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Assessing the combined water of cement pastes: comparing solvent exchange and silica gel as hydration stoppage methods

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Abstract

The assessment of the combined water is a reliable method to monitor the hydration of cement pastes. This method is also being used to screen different SCMs and cement formulations. However, to obtain reliable data it is necessary to stop the hydration of specimens, removing the free water. In this sense, this work evaluates the effect of different hydration stoppage methods on assessing the combined water of cement pastes. Three procedures were investigated, two using solvent exchange (RILEM and CEMtec), including the one recommended by RILEM TC 238, and the other using silica gel (Silica4h). Firstly, two cement formulations (OPC and LC50) were evaluated using thermogravimetric analysis and X-ray diffraction. The results of combined water at 7 and 28 days were similar independently of the hydration stoppage technique. A repeatability test was also conducted and demonstrated that all three methods presented good repeatability with a low coefficient of variation. Then, six Brazilian commercial cements had their hydration stopped at 7 and 28 days using the studied procedures. The results of combined water were comparable regardless of the used method. A qualitative analysis was also carried out indicating that for the assessment of combined water the Silica4h is the most practical and cost-effective method to stop the hydration of cement pastes and RILEM is the fastest procedure. Finally, both procedures with solvent exchange require attention due to their health and safety issues, solvent disposal, and acquisition.

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References

  1. Bullard JW, Jennings HM, Livingston RA, Nonat A, Scherer GW, Schweitzer JS, Scrivener KL, Thomas JJ (2011) Mechanisms of cement hydration. Cem Concr Res 41:1208–1223. https://doi.org/10.1016/j.cemconres.2010.09.011

    Article  Google Scholar 

  2. Zhang J, Scherer GW (2011) Comparison of methods for arresting hydration of cement. Cem Concr Res 41:1024–1036. https://doi.org/10.1016/j.cemconres.2011.06.003

    Article  Google Scholar 

  3. John VM, Quattrone M, Abrão PCRA, Cardoso FA (2019) Rethinking cement standards: Opportunities for a better future. Cem Concr Res 124:105832. https://doi.org/10.1016/j.cemconres.2019.105832

    Article  Google Scholar 

  4. P.C.R.A. Abrão, Pozzolan as supplementary cementitious material: availability, reactivity, water demand and environmental indicator, University of São Paulo, 2018.

  5. Abrão PCRA, Cardoso FA, John VM (2020) Efficiency of Portland-pozzolana cements: Water demand, chemical reactivity and environmental impact. Constr Build Mater 247:118546. https://doi.org/10.1016/j.conbuildmat.2020.118546

    Article  Google Scholar 

  6. European Standards (2005) EN196–1: Methods of testing cement - Part 1: determination of strength.

  7. 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. https://doi.org/10.1617/s11527-018-1237-5

    Article  Google Scholar 

  8. Muller ACA, Scrivener KL, Gajewicz AM, McDonald PJ (2013) Densification of C-S–H measured by 1H NMR relaxometry. J Phys Chem C 117:403–412. https://doi.org/10.1021/jp3102964

    Article  Google Scholar 

  9. Muller ACA, Scrivener KL, Gajewicz AM, McDonald PJ (2013) Use of bench-top NMR to measure the density, composition and desorption isotherm of C-S–H in cement paste. Microporous Mesoporous Mater 178:99–103. https://doi.org/10.1016/j.micromeso.2013.01.032

    Article  Google Scholar 

  10. 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 23:3431–3438. https://doi.org/10.1016/j.conbuildmat.2009.06.004

    Article  Google Scholar 

  11. Feldman RF, Sereda PJ (1970) A new model for hydrated Portland cement and its practical implications. Eng J 53:53–59

    Google Scholar 

  12. 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

    Article  Google Scholar 

  13. Hoppe Filho J, Rodrigues CS, Ribeiro LSOP, Medeiros MHF (2020) 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. https://doi.org/10.1007/s41024-020-00095-x

    Article  Google Scholar 

  14. Saraya MEI (2010) Stopping of cement hydration by various methods, HBRC J; 14.

  15. Gutteridge WA, Dalziel JA (1990) Filler cement: the effect of the secondary component on the hydration of Portland cement: part I a fine non-hydraulic filler. Cem Concr Res 20:778–782. https://doi.org/10.1016/0008-8846(90)90011-L

