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Characterization of catalysts in their active state by adsorption microcalorimetry: Experimental design and application to sulfated zirconia

MPS-Authors
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Wrabetz,  Sabine
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Yang,  Xiaobo
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Tzolova-Müller,  Genka
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Schlögl,  Robert
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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Jentoft,  Friederike C.
Inorganic Chemistry, Fritz Haber Institute, Max Planck Society;

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(Preprint), 304KB

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Citation

Wrabetz, S., Yang, X., Tzolova-Müller, G., Schlögl, R., & Jentoft, F. C. (2010). Characterization of catalysts in their active state by adsorption microcalorimetry: Experimental design and application to sulfated zirconia. Journal of Catalysis, 269(2), 351-358. Retrieved from http://dx.doi.org/10.1016/j.jcat.2009.11.018.


Cite as: http://hdl.handle.net/11858/00-001M-0000-0010-F653-B
Abstract
A method to characterize the surface sites of catalysts in their active state by adsorption microcalorimetry was developed. A calorimeter cell was used as a flow-type reactor, and the skeletal isomerization of n-butane (1 kPa) at 378 K and atmospheric pressure proceeded at comparable rates and with the same states of induction period, maximum and deactivation phase as in a tubular reactor. The reaction was run for selected times on stream and after removal of weakly adsorbed species, n-butane or isobutane were adsorbed at 313 K. The surface of activated sulfated zirconia was characterized by at least two different sites for n-butane adsorption, a small group of sites (about 20 µmol g-1) that yielded heats of 5060 kJ mol-1 and sites that were populated at higher pressures (above about 5 hPa n-butane) and yielded heats of about 40 kJ mol-1. The strongly interacting sites disappear during the induction period and are proposed to be the sites where the isomerization reaction is initiated.