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Temperature dependence of the structures of solution-grown and melt-grown samples of n-hexatetracontane

Published online by Cambridge University Press:  10 January 2013

J. Fenrych
Affiliation:
Department of Physics, University of South Africa, P.O. Box 392, Pretoria 0003, South Africa
E. C. Reynhardt
Affiliation:
Department of Physics, University of South Africa, P.O. Box 392, Pretoria 0003, South Africa
I. Basson
Affiliation:
Department of Physics, University of South Africa, P.O. Box 392, Pretoria 0003, South Africa

Abstract

The crystal structures of solution-grown and melt-grown polycrystalline samples of n-hexatetracontane (n-C46H94) in the temperature range 293–359 K have been investigated by X-ray powder diffraction. The solution-grown sample has an orthorhombic structure, with space group Pbc21 and cell dimensions a=4.952 Å, b=7.424 Å, and c=120.95 Å. While heating this sample a gradual transition to a monoclinic phase takes place, with onset temperature 335 K. At temperatures close to the melting point two configurations of the ab plane have been observed. Cooling a sample from the melt results in a mixture of a monoclinic and an orthorhombic structure. Rietveld refinements of the structures of solution-grown and melt-grown samples at 293 K have been performed.

Type
Research Article
Copyright
Copyright © Cambridge University Press 1997

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References

Boistelle, R., Simon, B., and Pépe, G. (1976). “Polytypic Structures of n-C 28H 58 (Octacosane) and n-C 36H 74 (Hexatriacontane),” Acta Crystallogr. Sec. B 32, 12401243.CrossRefGoogle Scholar
Craig, S. R., Hastie, G. P., Roberts, K. J., and Sherwood, J. N.(1994). “Investigation into structures of some normal alkanes within homologous series C 13H 28 to C 60H 122 using high-resolution synchrotron X-ray powder diffraction,” J. Mater. Chem. 4, 977982.CrossRefGoogle Scholar
Dollase, W. A. (1986). “Correction of intensities for preferred orientation in powder diffractometry: Application of the March model,” J. Appl. Crystallogr. 19, 267272.CrossRefGoogle Scholar
Fenrych, J., Reynhardt, E. C., and Basson, I.(1996). “Structures and molecular dynamics of solution-grown and melt-grown samples of n-heptatriacontane,” J. Phys.: Condens. Matter 8, 53015316.Google Scholar
Gerson, A. R., Roberts, K. J., and Sherwood, J. N. (1991). “X-ray powder diffraction studies of alkanes: Unit-cell parameters of the homologous series C 18H 38 to C 28H 58,” Acta Crystallogr. Sec. B 47, 280284.Google Scholar
Nyburg, S. C., and Potworowski, J. A. (1973). “Prediction of units cells and atomic coordinates for the n-alkanes,” Acta Crystallogr. Sec. B 29, 347352.CrossRefGoogle Scholar
Reynhardt, E. C., Fenrych, J., and Basson, I. (1994). “Structures and molecular dynamics of solution-grown and melt-grown samples of n-hexatriacontane,” J. Phys.: Condens. Matter. 6, 76057616.Google Scholar
Schneider, J.(1987). “Rietveld method runs on IBM-AT,” Acta Crystallogr. Sec. A 43, Suppl. C 295..CrossRefGoogle Scholar
Shearer, H. M., and Vand, V. (1956). “The crystal structure of the monoclinic form of n-hexatriacontane,” Acta Crystallogr. 9, 379384.Google Scholar
Sullivan, P. K., and Weeks, J. (1970). “The intensity as a function of temperature of the low-angle x-ray diffraction maxima of the n-paraffins: Hexatriacontane, tetratetracontane, and Tetranonacontane,” J. Res. Natl. Bur. Stand. Sec. A 74, 203214.CrossRefGoogle Scholar
Takamizawa, K., Ogawa, Y., and Oyama, O. (1982). “Thermal behavior of n-alkanes from n-C 32H 66 to n-C 80H 162, synthesized with attention paid to high purity,” Polym. J. 14, 441–456.Google Scholar
Teare, P. W. (1959). “The crystal structure of Orthorhombic Hexatriacontane C 36H 74,” Acta Crystallogr. 12, 294300.CrossRefGoogle Scholar