    Article  Google Scholar 

  16. Feldman RF, Beaudoin JJ (1991) Pretreatment of hardened hydrated cement pastes for mercury intrusion measurements. Cem Concr Res 21:297–308. https://doi.org/10.1016/0008-8846(91)90011-6

    Article  Google Scholar 

  17. Moukwa M, Aītcin P-C (1988) The effect of drying on cement pastes pore structure as determined by mercury porosimetry. Cem Concr Res 18:745–752. https://doi.org/10.1016/0008-8846(88)90098-1

    Article  Google Scholar 

  18. Konecny L, Naqvi SJ (1993) The effect of different drying techniques on the pore size distribution of blended cement mortars. Cem Concr Res 23:1223–1228. https://doi.org/10.1016/0008-8846(93)90183-A

    Article  Google Scholar 

  19. Gallé 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 31:1467–1477. https://doi.org/10.1016/S0008-8846(01)00594-4

    Article  Google Scholar 

  20. Scrivener K, Snellings R, Lothenbach B (2016) A practical guide to microstructural analysis of cementitious materials, CRC Press, Boca Raton. Chapters 1, 4 and 5. https://books.google.com.br/books?hl=pt-BR&lr=&id=yJ2mCwAAQBAJ&oi=fnd&pg=PP1&dq=a+practical+guide+to+microstructural+analysis&ots=nPKxfqXqsr&sig=3YcjiWSMrOLbLaptJUKwfuUVD5g. Accessed 20 July 2017

  21. Maciel MH, Soares GS, R.C. de O. Romano, M.A. Cincotto, (2018) 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. https://doi.org/10.1007/s10973-018-7734-5

    Article  Google Scholar 

  22. Korpa A, Trettin R (2006) The influence of different drying methods on cement paste microstructures as reflected by gas adsorption: comparison between freeze-drying (F-drying), D-drying, P-drying and oven-drying methods. Cem Concr Res 36:634–649. https://doi.org/10.1016/j.cemconres.2005.11.021

    Article  Google Scholar 

  23. 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 64:54–62. https://doi.org/10.1016/j.cemconres.2014.06.009

    Article  Google Scholar 

  24. 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 38:737–744. https://doi.org/10.1016/j.cemconres.2008.02.012

    Article  Google Scholar 

  25. Copeland LE, Bragg RH (1954) The hydrates of magnesium perchlorate. J Phys Chem 58:1075–1077. https://doi.org/10.1021/j150522a007

    Article  Google Scholar 

  26. Zhang L, Glasser FP (2000) Critical examination of drying damage to cement pastes. Adv Cem Res 12:79–88. https://doi.org/10.1680/adcr.2000.12.2.79

    Article  Google Scholar 

  27. Kißling PA, Lübkemann F, Mundstock A, Lohaus L, Haist M, Caro J, Bigall NC (2022) Is freeze-drying an alternative to solvent exchange for the hydration stop of cementitious suspensions? Cem Concr Res 159:106841. https://doi.org/10.1016/j.cemconres.2022.106841

    Article  Google Scholar 

  28. Cardoso FA, Innocentini MD, Akiyoshi MM, Pandolfelli VC (2004) Effect of curing time on the properties of CAC bonded refractory castables. J Eur Ceram Soc 24:2073–2078

    Article  Google Scholar 

  29. Cardoso FA, Innocentini MD, Miranda MF, Valenzuela FA, Pandolfelli VC (2004) Drying behavior of hydratable alumina-bonded refractory castables. J Eur Ceram Soc 24:797–802

    Article  Google Scholar 

  30. Muller ACA (2014) Characterization of porosity & C-S-H in cement pastes by 1H NMR, EPFL

  31. Weintraub S (2020) Demystifying silica gel 27

  32. Garci Juenger MC, Jennings HM (2001) The use of nitrogen adsorption to assess the microstructure of cement paste. Cem Concr Res 31:883–892. https://doi.org/10.1016/S0008-8846(01)00493-8

