Abstract
Monoclinic (I) and orthorhombic (II) polymorphs of paracetamol were studied by DSC and adiabatic calorimetry in the temperature range 5 - 450 K. At all the stages of the study, the samples (single crystals and powders) were characterized using X-ray diffraction. A single crystal → polycrystal II→ I transformation was observed on heating polymorph II, after which polymorph I melted at 442 K. The previously reported fact that the two polymorphs melt at different temperatures could not be confirmed. The temperature of the II→I transformation varied from crystal to crystal. On cooling the crystals of paracetamol II from ambient temperature to 5 K, a II→ I transformation was also observed, if the 'cooling-heating' cycles were repeated several times. Inclusions of solvent (water) into the starting crystals were shown to be important for this transformation. The values of the low-temperature heat-capacity of the I and II polymorphs of paracetamol were compared, and the thermodynamic functions calculated for the two polymorphs.
Similar content being viewed by others
References
E. Marti, E. Kaiserberger and G. Kaiser (Eds), Thermoanalytical Characterization of Pharmaceuticals, Netzsch Annual 2000, Netzsch-Geraetebau GmbH, 12 (2000), Selb, p. 29.
M. Haisa, S. Kashino and H. Maeda, Acta Crystallogr., B30 (1974) 2510.
M. Haisa, S. Kashino, R. Kawai and H. Maeda, Acta Crystallogr., B32 (1976) 1283.
G. Nichols and C. S. Frampton, J. Pharm. Sci., 87 (1998) 684.
D. Yu. Naumov, M. A. Vasilchenko and J. A. K. Howard, Acta Crystallogr., C54 (1998) 653.
C. C. Wilson, Z. Kristallogr., 215 (2000) 693.
E. V. Boldyreva, T. P. Shakhtshneider, M. A. Vasilchenko, H. Ahsbahs and H. Uchtmann, Acta Crystallogr., B56 (2000) 299.
T. N. Drebushchak and E. V. Boldyreva, Z. Kristallogr., 219 (2004) in press.
P. DiMartino, A.-M. Guyot-Hermann, P. Conflant, M. Drache and J.-C. Guyot, Int. J. Pharm., 128 (1996) 1.
F. N. de Wet, J. J. Gerber, A. P. Lötter, J. G. van der Watt and T. G. Dekker, Drug. Dev. Ind. Pharm., 24 (1998) 447.
E. V. Boldyreva, T. P. Shakhtshneider, H. Ahsbahs, H. Sowa and H. Uchtmann, J. Therm. Anal. Cal., 68 (2002) 437.
P. DiMartino, P. Conflant, M. Drache, J.-P. Huvenne and A.-M. Guyot-Hermann, J. Thermal Anal., 48 (1997) 447.
M. Szelagiewicz, C. Marcolli, S. Cianferani, A. P. Hard, A. Vit, A. Burkhard, M. von Raumer, U. C. Hofmeier, A. Zillan, E. Francotte and R. Schenker, J. Therm. Anal. Cal., 57 (1999) 23.
J. Barra, F. Kubel and E. Doelker, Book of Abstracts, 3rd Symposium on Pharmacy and Thermal Analysis, Ascona, Switzerland 1997, 2PO.
P. Conflant and A. M. Guyot-Hermann, Eur. J. Pharm. Biopharm., 40 (1994) 388.
E. Marti, J. Thermal Anal., 33 (1988) 37.
E. V. Boldyreva, V. A. Drebushchak, T. N. Drebushchak, I. E. Paukov, Y. A. Kovalevskaya and E. S. Shutova, J. Therm. Anal. Cal., 73 (2003) 409.
E. V. Boldyreva, V. A. Drebushchak, T. N. Drebushchak, I. E. Paukov, Y. A. Kovalevskaya and E. S. Shutova, J. Therm. Anal. Cal., 73 (2003) 419.
V. A. Drebushchak, M. A. Mikhailenko, E. V. Boldyreva, T. N. Drebushchak, T. P. Shakhtshneider and V. V. Boldyrev, Book of Abstracts of the 7th International Conference on Pharmacy and Applied Physical Chemistry (PhandTA 7), Innsbruck, 7–11 September 2003. P. PO 17.
M. A. Mikhailenko, J. Cryst. Growth, 265 (2004) 616.
V. G. Bessergenev, Yu. A. Kovalevskaya, I. E. Paukov and Yu. A. Shkredov, Thermochim. Acta, 139 (1989) 245.
V. G. Bessergenev, Yu. A. Kovalevskaya, I. E. Paukov, M. A. Starikov, H. Opperman and W. Reichelt, J. Chem. Thermodynam., 24 (1992) 85.
A. Burger and R. Ramberger, Microchim. Acta II, (1979) 273.
V. A. Drebushchak, Yu. A. Kovalevskaya, I. E. Paukov and E. V. Boldyreva, J. Therm. Anal. Cal., 74 (2003) 109.
V. A. Drebushchak, E. V. Boldyreva, Yu. A. Kovalevskaya, I. E. Paukov and T. N. Drebushchak, J. Therm. Anal. Cal., 2004, accepted.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Boldyreva, E.V., Drebushchak, V.A., Paukov, I.E. et al. DSC and adiabatic calorimetry study of the polymorphs of paracetamol. Journal of Thermal Analysis and Calorimetry 77, 607–623 (2004). https://doi.org/10.1023/B:JTAN.0000038998.47606.27
Issue Date:
DOI: https://doi.org/10.1023/B:JTAN.0000038998.47606.27