Tandem in situ monitoring for quantitative assessment of mechanochemical reactions involving structurally unknown phases

Lukin, Stipe; Stolar, Tomislav; Tireli, Martina; Blanco, Maria; Babić, Darko; Friščić, Tomislav; Užarević, Krunoslav; Halasz, Ivan

doi:10.1002/chem.201702489

Pregled bibliografske jedinice broj: 884106

Tandem in situ monitoring for quantitative assessment of mechanochemical reactions involving structurally unknown phases

Lukin, Stipe; Stolar, Tomislav; Tireli, Martina; Blanco, Maria; Babić, Darko; Friščić, Tomislav; Užarević, Krunoslav; Halasz, Ivan

Tandem in situ monitoring for quantitative assessment of mechanochemical reactions involving structurally unknown phases // Chemistry : a European journal, 23 (2017), 13941-13949 doi:10.1002/chem.201702489 (međunarodna recenzija, članak, znanstveni)

CROSBI ID: 884106 Za ispravke kontaktirajte CROSBI podršku putem web obrasca

Naslov
Tandem in situ monitoring for quantitative assessment of mechanochemical reactions involving structurally unknown phases

Autori
Lukin, Stipe ; Stolar, Tomislav ; Tireli, Martina ; Blanco, Maria ; Babić, Darko ; Friščić, Tomislav ; Užarević, Krunoslav ; Halasz, Ivan

Izvornik
Chemistry : a European journal (0947-6539) 23 (2017); 13941-13949

Vrsta, podvrsta i kategorija rada
Radovi u časopisima, članak, znanstveni

Ključne riječi
quantitative in situ monitoring, monitoring, mechanochemistry, Raman spectroscopy, synchrotron XRD, pharmaceutical cocrystals

Sažetak
Despite recent advances in real-time and in situ monitoring techniques, a thorough mechanistic understanding of mechanochemical milling reactions is often hindered by the inability of their quantitative evaluation. Here, a tandem approach combining in situ powder X-ray diffraction and Raman spectroscopy enabled quantitative assessment and kinetic analysis of mechanochemical reaction, even when involving new phases of unknown crystal structures, and short-lived intermediates. We also introduce in situ Raman monitoring as a standalone laboratory technique for quantitative assessment of mechanochemical reactions. Our approach is demonstrated on a complex and multi-step mechanochemical cocrystallization of benzoic acid and the model active pharmaceutical ingredient nicotinamide under neat and liquid-assisted grinding, which resulted in complex transformations between four polymorphs. Reaction pathways and polymorph selectivity can be tuned by both the choice of a liquid additive and its amount. Our results provide an important step toward a complete and high-throughput quantitative approach to mechanochemical reaction kinetics and mechanisms, necessary for the development of the mechanistic framework of milling reactions.

Izvorni jezik
Engleski

Znanstvena područja
Kemija, Farmacija

POVEZANOST RADA

Projekti:
HRZZ-UIP-2014-09-4744 - Mehanokemijska reaktivnost pod kontroliranim uvjetima temperature i atmosfere za čišću sintezu funkcionalnih materijala (MECHANOCONTROL) (Užarević, Krunoslav, HRZZ - 2014-09) ( CroRIS)

Ustanove:
Institut "Ruđer Bošković", Zagreb

Profili:

Ivan Halasz (autor)