Chapter 11
In Situ and Operando Techniques
in Catalyst Characterisation and Design
Przemysław Jodłowski and Joanna Łojewska
Abstract This chapter intends to present the classical and modern techniques that
are used for in situ characterisation of catalytic materials. Determination of the
structure of the catalyst presents three main problems: (1) heterogeneous catalysis
phenomena are limited to the outer surface of the material where the molecules
adsorb and react, and for this reason, there are only a few methods able to assess
catalyst surface structure and composition; (2) the catalyst surface under reaction
conditions and upon the influence of the reacting agents is different from that
occurring under ambient conditions, which limits the application of the analytical
methods to those which operate at normal or elevated pressures and high temperatures, (3) catalytic materials are complex and heterogeneous, so many analytical
methods, including surface imaging, should be employed in order to understand the
structure–activity relationships. The remedy for the problems is the application of
in situ analyses that rely on several complementary spectroscopic methods and
utilise surface sensitive probe molecules. Different kinds of probe molecules are
described: from universal probes to specific ones that enable the determination of
acidic and basic activity. The IR, Raman and UV-Vis methods are presented here
and described using examples from the literature. New trends in in situ experimentation involve time-resolved techniques for studying fast reactions, fluorescence
methods and coupled techniques for surface in situ imaging.
P. Jodłowski (&)
Faculty of Chemical Engineering and Technology, Cracow University
of Technology, Warszawska 24, 31-155 Kraków, Poland
e-mail: pjodlowski@pk.edu.pl
J. Łojewska
Faculty of Chemistry, Jagiellonian University, Gronostajowa 2,
30-387 Kraków, Poland
© Springer Nature Switzerland AG 2019
A. Koleżyński and M. Król (eds.), Molecular Spectroscopy—Experiment
and Theory, Challenges and Advances in Computational Chemistry
and Physics 26, https://doi.org/10.1007/978-3-030-01355-4_11
333
In Situ and Operando Techniques
in Catalyst Characterisation and Design
Przemysław Jodłowski and Joanna Łojewska
Abstract This chapter intends to present the classical and modern techniques that
are used for in situ characterisation of catalytic materials. Determination of the
structure of the catalyst presents three main problems: (1) heterogeneous catalysis
phenomena are limited to the outer surface of the material where the molecules
adsorb and react, and for this reason, there are only a few methods able to assess
catalyst surface structure and composition; (2) the catalyst surface under reaction
conditions and upon the influence of the reacting agents is different from that
occurring under ambient conditions, which limits the application of the analytical
methods to those which operate at normal or elevated pressures and high temperatures, (3) catalytic materials are complex and heterogeneous, so many analytical
methods, including surface imaging, should be employed in order to understand the
structure–activity relationships. The remedy for the problems is the application of
in situ analyses that rely on several complementary spectroscopic methods and
utilise surface sensitive probe molecules. Different kinds of probe molecules are
described: from universal probes to specific ones that enable the determination of
acidic and basic activity. The IR, Raman and UV-Vis methods are presented here
and described using examples from the literature. New trends in in situ experimentation involve time-resolved techniques for studying fast reactions, fluorescence
methods and coupled techniques for surface in situ imaging.
P. Jodłowski (&)
Faculty of Chemical Engineering and Technology, Cracow University
of Technology, Warszawska 24, 31-155 Kraków, Poland
e-mail: pjodlowski@pk.edu.pl
J. Łojewska
Faculty of Chemistry, Jagiellonian University, Gronostajowa 2,
30-387 Kraków, Poland
© Springer Nature Switzerland AG 2019
A. Koleżyński and M. Król (eds.), Molecular Spectroscopy—Experiment
and Theory, Challenges and Advances in Computational Chemistry
and Physics 26, https://doi.org/10.1007/978-3-030-01355-4_11
333