title: Quantitative in situ and real-time monitoring of mechanochemical reactions.
abstract: 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.
authors.affiliation: Ruđer Bošković Institute, Bijenička 54, 10000 Zagreb, Croatia. ihalasz@irb.hr.
authors.forename: Ivan
authors.initials: I
authors.lastname: Halasz
authors.forename: Tomislav
authors.initials: T
authors.lastname: Friščić
authors.forename: Simon A J
authors.initials: SA
authors.lastname: Kimber
authors.forename: Krunoslav
authors.initials: K
authors.lastname: Užarević
authors.forename: Andreas
authors.initials: A
authors.lastname: Puškarić
authors.forename: Cristina
authors.initials: C
authors.lastname: Mottillo
authors.forename: Patrick
authors.initials: P
authors.lastname: Julien
authors.forename: Vjekoslav
authors.initials: V
authors.lastname: Strukil
authors.forename: Veijo
authors.initials: V
authors.lastname: Honkimäki
authors.forename: Robert E
authors.initials: RE
authors.lastname: Dinnebier
mesh_terms: D007093:Imidazoles / Q000737:chemistry*; D012825:Silicon / Q000737:chemistry; D014961:X-Ray Diffraction; D015034:Zinc Oxide / Q000737:chemistry*
chemical_list: D007093:Imidazoles; C029899:imidazole; D015034:Zinc Oxide; D012825:Silicon