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Combined synchrotron XRD/Raman measurements: In situ identification of polymorphic transitions during crystallization processes

  • A combination of two analytical methods, time-resolved X-ray diffraction (XRD) and Raman spectroscopy, is presented as a novel tool for crystallization studies. An acoustic levitator was employed as sample environment. This setup enables the acquisition of XRD and Raman data in situ simultaneously within a 20 s period and hence permits investigation of polymorphic phase transitions during the crystallization process in different solvents (methanol, ethanol, acetone, dichloromethane, acetonitrile). These real time measurements allow the determination of the phase content from the onset of the first crystalline molecular assemblies to the stable system. To evaluate the capability of this approach, the setup was applied to elucidate the crystallization process of the polymorphic compound nifedipine. The results indicate the existence of solvent-dependent transient phases during the crystallization process. The quality of the data allowed the assignment of the lattice constants of theA combination of two analytical methods, time-resolved X-ray diffraction (XRD) and Raman spectroscopy, is presented as a novel tool for crystallization studies. An acoustic levitator was employed as sample environment. This setup enables the acquisition of XRD and Raman data in situ simultaneously within a 20 s period and hence permits investigation of polymorphic phase transitions during the crystallization process in different solvents (methanol, ethanol, acetone, dichloromethane, acetonitrile). These real time measurements allow the determination of the phase content from the onset of the first crystalline molecular assemblies to the stable system. To evaluate the capability of this approach, the setup was applied to elucidate the crystallization process of the polymorphic compound nifedipine. The results indicate the existence of solvent-dependent transient phases during the crystallization process. The quality of the data allowed the assignment of the lattice constants of the hitherto unknown crystal structure of the β-polymorph.zeige mehrzeige weniger

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Metadaten
Autoren/innen:Maria Klimakow, Jork Leiterer, Janina Kneipp, E. Rössler, Ulrich Panne, K. Rademann, Franziska EmmerlingORCiD
Dokumenttyp:Zeitschriftenartikel
Veröffentlichungsform:Verlagsliteratur
Sprache:Englisch
Titel des übergeordneten Werkes (Englisch):Langmuir
Jahr der Erstveröffentlichung:2010
Verlag:American Chemical Society
Verlagsort:Washington, DC
Jahrgang/Band:26
Ausgabe/Heft:13
Erste Seite:11233
Letzte Seite:11237
Freie Schlagwörter:Acoustic levitation; Crystallization; Nifedipine; Polymorphism; Raman spectroscopy; Synchrotron radiation; XRD
DOI:https://doi.org/10.1021/la100540q
ISSN:0743-7463
ISSN:1520-5827
Verfügbarkeit des Volltexts:Papiergebundenes Belegexemplar in der Bibliothek der BAM vorhanden ("Hard-copy Access")
Bibliotheksstandort:Sonderstandort: Publica-Schrank
Datum der Freischaltung:19.02.2016
Referierte Publikation:Ja
Datum der Eintragung als referierte Publikation:10.06.2010