journal article·2020-08-12Open access

Thermoporometry and Proton NMR Measurement on Cement Paste Equilibrated at Different Relative Humidities

Kiyofumi Kurumisawa, Ole Mejlhede Jensen

Abstract

In this study, thermoporometry by differential scanning calorimetry and proton NMR measurements of hardened cement paste equilibrated under different humidity conditions were carried out, and the results of both measurements were compared. The results reveal that thermoporometry by low temperature DSC measurement cannot detect the water present in samples equilibrated at low relative humidity. On the other hand, it is possible to detect a signal at low relative humidity by proton NMR measurement. It is clarified that water strongly bound to the surface, which cannot be detected by low temperature DSC, exists at a relative humidity of 33% or less. If it is relevant to detect tightly held water, such as water present in the fine gel pores, it is recommended to apply proton NMR measurements. This paper is an extended English version of the authors’ previous work [Kurumisawa, K. and Jensen, O. M., (2020). “Measurement of cement paste at different humidities by thermoporometry and proton NMR.” Proceedings of the Japan Concrete Institute, 42, 347-352. (in Japanese)].
Source: openalex_inverted_index · Quality: baseline

Research context

OpenAlex topics: Concrete and Cement Materials Research · Concrete Properties and Behavior · Smart Materials for Construction

SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.

Affiliations

Faculty of Engineering, Hokkaido University, Kita 13, Nishi 8, Kita-ku, Sapporo, Hokkaido 060-8628, Japan.

Department of Civil Engineering, Technical University of Denmark, DK-2800 Kgs. Lyngby, Denmark.

References (30)

