The comparison of Arrhenius plots enabled us to determine a temperature correction valid over a large temperature range. The use of an optical pyrometer was assessed with a view to determining the temperature of the surface of the powdered beds and that at the centre of the wafer. The optical pyrometer proved useful in the case of the catalyst powder, which behaved as a black non-reflecting body. In contrast, the temperature reading was inaccurate in the case of the pressed wafer, probably due to the shiny surface and minute thickness of the wafer, which led to a significant portion of the IR radiation of the surroundings being reflected by and transmitted through the wafer. The optical pyrometer data showed that the temperature of the surface of the powdered beds was significantly lower than that of the bulk of the bed, and that the total flow rate and composition did not affect this value. This work emphasises that the effective bed temperature in spectroscopic cells can be significantly different from that given by measure thermocouples, even when located in the vicinity of the sample, but that the calibration curves derived from rate measurements can be used to overcome this problem. The bulk and surface temperatures of sample beds of spectroscopic cells can be significantly lower than expected and can be derived from Arrhenius plots of model reactions and optical pyrometry.</description><subject>Catalysis</subject><subject>Chemical Sciences</subject><subject>Chemistry</subject><subject>Environment and Society</subject><subject>Environmental Sciences</subject><subject>Exact sciences and technology</subject><subject>General and physical chemistry</subject><subject>Theory of reactions, general kinetics. Catalysis. 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Catalysis. Nomenclature, chemical documentation, computer chemistry</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Li, Haoguang</creatorcontrib><creatorcontrib>Rivallan, Mickael</creatorcontrib><creatorcontrib>Thibault-Starzyk, Frederic</creatorcontrib><creatorcontrib>Travert, Arnaud</creatorcontrib><creatorcontrib>Meunier, Frederic C</creatorcontrib><collection>Pascal-Francis</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><collection>Hyper Article en Ligne (HAL)</collection><jtitle>Physical chemistry chemical physics : PCCP</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Li, Haoguang</au><au>Rivallan, Mickael</au><au>Thibault-Starzyk, Frederic</au><au>Travert, Arnaud</au><au>Meunier, Frederic C</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Effective bulk and surface temperatures of the catalyst bed of FT-IR cells used for in situ and operando studies</atitle><jtitle>Physical chemistry chemical physics : PCCP</jtitle><addtitle>Phys Chem Chem Phys</addtitle><date>2013-01-01</date><risdate>2013</risdate><volume>15</volume><issue>19</issue><spage>7321</spage><epage>7327</epage><pages>7321-7327</pages><issn>1463-9076</issn><eissn>1463-9084</eissn><abstract>The temperature prevailing in the catalyst bed of three different IR spectroscopic reaction cells was assessed by means of thermocouples, an optical pyrometer and reaction rate measurements. One of the cells was a custom-made transmission FT-IR cell for use with thin wafers and the two others were commercial Harrick and Spectra-Tech diffuse reflectance FT-IR (DRIFTS) cells used for the analysis of powdered samples. The rate of CO methanation measured over a 16 wt% Ni/alumina catalyst was used as a means to derive the effective temperature prevailing in the IR cells from that existing in a traditional (non-spectroscopic) reactor having a well-controlled temperature. The sample bed of these three IR cells exhibited a significantly lower temperature than that of the corresponding measure thermocouple, which was yet located in or close to the sample bed. The comparison of Arrhenius plots enabled us to determine a temperature correction valid over a large temperature range. The use of an optical pyrometer was assessed with a view to determining the temperature of the surface of the powdered beds and that at the centre of the wafer. The optical pyrometer proved useful in the case of the catalyst powder, which behaved as a black non-reflecting body. In contrast, the temperature reading was inaccurate in the case of the pressed wafer, probably due to the shiny surface and minute thickness of the wafer, which led to a significant portion of the IR radiation of the surroundings being reflected by and transmitted through the wafer. The optical pyrometer data showed that the temperature of the surface of the powdered beds was significantly lower than that of the bulk of the bed, and that the total flow rate and composition did not affect this value. This work emphasises that the effective bed temperature in spectroscopic cells can be significantly different from that given by measure thermocouples, even when located in the vicinity of the sample, but that the calibration curves derived from rate measurements can be used to overcome this problem. The bulk and surface temperatures of sample beds of spectroscopic cells can be significantly lower than expected and can be derived from Arrhenius plots of model reactions and optical pyrometry.</abstract><cop>Cambridge</cop><pub>Royal Society of Chemistry</pub><pmid>23576134</pmid><doi>10.1039/c3cp50442e</doi><tpages>7</tpages><orcidid>https://orcid.org/0000-0002-9579-8910</orcidid><orcidid>https://orcid.org/0000-0002-8095-0860</orcidid></addata></record>
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source Royal Society Of Chemistry Journals 2008-; Alma/SFX Local Collection
subjects Catalysis
Chemical Sciences
Chemistry
Environment and Society
Environmental Sciences
Exact sciences and technology
General and physical chemistry
Theory of reactions, general kinetics. Catalysis. Nomenclature, chemical documentation, computer chemistry
title Effective bulk and surface temperatures of the catalyst bed of FT-IR cells used for in situ and operando studies
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