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Molecules 2016, 21(4), 458; doi:10.3390/molecules21040458

Formation and Transformation Behavior of Sodium Dehydroacetate Hydrates

1
State Key Laboratory of Chemical Engineering, School of Chemical Engineering and Technology, Tianjin University, No. 92 Weijin Road, Nankai District, Tianjin 300072, China
2
Collaborative Innovation Center of Chemical Science and Chemical Engineering (Tianjin), Tianjin 300072, China
3
Department of Chemical and Biochemical Engineering, The University of Western Ontario, London, ON N6A 5B9, Canada
*
Authors to whom correspondence should be addressed.
Academic Editor: Derek J. McPhee
Received: 25 February 2016 / Revised: 30 March 2016 / Accepted: 1 April 2016 / Published: 6 April 2016
(This article belongs to the Special Issue Crystallization of Pharmaceuticals)
View Full-Text   |   Download PDF [4626 KB, uploaded 6 April 2016]   |  

Abstract

The effect of various controlling factors on the polymorphic outcome of sodium dehydroacetate crystallization was investigated in this study. Cooling crystallization experiments of sodium dehydroacetate in water were conducted at different concentrations. The results revealed that the rate of supersaturation generation played a key role in the formation of the hydrates. At a high supersaturation generation rate, a new sodium dehydroacetate dihydrate needle form was obtained; on the contrary, a sodium dehydroacetate plate monohydrate was formed at a low supersaturation generation rate. Furthermore, the characterization and transformation behavior of these two hydrated forms were investigated with the combined use of microscopy, powder X-ray diffraction (PXRD), Raman spectroscopy, Fourier transform infrared (FTIR), thermal gravimetric analysis (TGA), scanning electron microscopy (SEM) and dynamic vapor sorption (DVS). It was found that the new needle crystals were dihydrated and hollow, and they eventually transformed into sodium dehydroacetate monohydrate. In addition, the mechanism of formation of sodium dehydroacetate hydrates was discussed, and a process growth model of hollow crystals in cooling crystallization was proposed. View Full-Text
Keywords: sodium dehydroacetate; monohydrate; dihydrate; cooling crystallization; hollow crystal; formation mechanism; transformation sodium dehydroacetate; monohydrate; dihydrate; cooling crystallization; hollow crystal; formation mechanism; transformation
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Zhang, X.; Xie, C.; Huang, Y.; Hou, B.; Bao, Y.; Gong, J.; Yin, Q.; Rohani, S. Formation and Transformation Behavior of Sodium Dehydroacetate Hydrates. Molecules 2016, 21, 458.

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