Abstract
This paper presents a method for preparing crystals of triclinic calcium pyrophosphate (t-CPPD). A calcium pyrophosphate intermediate is first prepared by reaction of potassium pyrophosphate and calcium chloride. Samples of the intermediate are dissolved in hydrochloric acid and urea added. Upon heating to 95–100 °C, hydrolysis of the urea causes the pH to rise and t-CPPD crystallises out. Purity of the product was ascertained by chemical and physical analysis. Where large crystals are required an unstirred system is used, while smaller crystals are produced by stirring the reaction mixture.
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P. B. HALVERSON, Scanning Microsc. 6 (1992) 791
A. SWAN, B. R. HEYWOOD, B. CHAPMAN, H. SEWARD and P. A. DIEPPE, Ann. Rheum. Dis. 54 (1995) 825
E. H. BROWN, J. R. LEHR, J. P. SMITH and A. W. FRAZIER, Agr. Food Chem. 11 (1963) 214
G. S. MANDEL, K. M. RENNE, A. M. KOLBACH, W. D. KAPLAN, J. D. MILLER and N. S. MANDEL, J. Cryst. Growth 87 (1988) 453
D. A. SKOOG, D. M. WEST and F. J. HOLLER, Fundamentals of Analytical Chemistry, 6th edn (Saunders: Fort Worth, 1992) p. 83
P. S. CHEN, T. Y. TORIBARA and H. WARNER, Anal. Chem. 28 (1956) 1756
A. C. LARSON and R. B. VON DREELE, GSAS, General structure analysis system (Report, LAUR 86–748, Los Alamos National Laboratory, Los Alamos, 1986)
N. S. MANDEL, Acta Cryst. B31 (1975) 1730
R. A. YOUNG, The Rietveld Method (Oxford: Oxford University Press, 1995)
P.-T. CHENG and K. P. H. PRITZKER, J. Rheumatol. 8 (1981) 772
P.-T. CHENG, K. P. H. PRITZKER, M. E. ADAMS, S. C. NYBURG and S. A. OMAR, J. Rheumatol. 7 (1980) 609
O. SÖHNEL and J. GARSIDE, Precipitation (Oxford: Butterworth-Heinemann, 1992) p. 271
Acknowledgments
We thank Mrs M Marshall for carrying out the ion chromatography. The work was funded by a Project Grant from the Arthritis Research Council. Dr Wilson was supported by grant G9505593MA from the Medical Research Council of the U. K. Dr Shellis thanks Glaxo SmithKline PLC for financial support.
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Groves, P.J., Wilson, R.M., Dieppe, P.A. et al. Synthesis of triclinic calcium pyrophosphate crystals. J Mater Sci: Mater Med 18, 1355–1360 (2007). https://doi.org/10.1007/s10856-007-0129-y
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DOI: https://doi.org/10.1007/s10856-007-0129-y