Hostname: page-component-586b7cd67f-vdxz6 Total loading time: 0 Render date: 2024-11-26T14:00:20.819Z Has data issue: false hasContentIssue false

Analyzing Expanding Clays by Thermoporometry Using a Stochastic Deconvolution of the DSC Signal

Published online by Cambridge University Press:  01 January 2024

Tomasz Kozlowski*
Affiliation:
Kielce University of Technology, Al. Tysiąclecia Państwa Polskiego 7, 25-314, Kielce, Poland
Łukasz Walaszczyk
Affiliation:
Kielce University of Technology, Al. Tysiąclecia Państwa Polskiego 7, 25-314, Kielce, Poland
*
*E-mail address of corresponding author: [email protected]
Rights & Permissions [Opens in a new window]

Abstract

Core share and HTML view are not available for this content. However, as you have access to this content, a full PDF is available via the ‘Save PDF’ action button.

A version of thermoporometry dedicated to analyzing the pore network of expanding clays is proposed here. The blurred, wide Differential Scanning Calorimetry (DSC) peak obtained upon the melting of a frozen clay sample is processed by means of a deconvolution analysis based on searching for such a temperature distribution of “pulse-like heat events” which, convolved with the apparatus function, gives a minimal deviation from the observed heat flux function, i.e. the calorimetric signal. As a result, a sharp thermogram was obtained which can be transformed easily into the pore-size distribution curve. Results obtained for samples of two Clay Minerals Society Source Clays (montmorillonites SWy-2 from Wyoming and STx-1b from Texas) at different water contents indicate a greater resolution and sensitivity than that achieved by classical thermoporometry using the unprocessed DSC signal. Phenomena corresponding to the evolution of the pore network as a function of the water content have been detected in samples with large water contents subjected to free drying prior to the experiments.

