Evolution of distribution and content of water in cement paste by low field nuclear magnetic resonance

Abstract

The low field nuclear magnetic resonance (NMR), as a nondestructive and noninvasive technique, was employed to investigate the water distribution and content in cement paste with different water-to-cement ratio (w/c ratio) during early and later hydration stages. From the water distribution spectrum deduced from relaxation time distribution in paste, it is suggested that the water fills in the capillary pores at initial period, and then diffuses to the mesopores and gel pores in hydration products with the hydration proceeding. The decrease of peak area in water distribution spectrum reflects the transformation from physically bound water to chemically bound water. In addition, based on the connection between relaxation time and pore size, the relative content changes of water in various states and constrained in different types of pores were also measured. The results demonstrate that it is influenced by the formation of pore system and the original water-to-cement ratio in the paste. Consequently, the relative content of capillary water is dropped to less than 2% in the paste with low w/c ratio of 0.3 when being hydrated for 1 d, while the contents are still 16% and 36% in the pastes with w/c ratios of 0.4 and 0.5, respectively.

Keywords

cement water / distribution / water-to-cement ratio / pore / nuclear magnetic resonance

References

[1] TaylorH F WCement chemistry, 19972nd edLondonThomas Telford191-196

[2] McdonaldP J, RodinV, ValoriA. Characterisation of intra- and inter-C-S-H gel pore water in white cement based on an analysis of NMR signal amplitudes as a function of water content [J]. Cement and Concrete Research, 2010, 40(12): 1656-1663

[3] MindnessS, YoungJ F, DarwinDConcrete, 20032nd edUpper Saddle River, NJPrentice Hall69-80

[4] MaK-l, XieY-j, LongG-c, WuK-gang. Invading track of chloride ions in cemented-based materials [J]. Journal of Central South University of Technology, 2010, 17(2): 263-268

[5] BenboudjemaF, MeftahF, TorrentiJ M. Interaction between drying, shrinkage, creep and cracking phenomena in concrete [J]. Engineering Structures, 2005, 27(2): 239-250

[6] Escalante-GarciaJ I. Nonevaporable water from neat OPC and replacement materials in composite cements hydrated at different temperatures [J]. Cement and Concrete Research, 2003, 33(11): 1883-1888

[7] ZhangY-m, SunW, YanH-dong. Hydration of high-volume fly ash cement pastes [J]. Cement and Concrete Composites, 2000, 22(6): 445-452

[8] Baroghel-BounyV. Water vapour sorption experiments on hardened cementitious materials. Part I: Essential tool for analysis of hygral behaviour and its relation to pore structure [J]. Cement and Concrete Research, 2007, 37(3): 414-437

[9] ThomasJ J, FitzgeraldS A, NeumannD A, LivingstonR A. State of water in hydrating tricalcium silicate and Portland cement pastes as measured by quasi-elastic neutron scattering [J]. Journal of the American Ceramic Society, 2001, 84(8): 1811-1816

[10] BordalloH N, AldridgeL P, DesmedtA. Water dynamics in hardened ordinary Portland cement paste or concrete: From quasielastic neutron scattering [J]. Journal Physics Chemistry B, 2006, 110(36): 17966-17976

[11] KorbJ P. Multi-scales nuclear spin relaxation of liquids in porous media [J]. Comptes Rendus Physique, 2010, 11(2): 192-203

[12] ViolaR, TucciA, TimelliniG, FantazziniP. NMR techniques: A non-destructive analysis to follow microstructural changes induced in ceramics [J]. Journal of the European Ceramic Society, 2006, 26(15): 3343-3349

[13] KorbJ P. NMR and nuclear spin relaxation of cement and concrete materials [J]. Current Opinion in Colloid & Interface Science, 2009, 14(3): 192-202

[14] CheumaniY, NdikontarM, de JesoB, SebeG. Probing of wood-cement interactions during hydration of wood-cement composites by proton low-field NMR relaxometry [J]. Journal of Materials Science, 2011, 46(5): 1167-1175

[15] KarakostaE, DiamantopoulosG, KatsiotisM S, FardisM, PapavassilionG, PipilikakiP, ProtopapasM, PanagiotarasD. In situ monitoring of cement gel growth dynamics: Use of a miniaturized permanent Halbach magnet for precise H-1 NMR studies [J]. Industrial & Engineering Chemistry Research, 2010, 49(2): 613-622

[16] FriedemannK, StallmachF, KargerJ. Carboxylates and sulfates of polysaccharides for controlled internal water release during cement hydration [J]. Cement and Concrete Composites, 2009, 31(4): 244-249

[17] SheA-m, YaoWu. Probing the hydration of composite cement pastes containing fly ash and silica fume by proton NMR spin-lattice relaxation [J]. Science in China-Technological Sciences, 2010, 53(6): 1471-1476

[18] BrownsteinK R, TarrT C. Importance of classical diffusion in NMR studies of water in biological cells [J]. Physical Review A, 1979, 19(6): 2446-2453

[19] KorbJ P. Nuclear magnetic relaxation of liquids in porous media [J]. New Journal of Physics, 2011, 13(3): 1-26

[20] KeatingK, KnightR. A laboratory study of the effect of magnetite on NMR relaxation rates [J]. Journal of Applied Geophysics Resonance Sounding — A Reality in Applied Hydrogeophysics, 2008, 66(3/4): 188-196

[21] BohrisA J, GoerkeU, McdonaldP J, MulheronM, NewlingB, Le PageB. A broad line NMR and MRI study of water and water transport in portland cement pastes [J]. Magnetic Resonance Imaging, 1998, 16(5/6): 455-461

[22] FriedmannK, SchonfelderW, StallmachF, KargerJ. NMR relaxometry during internal curing of Potland cements by lightweight aggregates [J]. Materials and Structures, 2008, 41: 1647-1655

[23] WangZ-d, XiaoL-z, LiuT-yan. Application of multi-exponential inversion method to NMR measurements [J]. Science in China Series G, 2004, 47(3): 265-276

[24] BullardJ W, JenningsH M, LivingstonR A, NonatA, SchererG W, SchweitzerJ S, ScrivenerK L, ThomasJ J. Mechanisms of cement hydration [J]. Cement and Concrete Research, 2011, 41(12): 1208-1223

[25] FaureP F, CareS, MagatJ, ChaussadentT. Drying effect on cement paste porosity at early age observed by NMR methods [J]. Construction and Building Materials, 2012, 29(4): 496-503

[26] HalperinW P, JehngY, SongY. Application of spin-spin relaxation to measurement of surface area and pore size distributions in a hydrating cement paste [J]. Magnetic Resonance Imaging, 1994, 12(2): 169-173

[27] JenningsH M. A model for the microstructure of calcium silicate hydrate in cement paste [J]. Cement and Concrete Research, 2000, 30(1): 101-116

[28] JenningsH M. Refinements to colloid model of C-S-H in cement: CM-II [J]. Cement and Concrete Research, 2008, 38(3): 275-289

[29] PaneI, HansenW. Investigation of blended cement hydration by isothermal calorimetry and thermal analysis [J]. Cement and Concrete Research, 2005, 35: 1155-1164

[30] GallucciE, MathurP, ScrivenerK. Microstructural development of early age hydration shells around cement grains [J]. Cement and Concrete Research, 2010, 40(1): 4-13