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Influence of agitation and fluid shear on nucleation of m-hydroxybenzoic acid polymorphs

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Show simple item record Liu, Jin Svärd, Michael Rasmuson, Åke C. 2016-10-25T15:26:09Z 2016-10-25T15:26:09Z 2014
dc.identifier.citation Liu, J,Svard, M,Rasmuson, AC (2014) 'Influence of Agitation and Fluid Shear on Nucleation of m-Hydroxybenzoic Acid Polymorphs'. Crystal Growth & Design, 14 :5521-5531. en_US
dc.description peer-reviewed en_US
dc.description.abstract The influence of agitation and fluid shear on nucleation of m-hydroxybenzoic acid polymorphs from 1-propanol solution has been investigated through 1160 cooling crystallization experiments. The induction time has been measured at different supersaturations and temperatures in two different crystallizer setups: small vials agitated by magnetic stir bars, for which experiments were repeated 4080 times, and a rotating cylinder apparatus, for which each experiment was repeated five times. The nucleating polymorph has in each case been identified by FTIR spectroscopy. At high thermodynamic driving force for nucleation, only the metastable polymorph (form II) was obtained, while at low driving force both polymorphs were obtained. At equal driving force, a higher temperature resulted in a larger proportion of form I nucleations. The fluid dynamic conditions influence the induction time, as well as the polymorphic outcome. Experiments in small vials show that the agitation rate has a stronger influence on the induction time of form II compared to form I. The fraction of form I nucleations is significantly lower at intermediate agitation rates, coinciding with a reduced induction time of form II. In experiments in the rotating cylinder apparatus, the induction time is found to be inversely correlated to the shear rate. The difference in polymorphic outcome at different driving force is examined in terms of the ratio of the nucleation rates of the two polymorphs, calculated by classical nucleation theory using determined values of the pre-exponential factor and interfacial energy for each polymorph. A possible mechanism explaining the difference in the influence of fluid dynamics on the nucleation of the two polymorphs is based on differences between the two crystal structures. It is hypothesized that the layered structure of form II is comparatively more sensitive to changes in shear flow conditions than the more isotropic form I structure. en_US
dc.language.iso eng en_US
dc.publisher American Chemical Society en_US
dc.relation.ispartofseries Crystal Growth and Design;14, (11), pp. 5521-5531
dc.rights © 2014 ACS This document is the Accepted Manuscript version of a Published Work that appeared in final form in Crystal Growth and Design, copyright © American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see en_US
dc.subject MODELS en_US
dc.subject crystal-structures en_US
dc.subject aminobenzoic acid en_US
dc.subject force-field en_US
dc.subject crystallization en_US
dc.subject thermodynamics en_US
dc.subject kinetics en_US
dc.subject history en_US
dc.subject models en_US
dc.title Influence of agitation and fluid shear on nucleation of m-hydroxybenzoic acid polymorphs en_US
dc.type info:eu-repo/semantics/article en_US
dc.type.supercollection all_ul_research en_US
dc.type.supercollection ul_published_reviewed en_US 2016-10-22T11:12:54Z
dc.description.version ACCEPTED
dc.identifier.doi 10.1021/cg500698v
dc.contributor.sponsor SFI en_US
dc.contributor.sponsor Swedish Research Council en_US
dc.relation.projectid 10/IN.1/B3038 en_US
dc.relation.projectid 621-2010-5391 en_US
dc.rights.accessrights info:eu-repo/semantics/openAccess en_US
dc.internal.rssid 1575683
dc.internal.copyrightchecked Yes
dc.identifier.journaltitle Crystal Growth & Design
dc.description.status peer-reviewed

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