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Pure Appl. Chem., 2012, Vol. 84, No. 1, pp. 107-136

Published online 2011-12-12


Liquid intrusion and alternative methods for the characterization of macroporous materials (IUPAC Technical Report)

Jean Rouquerol1*, Gino Baron2, Renaud Denoyel1, Herbert Giesche3, Johan Groen4, Peter Klobes5, Pierre Levitz6, Alexander V. Neimark7, Sean Rigby8, Romas Skudas9, Kenneth Sing10, Matthias Thommes11 and Klaus Unger9

1 LCP, CNRS-University Aix-Marseille, Marseille, France
2 Vrije Universiteit Brussels, Brussels, Belgium
3 NYSCC at Alfred University, Alfred, NY, USA
4 Delft Solids Solutions B.V., Delft, The Netherlands
5 BAM Bundesanstalt für Materialforschung und -prüfung, Berlin, Germany
6 Ecole Polytechnique, Palaiseau, France
7 Rutgers University, Piscataway, NJ, USA
8 Bath University, Bath, UK
9 Johannes Gutenberg University, Mainz, Germany
10 Brunel University, Uxbridge, UK
11 Quantachrome Instruments, Boynton Beach, FL, USA

Abstract: This document deals with the characterization of porous materials having pore widths in the macropore range of 50 nm to 500 μm. In recent years, the development of advanced adsorbents and catalysts (e.g., monoliths having hierarchical pore networks) has brought about a renewed interest in macropore structures. Mercury intrusion–extrusion porosimetry is a well-established method, which is at present the most widely used for determining the macropore size distribution. However, because of the reservations raised by the use of mercury, it is now evident that the principles involved in the application of mercury porosimetry require reappraisal and that alternative methods are worth being listed and evaluated. The reliability of mercury porosimetry is discussed in the first part of the report along with the conditions required for its safe use. Other procedures for macropore size analysis, which are critically examined, include the intrusion of other non-wetting liquids and certain wetting liquids, capillary condensation, liquid permeation, imaging, and image analysis. The statistical reconstruction of porous materials and the use of macroporous reference materials (RMs) are also examined. Finally, the future of macropore analysis is discussed.