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Laboratory Real‐Time and In Situ Monitoring of Mechanochemical Milling Reactions by Raman Spectroscopy
Author(s) -
Gracin Davor,
Štrukil Vjekoslav,
Friščić Tomislav,
Halasz Ivan,
Užarević Krunoslav
Publication year - 2014
Publication title -
angewandte chemie international edition
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 5.831
H-Index - 550
eISSN - 1521-3773
pISSN - 1433-7851
DOI - 10.1002/anie.201402334
Subject(s) - mechanochemistry , raman spectroscopy , in situ , grinding , materials science , raman scattering , spectroscopy , chemical engineering , nanotechnology , analytical chemistry (journal) , chemistry , organic chemistry , optics , metallurgy , physics , engineering , quantum mechanics
Mechanistic understanding of mechanochemical reactions is sparse and has been acquired mostly by stepwise ex situ analysis. We describe herein an unprecedented laboratory technique to monitor the course of mechanochemical transformations at the molecular level in situ and in real time by using Raman spectroscopy. The technique, in which translucent milling vessels are used that enable the collection of a Raman scattering signal from the sample as it is being milled, was validated on mechanochemical reactions to form coordination polymers and organic cocrystals. The technique enabled the assessment of the reaction dynamics and course under different reaction conditions as well as, for the first time, direct insight into the behavior of liquid additives during liquid‐assisted grinding.