Hydraulic calcium phosphate cements (CPCs) that are used as osseous substitutes, set by an acid–base reaction between an acid calcium phosphate and a basic calcium salt (often a phosphate). In order to gain a better understanding of the setting of the monocalcium phosphate monohydrate–calcium oxide cement that we developed and in the aim to improve its mechanical properties, the setting reaction was studied by pH-metry. The two methods described in the literature were used. In the first, cement samples were prepared then crushed after different storage periods at 37 °C, 100% RH. The powder was then immersed in pure water with stirring and the pH was measured after equilibration. In the second technique, the starting materials were poured into water while stirring and the pH were followed over time. The two methods gave different results. The first procedure provided information concerning the pH of the surrounding liquid following the partial dissolution of the cement components, rather than any information about pH changes during setting. The second method is more appropriate to follow the pH variations during setting. In this second procedure, the effects of different parameters such as crushing time, stirring rate, liquid-to-powder (L/P) ratio and temperature were investigated. These parameters may impact substantially on the shape and position of the pH=f(t) curves. One or three pH jumps were observed during the setting depending on the composition of the liquid phase. The time at which these pH jumps occurred depended on the pH of the liquid phase, the concentration of the buffer, the crushing of starting materials, the L/P ratio and the temperature. Good linear correlations were obtained (i) between the time of the pH jumps and the L/P ratio and the temperature and (ii) between the time of the first pH jump and the compressive strength and the final setting time of the cements prepared with different liquid phases. It may be assumed in view of these correlations that the results obtained in dilute solution may be extrapolated to the conditions of cement sample preparation and that the mechanical properties of the cement are directly related to the phenomena that occur at the first pH jump which corresponds to precipitation of dicalcium phosphate dihydrate.
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K. Ishikawa, Y. Miyamoto, M. Nagamaya and K. Asaoka, Biomaterials 16 (1995) 527 and ref. 1–11 therein.
F. C. M. Driessens, M. G. Boltong, M. I. Zapatero, R. M. H. Verbeeck, W. Bonfield, O. Bermudez, E. Fernandez, M. P. Ginebra and J. A. Planell, J. Mater. Sci. Mater. Med. 6 (1995) 272 and refs 3–35 therein.
F. C. M. Driessens, in “Bioceramics of Calcium Phosphate”, edited by K. de Groot (CRC Press, Boca Raton, Florida, 1983).
W. E. Brown and L. C. Chow. Dental restorative cement pastes. US Patent 4 518 430 (1985).
J. L. Lacout, E. Mejdoubi and M. Hamad, J. Mater. Sci. Mater. Med. 7 (1996) 371.
I. C. Ison, M. T. Fulmer, B. M. Barr and B. R. Constantz, in “Hydroxyapatite and Related Materials” edited by P. W. Brown and B. R. Constantz (CRC Press and London, 1994) p. 215.
P. Frayssinet, L. Gineste, P. Comte, J. Fages and N. Rouquet, Biomaterials 19 (1998) 971.
O. Bermudez, M. G. Boltong, F. C. M. Driessens and J. A. Planell, J. Mater. Sci. Mater. Med. 4 (1993) 389.
F. C. M. Driessens, M. G. Boltong, O. Bermudez and J. A. Planell, ibid. 4 (1993) 503.
M. Bohner, P. Van Landuyt, H. P. Merkle and J. Lemaitre, ibid. 8 (1997) 675.
K. Ishikawa, S. Takagi, L. C. Chow and Y. Ishikawa, ibid. 6 (1995) 528.
M. P. Ginebra, E. Fernandez, M. G. Boltong, O. Bermudez and J. A. Planell, F. C. M. Driessens, Clin. Mater. 17 (1994) 99.
K. Kurashina, H. Kurita, M. Hirano, J. M. A. De Blieck, C. P. A. T. Klein and K. De Groot, J. Mater. Sci. Mater. Med. 6 (1995) 340.
T. Koshino, W. Kubota and T. Morii, Biomaterials 16 (1995) 125.
D. Knaack, M. Goad, M. Ailova, C. Rey, A. Tofighi, P. Chakravarthy and D. Duke Lee, J. Biomed. Mater. Res. (Appl Biomater) 43 (1998) 399.
F. C. M. Driessens, M. G. Boltong, J. A. Planell, O. Bermudez, M. P. Ginebra and E. Fernandez, Bioceramics, vol. 6, edited by P. Ducheyne and D. Christiansen (Proceedings of the 6th International Symposium on Ceramics in Medicine, Philadelphia, USA, November 1993) (Butterworth-Heinemann, 1993) p. 469.
L. C. Chow, S. Takagi and K. Ishikawa, in “Formation of Hydroxyapatite in Cement Systems. Hydroxyapatite and Related Materials”, edited by P. W. Brown and B. Constantz (CRC Press, London, 1994) p. 127.
E. Fernandez, M. G. Boltong, M. P. Ginebra, O. Bermudez, F. C. M. Driessens and J. A. Planell, Clin. Mater. 16 (1994) 99.
P. Boudeville, S. Serraj, J. M. Leloup, J. Margerit, B. Pauvert and A. Terol, J. Mater. Sci. Mater. Med. 10 (1999) 99.
S. Serraj, P. Boudeville and A. Terol, ibid. 12 (2001) 45.
F. C. M. Driessens, M. G. Boltong, O. Bermudez, J. A. Planell, M. P. Ginebra and E. Fernandez, ibid. 5 (1994) 164.
O. Bermudez, M. G. Boltong, F. C. M. Driessens and J. A. Planell, ibid. 5 (1994) 160.
C. Liu, W. Shen, Y. Gu and L. Hu, J. Biomed. Mater. Res. 351 (1997) 75.
R. I. Martin and P. W. Brown, ibid. 35(3) (1997) 299.
K. S. Tenhuisen and P. W. Brown, ibid. 36(2) (1997) 233.
P. W. Brown, N. Hocker and S. Hoyle, J. Am. Ceram. Soc. 74(8) (1991) 1848.
R. I. Martin and P. W. Brown, J. Mater. Sci. Mater. Med. 5 (1994) 96.
M. T. Fulmer, R. I. Martin and P. W. Brown, ibid. 3 (1992) 299.
K. S. Tenhuisen and P. W. Brown, J Biomed. Mater. Res. 36(3) (1997) 306.
E. Fernandez, F. J. Gil, M. P. Ginebra, F. C. M. Driessens, J. A. Planell and S. M. Best, J. Mater. Sci. Mater. Med. 10 (1999) 223.
S. Serraj, P. MichaÏlesco, J. Margerit, B. Bernard and P. Boudeville, ibid. 13 (2002) 125-131.
M. Kouassi, P. MichaÏlesco and P. Boudeville. J. Endodont. (2002) to appear.
P. W. Brown and M. T. Fulmer, J. Am. Ceram. Soc. 74(5) (1991) 934.
K. S. Tenhuisen and P. W. Brown, J. Mater. Sci. Mater. Med. 7 (1996) 309 and refs 20–26 therein.
K. L. Elmore and T. D. Farr, Ind. Engr. Chem. (1940) 580.
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Nurit, J., Margerit, J., Terol, A. et al. pH-metric study of the setting reaction of monocalcium phosphate monohydrate/calcium oxide-based cements. Journal of Materials Science: Materials in Medicine 13, 1007–1014 (2002). https://doi.org/10.1023/A:1020367900773
- Compressive Strength
- Calcium Phosphate
- Calcium Phosphate Cement
- Calcium Salt