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Simultaneous monitoring of hydration kinetics, microstructural evolution, and surface interactions in hydrating gypsum plaster in the presence of additives

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Abstract

In this article, we use rapid two-dimensional nuclear magnetic resonance T 1–T 2 relaxation time correlations to monitor hydration kinetics, microstructural evolution, and surface interactions simultaneously in gypsum plaster pastes of industrial relevance. In particular, we explore the influence of ground gypsum mineral (GGM) as an accelerator and citric acid as a retarding agent in the hydration of the β form of plaster. Quantitative relative water fractions are determined and the modified hydration processes are observed as expected. These measurements also reveal the evolution of a secondary water population in the presence of the retarding agent when sedimentation of the hemihydrate occurs prior to crystallisation. In these samples, the ratio of relaxation times T 1/T 2 provides an indication of both the number and the strength of interactions between water molecules and solid gypsum particles. It is observed that the GGM decreases the T 1/T 2 ratio, whilst the citric acid increases the T 1/T 2 ratio, relative to the T 1/T 2 ratio in the unmodified plaster paste. We interpret this as an increase in the water–hemihydrate interaction in the presence of GGM, and a decrease in the presence of citric acid, consistent with the current understanding of the behaviour of these additives as an accelerator and retardant, respectively. The T 1 relaxation time measurements provide an indication of the pore structure evolution: larger pores are present in the accelerated product, and smaller pores in the retarded product, compared to the unmodified plaster. These conclusions are supported by helium porosimetry and scanning electron microscopy. The rapid T 1–T 2 measurement described here will be applicable to other reactions that evolve on a time scale of several minutes.

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References

  1. Ridge MJ (1960) Rev Pure Appl Chem 10:243

    Google Scholar 

  2. Ridge MJ, Beretka J (1969) Rev Pure Appl Chem 19:17

    Google Scholar 

  3. Lewry AJ, Williamson J (1994) J Mater Sci 29:6085. doi:10.1007/BF00354546

    Article  ADS  Google Scholar 

  4. Panpa W, Jinawath S (2006) Adv Cem Res 18:145

    Article  Google Scholar 

  5. Jaffel H, Korb JP, Ndobo-Epoy JP, Morin V, Guicquero JP (2006) J Phys Chem B 110:7385

    Article  PubMed  Google Scholar 

  6. Singh NB, Middendorf B (2007) Prog Cryst Growth Charact Mater 53:57

    Article  Google Scholar 

  7. Koslowski T, Ludwig U (1984) The chemistry and technology of gypsum, ASTM STP, vol 861. American Society for Testing Materials, chap. Retardation of gypsum plasters with citric acid: mechanisms and properties, pp 97–104

