4.4 Article

Crystal growth of α and γ glycine polymorphs and their polymorphic phase transformations

期刊

JOURNAL OF CRYSTAL GROWTH
卷 311, 期 1, 页码 156-162

出版社

ELSEVIER SCIENCE BV
DOI: 10.1016/j.jcrysgro.2008.10.084

关键词

Crystal morphology; Solubility; X-ray diffraction; Growth from solutions; Single crystal growth; Non-linear optical materials

资金

  1. Science and Engineering Research Council (SERC) of the Department of Science and Technology (DST), Government of India

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The single crystals of alpha and gamma polymorphs of glycine were grown from aqueous solutions at ambient conditions. The metastable alpha-form was crystallized from pure aqueous solution and the stable gamma-form from aqueous solution in the presence of a critical concentration of a selective additive sodium chloride. Attempt to grow sizable beta-form single crystals were not successful because of their high instability. In stability terms at ambient conditions these three glycine polymorphs are like this: beta < alpha < gamma. The form of crystallization was confirmed by X-ray powder diffraction (XRD). The alpha- and beta-forms crystallize in the monoclinic system with centrosymmetric space groups P2(1)/n and P2(1), respectively, and the gamma-form crystallizes in trigonal-hexagonal system with non-centrosymmetric space group P3(2). At high-humidity conditions, the room temperature polymorphic phase transformations from alpha to gamma and solution-mediated phase transformation from beta to alpha were confirmed by XRD. The transformation from gamma to alpha while heating well above the room temperature observed at around 179 degrees C was recorded by thermogravimetry (TG) and differential thermal analysis (DTA) and confirmed by differential scanning calorimetry (DSC). The morphology of the grown polymorphs were analysed by goniometry. CHN analysis shows the non-existence of sodium chloride species in the grown gamma-glycine single crystals. The optical transparancy of the gamma-form was recorded by UV-vis-Near IR spectroscopy. (C) 2008 Elsevier B.V. All rights reserved.

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