Abstract
A recently developed dynamic desorption technique is used for obtaining vapor isotherms on porous materials. This gravimetric technique does not require any preliminary calibration and is based on analyzing the kinetics of liquid evaporation from a porous sample under quasi-steady state conditions. The crucial feature of the technique is concerned with the fact that no vapor pressure measurements are necessary. The technique is illustrated by desorption of benzene vapors from mesoporous silica MCM-41. To calculate the pore size distribution, the Derjaguin–Broekhoff–de Boer theory in its combination with the Wheeler model for capillary condensation is used. In the calculations, the reference data on benzene adsorption on a nonporous silica gel from two different sources (published by different authors) are applied. The mean mesopore sizes estimated from desorption isotherms are shown to be in a fair agreement with the calculations through the geometrical method based on the X-ray diffraction data. The dynamic desorption technique can serve as an additional tool for the characterization of a porous media.
Article PDF
Similar content being viewed by others
Avoid common mistakes on your manuscript.
References
Asefa, T., Duncan, C.T., Sharma, K.K.: Recent advances in nanostructured chemosensors and biosensors. Analyst 134, 1980–1990 (2009)
Beck, J.S., Vartuli, J.C., Roth, W.J., Leonowicz, M.E., Kresge, C.T., Schmitt, K.D., Chu, C.T.-W., Olson, D.H., Sheppard, E.W., McCullen, S.B., Higgins, J.B., Schlenker, J.L.: A new family of mesoporous molecular sieves prepared with liquid crystal templates. J. Am. Chem. Soc. 114, 10834–10843 (1992)
Beverley, K.J., Clint, J.H., Fletcher, P.D.I.: Evaporation rates of pure liquids measured using a gravimetric technique. Phys. Chem. Chem. Phys. 1, 149–153 (1999a)
Beverley, K.J., Clint, J.H., Fletcher, P.D.I., Thubron, S.: Evaporation rates of water contained within porous silica particles. Phys. Chem. Chem. Phys. 1, 909–911 (1999b)
Bird, R.B., Stewart, W.E., Lightfoot, E.N.: Transport Phenomena. Wiley, New York (1960)
Broekhoff, J.C.P., de Boer, J.H.: Studies on pore systems in catalysts. IX. Calculation of pore distributions from the adsorption branch of nitrogen sorption isotherms in the case of open cylindrical pores. A. Fundamental equations. J. Catal. 9, 8–14 (1967)
Broekhoff, J.C.P., de Boer, J.H.: Studies on pore systems in catalysts. XIII. Pore distributions from the desorption branch of a nitrogen sorption isotherms in the case of cylindrical pores. B. Applications. J. Catal. 10, 377–390 (1968)
Choma, J., Kloske, M., Jaroniec, M., Klinik, J.: Benzene adsorption isotherms on MCM-41 and their use for pore size analysis. Adsorption 10, 195–203 (2004)
Derjaguin, B.V.: Correct form of the equation of capillary condensation in porous bodies. In: Proc. Intern. Congr. Surface Activity, 2nd edn. London, vol. 2, pp. 153–159 (1957)
Dubinin, M.M.: Capillary effects and information concerning adsorbent pore structures. 3. Refinement of the theory of capillary vaporization from adsorbent mesopores. Russ. Chem. Bull. 29, 15–18 (1980)
Gregg, S.J., Sing, K.S.W.: Adsorption, Surface Area and Porosity, 2nd edn. Academic Press, New York (1982)
Isirikyan, A.A.: Dissertation. Moscow State University, Moscow (1957) (in Russian)
Isirikyan, A.A., Kiselev, A.V.: The heat of adsorption of benzene and hexane vapors on quartz. Dokl. Akad. Nauk USSR (Phys. Chem.), 119, 731–734 (1958) (in Russian)
