Abstract
Optical calorimetry is a powerful technique for the characterization of porous materials within only a few minutes (e.g. specific surface area, adsorption capacity). In the current work, optical calorimetry is presented to be a versatile tool for the pore size characterization of activated carbons. Therefore, measurements were performed with six different test gases (N2O, C2H6, C3H8, n-C4H10, i-C4H10, SF6) in the optical calorimeter InfraSORP at ambient conditions. By combining the results of optical calorimetric measurement for each adsorptive, a pore size distribution (PSD) can be estimated in the range of 0.4–6 nm which is in accurate accordance with the PSD of reference CO2 (273 K) and N2 (77 K) physisorption experiments. While common physisorption experiments can easily take a few days, the PSD by using the optical calorimetric screening is obtained within roughly 1 h.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
Böhringer, B., Guerra Gonzalez, O., Eckle, I., Müller, M., Giebelhausen, J.-M., Schrage, C., Fichtner, S.: Polymer-based spherical activated carbons—from adsorptive properties to filter performance. Chem. Ing. Tech. 83, 53–60 (2011)
Bon, V., Kavoosi, N., Senkovska, I., Kaskel, S.: Tolerance of flexible MOFs toward repeated adsorption stress. ACS Appl. Mater. Interfaces. 7, 22292–22300 (2015)
Cao, D., Sircar, S.: Heat of adsorption of pure sulfur hexafluoride on micro-mesoporous adsorbents. Adsorption 7, 73–80 (2001)
Cao, X.L., Colenutt, B.A., Sing, K.S.W.: Study of microporous carbons by gas chromatographic determination of heats of physisorption. J. Chromatogr. A. 555, 183–190 (1991)
Denoyel, R., Fernandez-Colinas, J., Grillet, Y., Rouquerol, J.: Assessment of the surface area and microporosity of activated charcoals from immersion calorimetry and nitrogen adsorption data. Langmuir 9, 515–518 (1993)
Ferreira, A.F.P., Mittelmeijer-Hazeleger, M.C., Bliek, A.: Adsorption and differential heats of adsorption of normal and iso-butane on zeolite MFI. Microporous Mesoporous Mater. 91, 47–52 (2006)
Hartmann, M., Kunz, S., Himsl, D., Tangermann, O., Ernst, S., Wagener, A.: Adsorptive separation of isobutene and isobutane on Cu3(BTC)2. Langmuir 24, 8634–8642 (2008)
Kulprathipanja, S.: Zeolites in Industrial Separation and Catalysis. Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim (2010)
Leistner, M., Grählert, W., Kaskel, S.: Screening of porous materials by thermal response measurements. Chem. Ing. Tech. 85, 747–752 (2013)
Li, J.-R., Kuppler, R.J., Zhou, H.-C.: Selective gas adsorption and separation in metal–organic frameworks. Chem. Soc. Rev. 38, 1477–1504 (2009)
Li, Z.J., Jin, S.L., Zhan, S.M., Jiang, N., Shao, X., Jin, M.L., Zhang, R.: Dibenzothiophene adsorption on activated carbons and its water effect. In: Hu, J.W. (ed.) Advanced materials and structural engineering, pp. 57–61. Taylor & Francis Group, London (2016)
Morris, R.E., Wheatley, P.S.: Gas storage in nanoporous materials. Angew. Chem. Int. Ed. Engl. 47, 4966–4981 (2008)
Oschatz, M., Leistner, M., Nickel, W., Kaskel, S.: Advanced structural analysis of nanoporous materials by thermal response measurements. Langmuir 31, 4040–4047 (2015)
Peng, Y., Zhang, F., Xu, C., Xiao, Q., Zhong, Y., Zhu, W.: Adsorption of nitrous oxide on activated carbons. J. Chem. Eng. Data. 54, 3079–3081 (2009)
Sandra, F., Klein, N., Leistner, M., Lohe, M.R., Benusch, M., Woellner, M., Grothe, J., Kaskel, S.: Speeding up chemisorption analysis by direct IR-heat-release measurements (infrasorp technology): a screening alternative to breakthrough measurements. Ind. Eng. Chem. Res. 54, 6677–6682 (2015)
Silvestre-Albero, J.: Characterization of microporous solids by immersion calorimetry. Colloids Surf. A 188, 151–165 (2001)
Sircar, S., Golden, T.C., Rao, M.B.: Activated carbon for gas separation and storage. Carbon. 34, 1–12 (1996)
Stoeckli, F., Centeno, T.A.: On the characterization of microporous carbons by immersion calorimetry alone. Carbon 35, 1097–1100 (1997)
Walton, K.S., Cavalcante, C.L. Jr., Douglas Levan, M.: Adsorption of light alkanes on coconut nanoporous activated carbon. Braz. J. Chem. Eng. 23, 555–561 (2006)
Wollmann, P., Leistner, M., Stoeck, U., Grünker, R., Gedrich, K., Klein, N., Throl, O., Grählert, W., Senkovska, I., Dreisbach, F., Kaskel, S.: High-throughput screening: speeding up porous materials discovery. Chem. Commun. 47, 5151–5153 (2011)
Wollmann, P., Leistner, M., Grählert, W., Throl, O., Dreisbach, F., Kaskel, S.: Infrasorb: optical detection of the heat of adsorption for high throughput adsorption screening of porous solids. Microporous Mesoporous Mater. 149, 86–94 (2012)
Zhu, W., Groen, J.C., Miltenburg, A., Kapteijn, F., Moulijn, J.A.: Comparison of adsorption behaviour of light alkanes and alkenes on kureha activated carbon. Carbon 43, 1416–1423 (2005)
Acknowledgements
This research did not receive any specific grant from funding agencies in the public, commercial, or not-for-profit sectors. Dr. Martin Oschatz and M. Sc. Winfried Nickel (TU Dresden) are kindly acknowledged for support during the physisorption experiments.
Author information
Authors and Affiliations
Corresponding author
Electronic supplementary material
Below is the link to the electronic supplementary material.
Rights and permissions
About this article
Cite this article
Wöllner, M., Leistner, M., Wollmann, P. et al. Estimating pore size distributions of activated carbons via optical calorimetry. Adsorption 23, 313–320 (2017). https://doi.org/10.1007/s10450-016-9852-3
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10450-016-9852-3