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Characterization of α and γ polymorphs of glycine crystallized from water‐ammonia solution
Author(s) -
Srinivasan K.,
Renuka Devi K.,
Anbuchudar Azhagan S.
Publication year - 2011
Publication title -
crystal research and technology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.377
H-Index - 64
eISSN - 1521-4079
pISSN - 0232-1300
DOI - 10.1002/crat.201000500
Subject(s) - nucleation , aqueous solution , ammonia , crystallization , chemistry , solubility , differential scanning calorimetry , yield (engineering) , crystallography , distilled water , analytical chemistry (journal) , materials science , organic chemistry , thermodynamics , chromatography , metallurgy , physics
Crystallization of metastable α and stable γ polymorphs of glycine was carried out from aqueous solution in the presence of ammonia. Pure aqueous solution and solution with lower concentration of ammonia yield α nucleation and solution with a critical concentration of ammonia yield γ nucleation. Variation in the solubility of glycine in double distilled water and pH of the resulting solution due to the ammonia incorporation was studied in a range of temperatures. The induction period for the α and γ nucleation in the solution was determined and its variation due to the ammonia incorporation was also studied. Single crystals of both the polymorphs were grown by slow evaporation method. Effect of ammonia concentration and the resultant pH of the solution on the nucleation, growth and morphology of the grown polymorphs were investigated. The unidirectional growth of the γ polymorph along the polar axis was revealed. X‐ray powder diffraction method was employed to distinguish both the polymorphs structurally. Their thermal stability above room temperature was studied by differential scanning calorimetry which revealed that the as‐grown γ polymorph transforms to α at 179.6 °C while the as‐grown α retains its phase until melting. The optical transmittance of the grown γ polymorph was studied in the UV‐Vis‐Near IR region. The second harmonic generation (SHG) efficiency of the grown γ polymorph was studied with a Nd:YAG laser source and is about 6.8% higher than that of the inorganic standard KDP. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)