Publication Type Journal Article
Title In-situ reaction monitoring of a mechanochemical ball mill reaction with solid state NMR
Authors Jan Gerrit Schiffmann Franziska Emmerling Ines C B Martins Leo Van Wuellen
Groups BioMol
Journal SOLID STATE NUCLEAR MAGNETIC RESONANCE
Year 2020
Month October
Volume 109
Number
Pages
Abstract We present an approach towards the in situ solid state NMR monitoring of mechanochemical reactions in a ball mill. A miniaturized vibration ball mill is integrated into the measuring coil of a home-built solid state NMR probe, allowing for static solid state NMR measurements during the mechanochemical reaction within the vessel. The setup allows to quantitatively follow the product evolution of a prototypical mechanochemical reaction, the formation of zinc phenylphosphonate from zinc acetate and phenylphosphonic acid. MAS NMR investigations on the final reaction mixture confirmed a reaction yield of 89\% in a typical example. Thus, NMR spectroscopy may in the future provide complementary information about reaction mechanisms of mechanochemical reactions and team up with other analytical methods which have been employed to follow reactions in situ, such as Raman spectroscopy or X-ray diffraction.
DOI http://dx.doi.org/10.1016/j.ssnmr.2020.101687
ISBN
Publisher ACADEMIC PRESS INC ELSEVIER SCIENCE
Book Title
ISSN 0926-2040
EISSN 1527-3326
Conference Name
Bibtex ID ISI:000576788000004
Observations
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