Show source-provided references
1. 1) AIJ, (2018). “JASS 5: Japanese architectural standard specification for reinforced concrete work.” Tokyo: Architectural Institute of Japan. (in Japanese)
2. 2) Bager, D. H. and Sellevold, E. J., (1986a). “Ice formation in hardened cement paste, Part I - Room temperature cured pastes with variable moisture contents.” Cement and Concrete Research, 16(5), 709-720.10.1016/0008-8846(86)90045-1 ↗
3. 3) Bager, D. H. and Sellevold, E. J., (1986b). “Ice formation in hardened cement paste, Part II - Drying and resaturation on room temperature cured pastes.” Cement and Concrete Research, 16(6), 835-844.10.1016/0008-8846(86)90006-2 ↗
4. 4) Bednarska, D. and Koniorczyk, M., (2020). “Freezing of partly saturated cementitious materials - Insight into properties of pore confined solution and microstructure.” Construction and Building Materials, 251, Article ID 118895.10.1016/j.conbuildmat.2020.118895 ↗
5. 5) Brun, M., Lallemand, A., Quinson, J. F. and Eyraud, C., (1977). “A new method for the simultaneous determination of the size and shape of pores: The thermoporometry.” Thermochimica Acta, 21(1), 59-88.10.1016/0040-6031(77)85122-8 ↗
6. 6) Doebelin, N. and Kleeberg, R., (2015). “Profex: A graphical user interface for the Rietveld refinement program BGMN.” Journal of Applied Crystallography, 48, 1573-1580.10.1107/S1600576715014685 ↗
7. 7) Holthausen, R. S. and Mcdonald, P. J., (2020). “On the quantification of solid phases in hydrated cement paste by 1H nuclear magnetic resonance relaxometry.” Cement and Concrete Research, 135, Article ID 106095.
8. 8) Ishikiriyama, K., Todoki, M., Kobayashi, T. and Tanzawa, H., (1995). “Pore size distribution measurements of poly (methyl methacrylate) hydrogel membranes for artificial kidneys using differential scanning calorimetry.” Journal of Colloid and Interface Science, 173(2), 419-428.10.1006/jcis.1995.1342 ↗
9. 9) JSA, (1998). “JIS K0557: Water used for industrial water and wastewater analysis.” Tokyo: Japanese Standards Association.
10. 10) Kose, Y., Takahashi, T., Tanaka, T. and Ohkubo, T., (2013). “Observation of time-dependent behavior of micro-pore structures in cement paste using 1H NMR.” Concrete Research and Technology, 24(3), 67-73. (in Japanese)10.3151/crt.24.67 ↗
11. 11) Koniorczyk, M., Bednarska, D., Nowosielska, M. and Rynkowski, J., (2018). “Nucleation model for mesopore-confined water freezing kinetics.” International Journal of Heat and Mass Transfer, 120, 575-586.10.1016/j.ijheatmasstransfer.2017.12.035 ↗
12. 12) Kuhn, W., Peterli, E. and Majer, H., (1955). “Freezing point depression of gels produced by high polymer network.” Journal of Polymer Science, 16(82), 539-548.10.1002/pol.1955.120168238 ↗
13. 13) Kurumisawa, K., (2015). “Application of thermoporometry for evaluation of properties of hardened cement paste.” Construction and Building Materials, 101, 926-931.10.1016/j.conbuildmat.2015.10.061 ↗
14. 14) Kurumisawa, K., (2019). “Relaxation time of hardened cement paste measured by proton NMR and transport properties.” In: J. Gemrich, Ed. Proceedings of the 15th International Congress on the Chemistry of Cement, Prague, Czech Republic 16-20 September 2019. Prague: Guarant International.
15. 15) Kurumisawa, K. and Jensen, O. M., (2020). “Measurement of cement paste at different humidities by thermoporometry and proton NMR.” Proceedings of the Japan Concrete Institute, 42, 347-352. (in Japanese)
16. 16) Landry, M. R., (2005). “Thermoporometry by differential scanning calorimetry: Experimental considerations and applications.” Thermochimica Acta, 433(1-2), 27-50.10.1016/j.tca.2005.02.015 ↗
17. 17) Maruyama, I., (2010). “Origin of drying shrinkage of hardened cement paste: Hydration pressure.” Journal of Advanced Concrete Technology, 8(2), 187-200.10.3151/jact.8.187 ↗
18. 18) Maruyama, I., Ohkubo, T., Haji, T. and Kurihara, R., (2019). “Dynamic microstructural evolution of hardened cement paste during first drying monitored by 1H NMR relaxometry.” Cement and Concrete Research, 122, 107-117.10.1016/j.cemconres.2019.04.017 ↗
19. 19) McDonald, P. J., Gajewicz, A. M. and Morrell, R., (2017). “Good practice guide 144: The characterisation of cement based materials using T2 1H nuclear magnetic resonance relaxation analysis.” Middlesex, UK: National Physical Laboratory.
20. 20) Muller, A. C. A., Scrivener, K. L., Gajewicz, A. M. and McDonald, P. J., (2013a). “Densification of C-S-H measured by 1H NMR relaxometry.” Journal of Physical Chemistry C, 117(1), 403-412.10.1021/jp3102964 ↗
21. 21) Muller, A. C. A., Scrivener, K. L., Gajewicz, A. M. and McDonald, P. J., (2013b). “Use of bench-top NMR to measure the density, composition and desorption isotherm of C-S-H in cement paste.” Microporous and Mesoporous Materials, 178, 99-103.10.1016/j.micromeso.2013.01.032 ↗
22. 22) Muller, A. C. A., Scrivener, K. L., Skibsted, J., Gajewicz, A. M. and McDonald, P. J., (2015). “Influence of silica fume on the microstructure of cement pastes: New insights from 1H NMR relaxometry.” Cement and Concrete Research, 74, 116-125.10.1016/j.cemconres.2015.04.005 ↗
23. 23) Provencher, S. W., (1976). “An eigenfunction expansion method for the analysis of exponential decay curves.” The Journal of Chemical Physics, 64(7), 2772-2777.10.1063/1.432601 ↗
24. 24) Provencher, S. W., (1982). “Contin: A general purpose constrainded regularization program for inverting noisy linear algebraic and integral equations.” Computer Physics Communications, 27(3), 229-242.10.1016/0010-4655(82)90174-6 ↗
25. 25) Scrivener, K., Snellings, R. and Lothenbach, B., (2016). “A practical guide to microstructural analysis of cementitious materials.” London and New York: CRC Press.
26. 26) Snyder, K. A. and Bentz, D. P., (2004). “Suspended hydration and loss of freezable water in cement pastes exposed to 90% relative humidity.” Cement and Concrete Research, 34(11), 2045-2056.10.1016/j.cemconres.2004.03.007 ↗
27. 27) Sun, Z. and Scherer, G. W., (2010). “Pore size and shape in mortar by thermoporometry.” Cement and Concrete Research, 40(5), 740-751.10.1016/j.cemconres.2009.11.011 ↗
28. 28) Yonemura, M., Kitagaki, R., Ohkubo, T. and Kim, J., (2015). “Pore structure analysis of hardened cement using 1H NMR.” Proceedings of the Japan Concrete Institute, 37(1), 511-516. (in Japanese)
29. 29) Wu, M. and Johannesson, B., (2014). “Impact of sample saturation on the detected porosity of hardened concrete using low temperature calorimetry.” Thermochimica Acta, 580, 66-78.10.1016/j.tca.2014.02.002 ↗
30. 30) Wu, M., Johannesson, B. and Geiker, M., (2014). “A preliminary study of the influence of ions in the pore solution of hardened cement pastes on the porosity determination by low temperature calorimetry.” Thermochimica Acta, 589, 215-225.10.1016/j.tca.2014.05.027 ↗