  8. Amathieu L, Boistelle R (1986) J Cryst Growth 79:169

    Article  ADS  Google Scholar 

  9. Singh M, Garg M (1997) Cem Concr Res 27:947

    Article  Google Scholar 

  10. Badens E, Veesler S, Boistelle R (1999) J Cryst Growth 198:704

    Article  ADS  Google Scholar 

  11. Singh NB, Vellmer C, Middendorf B (2005) Indian J Eng Mater Sci 12:337

    Google Scholar 

  12. Vellmer C, Middendorf B, Singh NB (2006) J Therm Anal Calorim 86:721

    Article  Google Scholar 

  13. Ersen A, Smith A, Chotard T (2006) J Mater Sci 41:7210. doi: 10.1007/s10853-006-0918

    Article  ADS  Google Scholar 

  14. Magallanes-Rivera RX, Escalante-García JI, Gorokhovsky A (2009) Constr Build Mater 23:1298

    Article  Google Scholar 

  15. Lewry AJ, Williamson J (1994) J Mater Sci 29:5279. doi: 10.1007/BF01171536

    Article  ADS  Google Scholar 

  16. Galtier P, Soustelle M, Guilho B (1983) Cem Concr Res 13:703

    Article  Google Scholar 

  17. Ludwig U, Singh NB (1978) Cem Concr Res 8:291

    Article  Google Scholar 

  18. Bensted J, Varma SP (1972) Cem Technol 3:67

    Google Scholar 

  19. Lewry AJ, Williamson J (1994) J Mater Sci 29:5524. doi: 10.1007/BF003499

    Article  ADS  Google Scholar 

  20. Kunkely H, Vogler A (2008) Mater Chem Phys 109:506

    Article  Google Scholar 

  21. Miyazaki H (1968) Shinku Kagaku 15:113

    MathSciNet  Google Scholar 

  22. Šatava V (1970) Sprechsaal Keram Glas Email 103:792

    Google Scholar 

  23. Kuzel HJ, Hauner M (1987) Zement-Kalk-Gips 40:628

    Google Scholar 

  24. Song KM, Mitchell J, Gladden LF (2009) J Mater Sci 44:5004. doi: 10.1007/s10853-009-3765

    Article  ADS  Google Scholar 

  25. Witkamp GJ, van der Eerden JP, van Rosmalen GM (1990) J Cryst Growth 102:281

    Article  ADS  Google Scholar 

  26. Jaffel H, Korb JP, Ndobo-Epoy JP, Guicquero JP, Morin V (2006) J Phys Chem B 110:18401

    Article  PubMed  Google Scholar 

  27. Brownstein KR, Tarr CE (1979) Phys Rev A 19:2446

    Article  ADS  Google Scholar 

  28. Korb JP, Levitz PE (2009) AIP Conf Proc 1081:55

    ADS  Google Scholar 

  29. Emid S, Creyghton JHN (1985) Physica B & C 128:81

    Article  ADS  Google Scholar 

  30. Balcom BJ, MacGregor RP, Beyea SD, Green DP, Armstrong RL, Bremner TW (1996) J Magn Reson A 123:131

    Article  PubMed  Google Scholar 

  31. Mastikhin IV, Mullally H, MacMillan B, Balcom BJ (2002) J Magn Reson 156:122

    Article  PubMed  ADS  Google Scholar 

  32. Faure P, Caré S, Po C, Rodts S (2005) Magn Reson Imaging 23:311

    Article  PubMed  Google Scholar 

  33. Song YQ, Venkataramanan L, Hürlimann MD, Flaum M, Frulla P, Straley C (2002) J Magn Reson 154:261

    Article  PubMed  ADS  Google Scholar 

  34. Venkataramanan L, Song YQ, Hürlimann MD (2002) IEEE Trans Signal Process 50:1017

    Article  MathSciNet  ADS  Google Scholar 

  35. Wahba G (1977) SIAM J Numer Anal 14:651

    Article  MATH  MathSciNet  Google Scholar 

  36. McDonald PJ, Korb JP, Mitchell J, Monteilhet L (2005) Phys Rev E 72:011409

    Article  ADS  Google Scholar 

  37. McDonald PJ, Mitchell J, Mulheron M, Aptaker PS, Korb JP, Monteilhet L (2007) Cem Concr Res 37:303

    Article  Google Scholar 

  38. Seland JG, Bruvold M, Brurok H, Jynge P, Krane J (2007) Magn Reson Med 58:674

    Article  PubMed  Google Scholar 

  39. Mitchell J, Hürlimann MD, Fordham EJ (2009) J Magn Reson 200:198

    Article  PubMed  ADS  Google Scholar 

  40. Kleinberg RL, Kenyon WE, Mitra PP (1994) J Magn Reson A 108:206

    Article  Google Scholar 

  41. Liu G, Li Y, Jonas J (1991) J Chem Phys 95:6892

    Article  ADS  Google Scholar 

  42. Weber D, Mitchell J, McGregor J, Gladden LF (2009) J Phys Chem C 113:6610

    Article  Google Scholar 

  43. Vold R, Waugh J, Klein M, Phelps D (1968) J Chem Phys 48:3831

    Article  ADS  Google Scholar 

  44. Carr H, Purcell E (1954) Phys Rev 94:630

    Article  ADS  Google Scholar 

  45. Meiboom S, Gill D (1958) Rev Sci Instrum 29:688

    Article  ADS  Google Scholar 

  46. Godefroy S, Korb JP, Fleury M, Bryant RG (2001) Phys Rev E 64:021605

    Article  ADS  Google Scholar 

  47. Hürlimann MD (1998) J Magn Reson 131:232

    Article  PubMed  ADS  Google Scholar 

  48. Barberon F, Korb JP, Petit D, Morin V, Bermejo E (2003) Phys Rev Lett 90:116103

    Article  PubMed  ADS  Google Scholar 

Download references

Acknowledgements

The authors thank Mr. Thusara Chandrasekera for providing modifications to the inversion methods. K. M. Song thanks Dr J. Sohn of Cambridge Nanoscience Centre for assistance with the SEM and Mr J. Staniland of Schlumberger Cambridge Research for the helium porosimetry measurements. For financial support K. M. Song thanks Saint-Gobain and J. Mitchell thanks Schlumberger Cambridge Research.

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Authors and Affiliations

  1. Department of Chemical Engineering and Biotechnology, University of Cambridge, Pembroke Street, Cambridge, CB2 3RA, UK

    K. M. Song, J. Mitchell & L. F. Gladden

  2. Saint-Gobain Recherche, 39 Quai Lucien Lefranc, 93303, Aubervilliers, France

    H. Jaffel

Authors
  1. K. M. Song
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  2. J. Mitchell
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  3. H. Jaffel
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  4. L. F. Gladden
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Correspondence to J. Mitchell.

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Song, K.M., Mitchell, J., Jaffel, H. et al. Simultaneous monitoring of hydration kinetics, microstructural evolution, and surface interactions in hydrating gypsum plaster in the presence of additives. J Mater Sci 45, 5282–5290 (2010). https://doi.org/10.1007/s10853-010-4572-7

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  • DOI: https://doi.org/10.1007/s10853-010-4572-7

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