Type
Article
Copyright
Copyright © Clay Minerals Society 2014

References

Alba-Simionesco, C. Coasne, B. Dosseh, G. Dudziak, G. Gubbins, K.E. Radhakrishnan, R. and Sliwinska-Bartkowiak, M., 2006 Effects of confinement on freezing and melting Journal of Physics: Condensed Matter 18 R15R68.Google ScholarPubMed
Bergaya, F. and Lagaly, G., 2001 Surface modification of clay minerals Applied Clay Science 19 130.CrossRefGoogle Scholar
Beurroies, I. Denoyel, R. Llewellyn, P. and Rouquerol, J., 2004 A comparison between melting-solidification and capillary condensation hysteresis in mesoporous materials: application to the interpretation of thermoporometry data Thermochimica Acta 421 1118.CrossRefGoogle Scholar
Bogdan, A. and Kulmala, M., 1997 DSC study of the freezing and thawing behavior of pure water and binary H2O/HNO3 and H2O/HCl systems adsorbed by pyrogenic silica: implications for the atmosphere Journal of Aerosol Science 28 Suppl.1 S507S508.CrossRefGoogle Scholar
Brun, M. Lallemand, A. Quinson, J.-F. and Eyraud, C.h., 1977 A new method for the simultaneous determination of the size and the shape of pores: the thermoporometry Thermochimica Acta 21 5988.CrossRefGoogle Scholar
Carrado, K.A. and Komadel, P., 2009 Acid activation of bentonites and polymer-clay nanocomposites Elements 5 111116.CrossRefGoogle Scholar
Dogan, A.U. Dogan, M. Onal, M. Sarikaya, Y. Aburub, A. and Wurster, D.E., 2006 Baseline studies of the Clay Minerals Society Source Clays: Specific Surface Area by Brunauer Emmett Teller (BET) method Clays and Clay Minerals 54 6266.CrossRefGoogle Scholar
Dogan, M. Dogan, A.U. Yesilyurt, F.I. Alaygut, D. Buckner, I. and Wurster, D.E., 2007 Baseline studies of the Clay Minerals Society Special Clays: Specific Surface Area by Brunauer Emmett Teller (BET) method Clays and Clay Minerals 55 534541.CrossRefGoogle Scholar
Efimov, S.S., 1986 Temperature dependence of the heat of crystallization of water Journal of Engineering Physics and Thermophysics 49 12291233.CrossRefGoogle Scholar
Fabbri, A. Fen-Chong, T. and Coussy, O., 2006 Dielectric capacity, liquid water content, and pore structure of thawing-freezing materials Cold Regions Science and Technology 44 5266.CrossRefGoogle Scholar
Fung, CAFK and Burke, M.F., 1996 Investigation of the behaviour of water on the surface of modified silica using differential scanning calorimetry Journal of Chromatography A 752 4157.CrossRefGoogle Scholar
Gates, W. Bouazza, M. and Churchman, G., 2009 Bentonite clay keeps pollutants at bay Elements 5 105110.CrossRefGoogle Scholar
Höhne, G.W.H. Hemminger, W.F. and Flammersheim, H.-J., 2003 Differential Scanning Calorimetry Berlin, Heidelberg, New York Springer-Verlag.CrossRefGoogle Scholar
Homshaw, L.G., 1980 Freezing and melting temperature hysteresis of water in porous materials: Application to the study of pore form European Journal of Soil Science 31 399414.CrossRefGoogle Scholar
Homshaw, L.G. and Cambier, P., 1980 Wet and dry pore size distribution in a kaolinitic soil before and after removal of iron and quartz European Journal of Soil Science 31 415428.CrossRefGoogle Scholar
Horiguchi, K., 1985 Determination of unfrozen water content by DSC Proceedings of the 4thInternational Symposium on Ground Freezing, Sapporo, Japan, Vol. 1 Rotterdam A.A. Balkema 3338.Google Scholar
Ishikiriyama, K. Todoki, M. Min, K.H. Yonemori, S. and Noshiro, M., 1996 Thermoporosimetry: Pore size distribution measurements for microporous glass using differential scanning calorimetry Journal of Thermal Analysis 46 11771189.CrossRefGoogle Scholar
Iza, M. Woerly, S. Danumah, C. Kaliaguine, S. and Bousmina, M., 2000 Determination of pore size distribution for mesoporous materials and polymeric gels by means of DSC measurements: thermoporometry Polymer 41 58855893.CrossRefGoogle Scholar
Kaneko, K., 1994 Determination of pore size and pore size distribution: 1. Adsorbents and catalysts Journal of Membrane Science 96 5989.CrossRefGoogle Scholar
Montes, G. Duplay, J. Martinez, L. and Mendoza, C., 2003 Swelling-shrinkage kinetics of MX80 bentonite Applied Clay Science 22 279293.CrossRefGoogle Scholar
Neffati, R. and Rault, J., 2001 Pore size distribution in porous glass: fractal dimension obtained by calorimetry The European Physical Journal B 21 205210.CrossRefGoogle Scholar
Nevzorov, A.N., 2006 Internal mechanism of metastable liquid water crystallization and its effects on intracloud processes Izvestiya AtmosphericandOceanicPhysics 42, 765772.Google Scholar
Opitz, A. Scherge, M. Ahmed, SI-U and Schaefer, J.A., 2007 A comparative investigation of thickness measurements of ultra-thin water films by scanning probe techniques Journal of Applied Physics 101 6064310.CrossRefGoogle Scholar
Price, D.M. and Bashir, Z., 1995 A study of the porosity of water plasticised polyacrylonitrile films by thermal analysis and microscopy Thermochimica Acta 249 351366.CrossRefGoogle Scholar
Ravikovitch, P. Wei, D. Chueh, W.T. Haller, G.L. and Neimark, A.V., 1997 Evaluation of pore structure parameters of MCM-41 catalyst supports and catalysts by means of nitrogen and argon adsorption Journal of Physical Chemistry 101 36713679.CrossRefGoogle Scholar
Rigacci, A. Achard, P. Ehrburger-Dolle, F. and Pirard, R., 1998 Structural investigation in monolithic silica aerogels and thermal properties Journal of Non-Crystalline Solids 225 260265.CrossRefGoogle Scholar
Rouquerol, J. Avnir, D. Fairbridge, C.W. Everett, D.H. Haynes, J.M. Pernicone, N. Ramsay, J.D.F. Sing, K.S.W. and Unger, K.K., 1994 Recommendations for the characterization of porous solids (Technical Report) Pure and Applied Chemistry 66 17391758.CrossRefGoogle Scholar
Salles, F. Beurroies, I. Bildstein, O. Jullien, M. Raynal, J. Denoyel, R. and Van Damme, H., 2008 A calorimetric study of mesoscopic swelling and hydration sequence in solid Na-montmorillonite Applied Clay Science 39 186201.CrossRefGoogle Scholar
Stepkowska, E.T. Pérez-Rodríguez, J.L. Maqueda, C. and Starnawska, E., 2004 Variability in water sorption and in particle thickness of standard smectites Applied Clay Science 24 185199.CrossRefGoogle Scholar
Swenson, J. Elamin, K. Jansson, H. and Kittaka, S., 2013 Why is there no clear glass transition of confined water? Chemical Physics 424 2025.CrossRefGoogle Scholar
Titulaer, M.K. Van Miltenburg, J.C. Jansen, J.B.H. and Geus, J.W., 1995 Thermoporometry applied to hydrothermally aged silica hydrogels Recueil Des Travaux Chimiques Des Pays Bas 114 361370.CrossRefGoogle Scholar
Torralvo, M.J. Grillet, Y. Llewellyn, P.L. and Rouquerol, F., 1998 Microcalorimetric study of argon, nitrogen, and carbon monoxide adsorption on mesoporous Vycor glass Journal of Colloid and Interface Science 206 527531.CrossRefGoogle ScholarPubMed
Turov, V.V. and Leboda, R., 1999 Application of 1H NMR spectroscopy method for determination of characteristics of thin layers of water adsorbed on the surface of dispersed and porous adsorbents Advances in Colloid and Interface Science 79 173211.CrossRefGoogle ScholarPubMed
Velde, B. Moreau, E. and Terribile, F., 1996 Pore networks in an Italian vertisol: quantitative characterization by two dimensional image analysis Geoderma 72 271285.CrossRefGoogle Scholar
Yang, T. Xiao-Dong, W. Junfen, L. and Liming, Y., 2006 Theoretical and experimental investigations on the structures of purified clay and acid-activated clay Applied Surface Science 252 61546161.CrossRefGoogle Scholar
Zuber, B. and Marchand, J., 2000 Modeling the deterioration of hydrated cement systems exposed to frost action. Part 1: Description of the mathematical model Cement and Concrete Research 30 19291939.CrossRefGoogle Scholar