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Materials and Structures

, 51:111 | Cite as

Report of TC 238-SCM: hydration stoppage methods for phase assemblage studies of blended cements—results of a round robin test

  • Ruben Snellings
  • Jacek Chwast
  • Özlem Cizer
  • Nele De Belie
  • Yuvaraj Dhandapani
  • Pawel Durdzinski
  • Jan Elsen
  • Johannes Haufe
  • Doug Hooton
  • Cédric Patapy
  • Manu Santhanam
  • Karen Scrivener
  • Didier Snoeck
  • Laurent Steger
  • Sui Tongbo
  • Anya Vollpracht
  • Frank Winnefeld
  • Barbara Lothenbach
Original Article

Abstract

For many microstructural studies it is necessary to “stop” cement hydration—to remove free water. This paper describes the results of a round robin test on the impact of hydration stoppage methods on the composition of hydrated cements. A regular and a fly ash blended Portland cement hydrated for 90 days were selected. Ten laboratories participated in the round robin test. Four common hydration stoppage methods were studied: (1) oven drying at 105 °C, (2) solvent exchange by isopropanol, (3) vacuum drying and (4) freeze drying. After the stoppage of hydration powder samples were studied by thermogravimetry (TG) and X-ray diffraction (XRD). Bound water and Ca(OH)2 content were determined based on the TG data. Portlandite and ettringite content were quantified by Rietveld analysis of the XRD data. The goal was to establish interlaboratory reproducibility and to identify the best available protocols for research and standardization purposes. Based on the results of the round robin test three recommendations are made. (1) Oven drying at 105 °C is not recommended. This dehydrates, alters and decomposes calcium aluminate hydrates significantly more than other methods and often produced carbonation artefacts. (2) Isopropanol exchange is the most appropriate hydration stoppage method for the study of the complete hydrate assemblage of cements, including calcium aluminate hydrates such as ettringite and AFm phases. (3) For quantification of portlandite (Ca(OH)2) all tested hydration stoppage protocols are satisfactory, with the exception of oven drying.

Keywords

Supplementary cementitious materials Hydration stoppage Round robin test Protocol Blended cement Hydration products 

Notes

Acknowledgements

This work was carried out as part of the activities of RILEM Technical Committee 238-SCM on Supplementary Cementitious Materials. Maria Juenger is gratefully acknowledged for the detailed review that considerably improved the paper. As Postdoctoral Research Assistant of the Research Foundation-Flanders (FWO-Vlaanderen), Didier Snoeck wants to thank the foundation for its financial support.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

11527_2018_1237_MOESM1_ESM.docx (35 kb)
Supplementary material 1 (DOCX 34 kb)

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Copyright information

© RILEM 2018

Authors and Affiliations

  • Ruben Snellings
    • 1
  • Jacek Chwast
    • 2
  • Özlem Cizer
    • 3
  • Nele De Belie
    • 4
  • Yuvaraj Dhandapani
    • 5
  • Pawel Durdzinski
    • 6
  • Jan Elsen
    • 2
  • Johannes Haufe
    • 7
  • Doug Hooton
    • 8
  • Cédric Patapy
    • 9
  • Manu Santhanam
    • 5
  • Karen Scrivener
    • 6
  • Didier Snoeck
    • 4
  • Laurent Steger
    • 9
  • Sui Tongbo
    • 10
  • Anya Vollpracht
    • 7
  • Frank Winnefeld
    • 11
  • Barbara Lothenbach
    • 11
  1. 1.Sustainable Materials ManagementVITOMolBelgium
  2. 2.Department of Earth and Environmental SciencesKU LeuvenLeuvenBelgium
  3. 3.Department of Civil EngineeringKU LeuvenLeuvenBelgium
  4. 4.Magnel Laboratory for Concrete Research, Department of Structural EngineeringGhent UniversityGhentBelgium
  5. 5.Department of Civil EngineeringIIT MadrasChennaiIndia
  6. 6.Institute of MaterialsEPFLLausanneSwitzerland
  7. 7.Institute for Building Materials ResearchRWTH Aachen UniversityAachenGermany
  8. 8.Department of Civil EngineeringUniversity of TorontoTorontoCanada
  9. 9.Laboratoire Matériaux et Durabilité des ConstructionsINSA ToulouseToulouse Cedex 4France
  10. 10.Sinoma Research InstituteBeijingChina
  11. 11.Laboratory for Concrete and Construction Chemistry, EmpaSwiss Federal Laboratories for Materials Science and TechnologyDuebendorfSwitzerland

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