An In-Line Study of Oiling Out and Crystallization

Autor:	Emilie Deneau, Gerry Steele
Rok vydání:	2005
Předmět:	Supersaturation Materials science Organic Chemistry Jacketed vessel law.invention Crystallography Chemical engineering law Oil droplet Scientific method Phase (matter) Physical and Theoretical Chemistry Crystallization Line (formation)
Zdroj:	Organic Process Research & Development. 9:943-950
ISSN:	1520-586X 1083-6160
DOI:	10.1021/op050107c
Popis:	The oiling out and crystallization of a pharmaceutical compound from a water−ethanol mixture has been studied using a range of in-line process analytical techniques in order to more fully understand the phenomenon and build in control of its crystallization. Mechanistically, oiling out was found to follow a number of steps. It was shown that, in a well-mixed jacketed vessel, the small oil droplets formed on cooling a supersaturated solution grew and then coalesced into larger droplets, which subsequently crystallized. Cooling a static supersaturated solution of the compound resulted in two liquid layers, which if undisturbed were relatively stable. Chromatographic analysis of these layers showed that they contained each of the components, but in different amounts, and that crystallization occurred in the compound rich phase. In situ measurements showed that the temperature−solubility and the cloud point curve were well separated at lower temperatures but merged at higher temperatures. Identification of a ...
Databáze:	OpenAIRE
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