Abstract
The hydration of Portland cement incorporates chemically bound water (CBW) into the structure of the formed hydrates and keeps water adsorbed on their surface, especially in calcium silicate hydrate (C-S-H). The evolution of hydration gradually reduces the porosity of the paste, keeping water remaining in the pores. Determining the volume of voids contained in the solid requires the removal of non-constitutive water from the hydrates without significant degradation of the microstructure. The free water withdrawal is performed by different methods, but some impact the adsorbed water (gel water) and also the chemically bound water. In this situation, partial degradation of hydrates interferes with the porosity of the paste and the estimation of the degree of hydration. This work determined the apparent porosity and compressive strength of Portland cement paste type CP V – ARI (high early strength cement) and CP II – Z (cement with pozzolan), molded with water/cement ratio of 0.35; 0.45 and 0.55 at the ages of 7, 28 and 56 days. The removal of free water contained in the pores of the pastes was performed by the following methods: oven drying, solvent exchange, and lyophilization (freeze-drying). The apparent porosity results were influenced by the drying methods, especially when the samples were submitted to a temperature of 105 °C. Oven drying results in apparent porosity significantly higher than those determined by solvent exchange or lyophilization. This method causes desaturation, desorption, and partial dehydration in the paste. The degradation of hydrated compounds can be in the order of 10%. The porosities obtained in the solvent exchange and lyophilization were similar, showing the potential of immersion in alcohol for drying samples. These methods promote the desaturation of the paste, keeping gel water and CBW in the hydrated compounds.
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References
Collier NC, Sharp JH, Milestone NB, Hill J, Godfrey IH (2008) The influence of water removal techniques on the composition and microstructure of hardened cement pastes. Cem Concr Res 38(6) 737–744. https://doi.org/10.1016/j.cemconres.2008.02.012
Knapen E, Cizer O, Van Balen K, Van Gemert D (2009) Effect of free water removal from early-age hydrated cement pastes on thermal analysis. Constr Build Mater 23(11):3431–3438. https://doi.org/10.1016/j.conbuildmat.2009.06.004
Askushaj D, Mulaj T (2016) The influence of solvent exchange on porosity of cement pastes identified by mercury intrusion porosimetry. J Multidisciplin Eng Sci Technol 3(12): 6281–6284
Cabrera J, Rojas MF (2001) Mechanism of hydration of the metakaolin-lime-water system. Cement Concrete Res 31(2): 177–182. https://doi.org/10.1016/S0008-8846(00)00456-7
Maciel MH, Soares GS, Romano RCO, Cincotto MA (May 2019) Monitoring of Portland cement chemical reaction and quantification of the hydrated products by XRD and TG in function of the stoppage hydration technique. J Therm Anal Calorim 136(3):1269–1284. https://doi.org/10.1007/s10973-018-7734-5
Pane I, Hansen W (2005) Investigation of blended cement hydration by isothermal calorimetry and thermal analysis. Concrete Cement Res 35(6): 1155–1164. https://doi.org/10.1016/j.cemconres.2004.10.027
Snellings R, Chwast J, Cizer Ö, De Belie N, Dhandapani Y, Durdzinski P, Elsen J, Haufe J, Hooton D, Patapy C, Santhanam M, Scrivener K, Snoeck D, Steger L, Tongbo S, Vollpracht A, Winnefeld F, Lothenbach B (2018) Report of TC 238-SCM: hydration stoppage methods for phase assemblage studies of blended cements – results of a round robin test. Mater Struct 51:111. https://doi.org/10.1617/s11527-018-1237-5
Zhang L, Glasser FP (2000) Critical examination of drying damage to cement pastes. Adv Cem Res 12(2):79–88. https://doi.org/10.1680/adcr.2000.12.2.79
Zhang J, Scherer W (2011) Comparison of methods for arresting hydration of cement. Cem Concr Res 41(10):1024–1036. https://doi.org/10.1016/j.cemconres.2011.06.003
Snoeck D, Velasco LF, Mignon A, Van Vlierberghe S, Dubruel P, Lodewyckx P; De Belie N (2014) The influence of different drying techniques on the water sorption properties of cement-based materials. Cem Concr Res 64(1): 54–62
Galle C (2001) Effect of drying on cement-based materials pore structure as identified by mercury intrusion porosimetry. A comparative study between oven-, vacuum-, and freeze-drying. Cem Concr Res 31(10): 1467–1477
Konecny L, Naqvi SJ (1993) The effect of different drying techniques on the pore size distribution of blended cement mortars. Cem Concr Res 23(5): 1223–1228
Mitchell LD, Margeson JC (2006) The effects of solvents on C-S-H as determined by thermal analysis. J Therm Anal Calorim 86(3):591–594
Winnefeld F, Schöler A, Lothenbach (2016) Sample preparation. In: Scrivener K, Snellings R, Lothenbach B (eds) A practical guide to microstructural analysis of cementitious materials. CRC Press, Boca Raton, pp 1–36
Taylor HFW, Turner AB (1987) Reactions of tricalcium silicate paste with organic liquids. Cem Concr Res 17(4):613–623
Taylor HFW (1997) Cement Chemistry. Thomas Telford, London
Neville AM (1997) Propriedades do concreto. Editora PINI, São Paulo
Mehta PK, Monteiro PJM (1994) Concreto: estrutura, propriedades e materiais. PINI, São Paulo
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Hoppe Filho, J., Rodrigues, C.S., Ribeiro, L.S.O.P. et al. Evaluation of sample drying methods to determine the apparent porosity and estimation of degree of hydration of portland cement pastes. J Build Rehabil 6, 1 (2021). https://doi.org/10.1007/s41024-020-00095-x
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DOI: https://doi.org/10.1007/s41024-020-00095-x