Lukens, W.W. Jr., Schmidt-Winkel, P., Zhao, D., Feng, J., Stucky, G.D.: Evaluating pore sizes in mesoporous materials: a simplified standard adsorption method and a simplified Broekhoff-de Boer method. Langmuir 15, 5403–5409 (1999)
Klotz, M., Ayral, A., Guizard, C., Cot, L.: Synthesis conditions for hexagonal mesoporous silica layers. J. Mater. Chem. 10, 663–669 (2000)
Klotz, M., Ayral, A., Guizard, C., Cot, L.: Synthesis and characterization of silica membranes exhibiting an ordered mesoporosity. Control of the porous texture and effect on the membrane permeability. Separation/Purification Technol. 25, 71–78 (2001)
Kowalczyk, P., Jaroniec, M., Terzyk, A.P., Kaneko, K., Do, D.D.: Improvement of the Derjaguin–Broekhoff–de Boer theory for capillary condensation/evaporation of nitrogen in mesoporous systems and its implications for pore size analysis of MCM-41 silicas and related materials. Langmuir 21, 1827–1833 (2005)
Kruk, M., Jaroniec, M., Sayari, A.: Relations between pore structure parameters and their implications for characterization of MCM-41 using gas adsorption and X-ray diffraction. Chem. Mater. 11, 492–500 (1999)
Morishige, K., Tateishi, M.: Accurate relations between pore size and the pressure of capillary condensation and the evaporation of nitrogen in cylindrical pores. Langmuir 22, 4165–4169 (2006)
Naono, H., Hakuman, M., Nakai, K.: Determination of pore size distribution of mesoporous and macroporous silicas by means of benzene-desorption isotherms. J. Colloid Interface Sci. 165, 532–535 (1994)
Nguyen, C., Do, D.D.: Sizing of cylindrical pores by nitrogen and benzene vapor adsorption. J. Phys. Chem. B 104, 11435–11439 (2000)
Qiao, S.Z., Bhatia, S.K., Nicholson, D.: Study of hexane adsorption in nanoporous MCM-41 silica. Langmuir 20, 389–395 (2004)
Rouessac, V., van der Lee, A., Bosc, F., Durand, J., Ayral, A.: Three characterization techniques coupled with adsorption for studying the nanoporosity of supported films and membranes. Microporous Mesoporous Mater. 111, 417–428 (2008)
Selvam, P., Bhatia, S.K., Sonwane, C.G.: Recent advances in processing and characterization of periodic mesoporous MCM-41 silicate molecular sieves. Ind. Eng. Chem. Res. 40, 3237–3261 (2001)
Shkol’nikov, E.I., Volkov, V.V.: Dynamic desorption porometry: a new method for the analysis of membrane porous structure. In: Proc. Intern. Symp. “Euromembrane 99”, Leuven, Belgium, September, 19–22, vol. 2, pp. 482 (1999)
Shkol’nikov, E.I., Volkov, V.V.: Obtaining vapor desorption isotherms without monitoring pressure. Dokl., Phys. Chem. 378, 152–155 (2001)
Staszczuk, P., Nasuto, R., Rudy, S.: Studies of benzene adsorption layers on silica gels by thermal analysis and McBain balance methods. J. Therm. Anal. Calorim. 62, 461–468 (2000)
Ustinov, E.A., Do, D.D., Jaroniec, M.: Equilibrium adsorption in cylindrical mesopores: a modified Broekhoff and de Boer theory versus density functional theory. J. Phys. Chem. B 109, 1947–1958 (2005)
Wheeler, A.: Reaction rates and selectivity in catalyst pores. In: Emmett, P.H. (eds.) Catalysis, vol. 2, pp. 105–165. Reinhold, New York (1955)
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Shkolnikov, E.I., Sidorova, E.V., Malakhov, A.O. et al. Estimation of pore size distribution in MCM-41-type silica using a simple desorption technique. Adsorption 17, 911–918 (2011). https://doi.org/10.1007/s10450-011-9368-9
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10450-011-9368-9