    Article  Google Scholar 

  33. Zhang Z, Zhu Y, Zhu H, Zhang Y, Provis JL, Wang H (2019) Effect of drying procedures on pore structure and phase evolution of alkali-activated cements. Cement Concr Compos 96:194–203. https://doi.org/10.1016/j.cemconcomp.2018.12.003

    Article  Google Scholar 

  34. Beaudoin JJ, Tamtsia BT (2004) Effect of drying methods on microstructural changes in hardened cement paste: an A. C. impedance spectroscopy evaluation. ACT 2:113–120. https://doi.org/10.3151/jact.2.113

    Article  Google Scholar 

  35. Fagerlund G (2009) Chemically bound water as measure of degree of hydration: method and potential errors. Division of Building Materials, Lund Institute of Technology Lund, Sweden

  36. ASTM (2009) Standard practice for measuring hydration kinetics of hydraulic cementitious mixtures using isothermal calorimetry. ASTM, West Conshohocken

    Google Scholar 

  37. Avet F, Snellings R, Alujas Diaz A, Ben Haha M, Scrivener K (2016) Development of a new rapid, relevant and reliable (R3) test method to evaluate the pozzolanic reactivity of calcined kaolinitic clays. Cem Concr Res 85:1–11. https://doi.org/10.1016/j.cemconres.2016.02.015

    Article  Google Scholar 

  38. R. Snellings, X. Li, F. Avet, K. Scrivener (2019) Rapid, robust, and relevant (R3) reactivity test for supplementary cementitious materials. ACI Mater J. 116

  39. Brazilian Association of Technical Standards, ABNT - NBR 16697: Portland cements - Requirements (2018)

  40. Mantellato S, Palacios M, Flatt RJ (2016) Impact of sample preparation on the specific surface area of synthetic ettringite. Cem Concr Res 86:20–28. https://doi.org/10.1016/j.cemconres.2016.04.005

    Article  Google Scholar 

  41. Ratel L, Kuznik F, Johannes K (2022) Open Sorption Systems. In: Cabeza LF (ed) Encyclopedia of Energy Storage. Elsevier, Oxford, pp 526–541. https://doi.org/10.1016/B978-0-12-819723-3.00120-7

    Chapter  Google Scholar 

  42. Ng KC, Chua HT, Chung CY, Loke CH, Kashiwagi T, Akisawa A, Saha BB (2001) Experimental investigation of the silica gel–water adsorption isotherm characteristics. Appl Therm Eng 21:1631–1642. https://doi.org/10.1016/S1359-4311(01)00039-4

    Article  Google Scholar 

  43. Tetreault J (2023) Airborne pollutants in museums, galleries and archives : risk assessment, control strategies and preservation management, Canadian Conservation Institute. https://repository.museumsiam.org/handle/6622252777/17. (Accessed Sept 5, 2022)

  44. C09 Committee (2020) Standard test methods for measuring the reactivity of supplementary cementitious materials by isothermal calorimetry and bound water measurements. ASTM International. https://doi.org/10.1520/C1897-20

  45. de A. Gobbo L (2009) Application of X-ray diffraction and Rietveld Method in Portland cement study (in Portuguese), Universidade de São Paulo. http://www.teses.usp.br/teses/disponiveis/44/44137/tde-23072009-144653/en.php.

  46. Feldman RF, Ramachandran VS (1971) Differentiation of interlayer and adsorbed water in hydrated Portland cement by thermal analysis. Cem Concr Res 1:607–620. https://doi.org/10.1016/0008-8846(71)90016-0

    Article  Google Scholar 

  47. Powers TC, Brownyard TL (1946) Studies of the physical properties of hardened portland cement paste, JP. 43: 101–132. https://doi.org/10.14359/8745

  48. Neville AM (2011) Properties of concrete. Longman, London

    Google Scholar 

  49. Mitsuda T, Taylor HFW (1978) Normal and anomalous tobermorites. Mineral Mag 42:229–235. https://doi.org/10.1180/minmag.1978.042.322.09

    Article  Google Scholar 

  50. Zhang Z, Scherer GW (2021) Physical and chemical effects of isopropanol exchange in cement-based materials. Cem Concr Res 145:106461. https://doi.org/10.1016/j.cemconres.2021.106461

    Article  Google Scholar 

  51. Taylor HFW, Turner AB (1987) Reactions of tricalcium silicate paste with organic liquids. Cem Concr Res 17:613–623. https://doi.org/10.1016/0008-8846(87)90134-7

