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Determination of basic sites in Mg–Al mixed oxides by combination of TPD-CO2 and CO2 adsorption calorimetry

When the same basic sites are reported from both techniques?

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Abstract

We present the critical analysis of the utilization of CO2 adsorption calorimetry/volumetry and TPD-CO2 for the determination of the Mg–Al mixed oxide basicity. The aim of work is the description and the evaluation of both methods with respect to the fact when the same types of CO2 adsorption complexes are involved. Critical parts of basic sites determination are originally discussed for both methods. In TPD-CO2, the process of the purging of non-specifically physisorbed CO2 is stressed. In CO2 adsorption calorimetry, the differential heat of CO2 distinguishing CO2 adsorption on weak basic sites and non-specific CO2 physisorption is stressed. Both methods are applied on series of selected Mg/Al mixed oxides varying in Mg/Al molar ratio and alkali co-cation. We show that the generally used TPD-CO2 does not provide complete information about basic sites since some weak sites form unstable CO2 species and these species could not be involved in TPD experiments. All our TPD-CO2 experiments reflect at 0–485 °C those CO2 adsorbed in the range of the differential heat of CO2 above 30–32 kJ mol−1.

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Acknowledgements

The authors gratefully thank to the Czech Science Foundation (Project No. GA15-21817S).

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Authors and Affiliations

  1. Department of Physical Chemistry, Faculty of Chemical Technology, University of Pardubice, Studentská 573, 532 10, Pardubice, Czech Republic

    Lucie Smoláková, Karel Frolich, Ivana Troppová, Petr Kutálek, Eva Kroft & Libor Čapek

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  1. Lucie Smoláková
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Correspondence to Libor Čapek.

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Smoláková, L., Frolich, K., Troppová, I. et al. Determination of basic sites in Mg–Al mixed oxides by combination of TPD-CO2 and CO2 adsorption calorimetry. J Therm Anal Calorim 127, 1921–1929 (2017). https://doi.org/10.1007/s10973-016-5851-6

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