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Polymorphism in Containerless Crystallization.

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Title: Polymorphism in Containerless Crystallization.
Authors: David Ehre1, Ke Fang1, Janice E. Aber1, Stephen Arnold1, Michael D. Ward1, Bruce A. Garetz1
Source: Crystal Growth & Design. Oct2011, Vol. 11 Issue 10, p4572-4580. 9p.
Subjects: Polymorphism (Crystallography), Containerless processing, Humidity, Malonic acid, Electrodynamics, Solution (Chemistry), Mass transfer, Nucleation
Abstract: The effect of the ambient relative humidity (RH) on the crystallization of malonic and glutaric acid in aqueous microdroplets was investigated using an electrodynamic balance (EDB). Aqueous droplets containing a solute were injected into a chamber maintained at selected RH values, after which the RH was cycled to characterize crystallization and deliquescence behavior. Glutaric acid crystals that were formed at >40% RH deliquesced at 85 ± 2% RH, consistent with the metastable α polymorph. Glutaric acid crystals initially formed at ≤30% RH, however, deliquesced at 90 ± 2% RH, corresponding to the stable β polymorph. These polymorph identifications were confirmed using in situ Raman spectroscopy. In the case of malonic acid, the mass change measured with the EDB at deliquescence revealed the formation of a hydrate, C3H4O4·1.5H2O, when the crystals were initially formed at ≥20% RH. The EDB response for malonic acid crystals initially formed at ∼5% RH, however, corresponded to an anhydrous form. These observations suggest that, contrary to expectation, metastable crystals were favored at lower supersaturation levels compared with their respective stable forms. This unanticipated behavior is attributed to nucleation within the droplet at the higher RH value but at the air–solution interface of the droplet for lower RH values. [ABSTRACT FROM AUTHOR]
Copyright of Crystal Growth & Design is the property of American Chemical Society and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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DbLabel: Engineering Source
An: 66417155
AccessLevel: 6
PubType: Academic Journal
PubTypeId: academicJournal
PreciseRelevancyScore: 0
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  Data: Polymorphism in Containerless Crystallization.
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  Data: <searchLink fieldCode="DE" term="%22Polymorphism+%28Crystallography%29%22">Polymorphism (Crystallography)</searchLink><br /><searchLink fieldCode="DE" term="%22Containerless+processing%22">Containerless processing</searchLink><br /><searchLink fieldCode="DE" term="%22Humidity%22">Humidity</searchLink><br /><searchLink fieldCode="DE" term="%22Malonic+acid%22">Malonic acid</searchLink><br /><searchLink fieldCode="DE" term="%22Electrodynamics%22">Electrodynamics</searchLink><br /><searchLink fieldCode="DE" term="%22Solution+%28Chemistry%29%22">Solution (Chemistry)</searchLink><br /><searchLink fieldCode="DE" term="%22Mass+transfer%22">Mass transfer</searchLink><br /><searchLink fieldCode="DE" term="%22Nucleation%22">Nucleation</searchLink>
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  Data: The effect of the ambient relative humidity (RH) on the crystallization of malonic and glutaric acid in aqueous microdroplets was investigated using an electrodynamic balance (EDB). Aqueous droplets containing a solute were injected into a chamber maintained at selected RH values, after which the RH was cycled to characterize crystallization and deliquescence behavior. Glutaric acid crystals that were formed at >40% RH deliquesced at 85 ± 2% RH, consistent with the metastable α polymorph. Glutaric acid crystals initially formed at ≤30% RH, however, deliquesced at 90 ± 2% RH, corresponding to the stable β polymorph. These polymorph identifications were confirmed using in situ Raman spectroscopy. In the case of malonic acid, the mass change measured with the EDB at deliquescence revealed the formation of a hydrate, C3H4O4·1.5H2O, when the crystals were initially formed at ≥20% RH. The EDB response for malonic acid crystals initially formed at ∼5% RH, however, corresponded to an anhydrous form. These observations suggest that, contrary to expectation, metastable crystals were favored at lower supersaturation levels compared with their respective stable forms. This unanticipated behavior is attributed to nucleation within the droplet at the higher RH value but at the air–solution interface of the droplet for lower RH values. [ABSTRACT FROM AUTHOR]
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  Data: <i>Copyright of Crystal Growth & Design is the property of American Chemical Society and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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RecordInfo BibRecord:
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        Value: 10.1021/cg200824h
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      – Code: eng
        Text: English
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        PageCount: 9
        StartPage: 4572
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      – SubjectFull: Polymorphism (Crystallography)
        Type: general
      – SubjectFull: Containerless processing
        Type: general
      – SubjectFull: Humidity
        Type: general
      – SubjectFull: Malonic acid
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      – SubjectFull: Electrodynamics
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      – SubjectFull: Solution (Chemistry)
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      – SubjectFull: Mass transfer
        Type: general
      – SubjectFull: Nucleation
        Type: general
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      – TitleFull: Polymorphism in Containerless Crystallization.
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              Text: Oct2011
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