    Article  Google Scholar 

  52. Baquerizo LG, Matschei T, Scrivener KL (2016) Impact of water activity on the stability of ettringite. Cem Concr Res 79:31–44. https://doi.org/10.1016/j.cemconres.2015.07.008

    Article  Google Scholar 

  53. Spex CertiPrep, Isopropanol Safety Data Sheet (2016) https://sds.chemicalsafety.com/sds/pda/msds/getpdf.ashx?action=msdsdocument&auth=200C200C200C200C2008207A200D2078200C200C200C200C200C200C200C200C200C2008&param1=ZmRwLjFfMjg1NjkxMDNORQ==&unique=1693330072&session=942e5fe2fbf2b755126b8ed7086bebc8&hostname=143.107.3.7

  54. ThermoFisher, Diethyl ether Safety data sheet (2009) https://sds.chemicalsafety.com/sds/pda/msds/getpdf.ashx?action=msdsdocument&auth=200C200C200C200C2008207A200D2078200C200C200C200C200C200C200C200C200C2008&param1=ZmRwLjJfNzYzNTEwMDNORQ==&unique=1694458088&session=f3705b56ae302fb5bd52c85aef117c11&hostname=143.107.96.73

  55. AquaSolutions, Silica gel Safety Data Sheet (2014) https://sds.chemicalsafety.com/sds/pda/msds/getpdf.ashx?action=msdsdocument&auth=200C200C200C200C2008207A200D2078200C200C200C200C200C200C200C200C200C2008&param1=ZmRwLjFfMjk1ODU5MjNORQ==&unique=1693329532&session=942e5fe2fbf2b755126b8ed7086bebc8&hostname=143.107.3.7

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Acknowledgements

This research is part of the CEMtec project—National Institute on Advanced Eco-Efficient Cement Based Technologies—funded by CNPq (Conselho Nacional de Desenvolvimento Científico e Tecnológico—Brazil, Process 485340/2013-5) and FAPESP (São Paulo Research Foundation, Process 14/50948-3 INCT/2014). P.C.R.A. Abrão's work was supported by the FAPESP scholarship (19/13150-7). F.A. Cardoso and M. Quattrone’s work was partially funded by the FUSP EMBRAPII scholarships. The information presented in this study is those of the authors and does not necessarily reflect the opinion of CNPq, FAPESP, CAPES or EMBRAPII.

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Authors and Affiliations

  1. National Institute On Advanced Eco-Efficient Cement-Based Technologies, São Paulo, Brazil

    Pedro Cesar R. A. Abrão, Fábio A. Cardoso, Marco Quattrone & Vanderley M. John

  2. Department of Civil Engineering, Escola Politécnica, University of São Paulo, São Paulo, 05508-070, Brazil

    Pedro Cesar R. A. Abrão, Fábio A. Cardoso, Marco Quattrone & Vanderley M. John

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  1. Pedro Cesar R. A. Abrão
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  2. Fábio A. Cardoso
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  4. Vanderley M. John
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Contributions

PCRAA: Conceptualization, methodology, validation, investigation, writing—original draft, visualization. FAC: Conceptualization, methodology, investigation, writing—review and editing, supervision. MQ: Methodology, investigation, writing—review and editing. VMJ: Conceptualization, Investigation, writing—review and editing, supervision, funding acquisition.

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Correspondence to Pedro Cesar R. A. Abrão or Vanderley M. John.

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We declare that we do not have any commercial or associative interest that represents a conflict of interest in connection with the work submitted.

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This paper is dedicated to the memory of Prof. Maria Alba Cincotto. She has contributed to Mr. Abrão’s Ph.D. during the early stages of his research, and, most importantly, she has formed and inspired most Brazilian researchers and professionals working on chemistry of building materials. Her passion for science, her excellence in teaching and, her kindness will be remembered.

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Abrão, P.C.R.A., Cardoso, F.A., Quattrone, M. et al. Assessing the combined water of cement pastes: comparing solvent exchange and silica gel as hydration stoppage methods. Mater Struct 57, 49 (2024). https://doi.org/10.1617/s11527-024-02322-0

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