Struct Bond (2020) 184: 31–56
https://doi.org/10.1007/430_2020_69
# Springer Nature Switzerland AG 2020
Published online: 24 October 2020
Critical Overview of Textural
Characterization of Zeolites by Gas
Adsorption
Jhonny Villarroel-Rocha, Deicy Barrera, José J. Arroyo-Gómez, and
Karim Sapag
Contents
1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
2 Gas Adsorption: Basic Principles and Experimental Considerations . . . . . . . . . . . . . . . . . . . . . . . . 34
2.1 Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
2.2 Sample Pretreatment . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . 35
2.3 Choice of Adsorptive Gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
3 Textural Properties Analysis . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . 39
3.1 Specific Surface Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
3.2 Pore Volume . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
3.3 Pore Size Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
4 Conclusions and Final Remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
Abstract Porous materials with pores within molecular size are essential to solve
several technological problems taking advantage of their textural properties related
to their exposed surface and porosity. Among these materials, zeolites are in the
podium, with technological and industrial applications, which are directly related to
pore properties (e.g., size, surface chemistry, among others). To obtain their textural
properties, there are several techniques, but gas adsorption plays an important role,
and it is among the most widely used for this purpose. Despite being a popular
technique, with nitrogen at 77 K as the reference probe molecule to obtain adsorption
isotherms, the estimation of the textural properties is not a trivial procedure. On the
other hand, it is possible to perform adsorption measurements with different gases at
different temperatures and pressures, whereby is crucial the choice of adequate
J. Villarroel-Rocha, D. Barrera, J. J. Arroyo-Gómez, and K. Sapag (*)
Laboratorio de Sólidos Porosos (LabSoP), Departamento de Física, INFAP-CONICET,
Universidad Nacional de San Luis, San Luis, Argentina
e-mail: jhonny@unsl.edu.ar; deicybarrera@unsl.edu.ar; jarroyo@unsl.edu.ar; sapag@unsl.edu.ar
https://doi.org/10.1007/430_2020_69
# Springer Nature Switzerland AG 2020
Published online: 24 October 2020
Critical Overview of Textural
Characterization of Zeolites by Gas
Adsorption
Jhonny Villarroel-Rocha, Deicy Barrera, José J. Arroyo-Gómez, and
Karim Sapag
Contents
1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
2 Gas Adsorption: Basic Principles and Experimental Considerations . . . . . . . . . . . . . . . . . . . . . . . . 34
2.1 Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
2.2 Sample Pretreatment . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . 35
2.3 Choice of Adsorptive Gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
3 Textural Properties Analysis . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . 39
3.1 Specific Surface Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
3.2 Pore Volume . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
3.3 Pore Size Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
4 Conclusions and Final Remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
Abstract Porous materials with pores within molecular size are essential to solve
several technological problems taking advantage of their textural properties related
to their exposed surface and porosity. Among these materials, zeolites are in the
podium, with technological and industrial applications, which are directly related to
pore properties (e.g., size, surface chemistry, among others). To obtain their textural
properties, there are several techniques, but gas adsorption plays an important role,
and it is among the most widely used for this purpose. Despite being a popular
technique, with nitrogen at 77 K as the reference probe molecule to obtain adsorption
isotherms, the estimation of the textural properties is not a trivial procedure. On the
other hand, it is possible to perform adsorption measurements with different gases at
different temperatures and pressures, whereby is crucial the choice of adequate
J. Villarroel-Rocha, D. Barrera, J. J. Arroyo-Gómez, and K. Sapag (*)
Laboratorio de Sólidos Porosos (LabSoP), Departamento de Física, INFAP-CONICET,
Universidad Nacional de San Luis, San Luis, Argentina
e-mail: jhonny@unsl.edu.ar; deicybarrera@unsl.edu.ar; jarroyo@unsl.edu.ar; sapag@unsl.edu.ar