Quantitative in situ and real-time monitoring of mechanochemical reactions

An experimental technique for in situ and real-time monitoring of mechanochemical reactions in a shaker ball mill was recently described, which utilises highly penetrating X-ray radiation available at the ID15B beamline of the European Synchrotron Radiation Facility. Herein, we describe the first at...

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Veröffentlicht in:	Faraday discussions 2014-01, Vol.17, p.23-221
Hauptverfasser:	Halasz, Ivan, Friš i, Tomislav, Kimber, Simon A. J, U arevi, Krunoslav, Puškari, Andreas, Mottillo, Cristina, Julien, Patrick, Štrukil, Vjekoslav, Honkimäki, Veijo, Dinnebier, Robert E
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Sprache:	eng
Schlagworte:	Imidazoles - chemistry Silicon - chemistry X-Ray Diffraction Zinc Oxide - chemistry
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container_title	Faraday discussions
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creator	Halasz, Ivan Friš i, Tomislav Kimber, Simon A. J U arevi, Krunoslav Puškari, Andreas Mottillo, Cristina Julien, Patrick Štrukil, Vjekoslav Honkimäki, Veijo Dinnebier, Robert E
description	An experimental technique for in situ and real-time monitoring of mechanochemical reactions in a shaker ball mill was recently described, which utilises highly penetrating X-ray radiation available at the ID15B beamline of the European Synchrotron Radiation Facility. Herein, we describe the first attempts to perform such reaction monitoring in a quantitative fashion, by introducing an internal X-ray diffraction standard. The use of silicon as an internal standard resolved the issue with variations of the amount of the sample in the X-ray beam due to the non-uniform distribution of the sample in the reaction jar and allowed, via Rietveld analysis, the first quantitative estimate of the amorphous phase content in a mechanochemical reaction as it is being milled. We also highlight problems associated with the non-ideal mixing of the reaction mixture.
doi_str_mv	10.1039/c4fd00013g
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source	MEDLINE; Royal Society Of Chemistry Journals 2008-; Alma/SFX Local Collection
subjects	Imidazoles - chemistry Silicon - chemistry X-Ray Diffraction Zinc Oxide - chemistry
title	Quantitative in situ and real-time monitoring of mechanochemical reactions
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