Challenges of Mechanochemistry: Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation | Sciact - CRIS-system of Boreskov Institute of Catalysis

Challenges of Mechanochemistry: Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation Full article

Journal

Advanced Science
, E-ISSN: 2198-3844

Output data

Year: 2017, Volume: 4, Number: 9, Article number : 1700132, Pages count : 7 DOI: 10.1002/advs.201700132

Tags

kinetics, mechanochemistry, organic salts, X-ray powder diffraction

Authors

Michalchuk Adam A.L. ^1,2,3 , Tumanov Ivan A. ^1,4 , Konar Sumit ² , Kimber Simon A.J. ⁵ , Pulham Colin R. ^2,3 , Boldyreva Elena V. ^1,4

Affiliations

1	REC-008 Novosibirsk State University ul. Pirogova 2, 630090 Novosibirsk, Russian Federation
2	EaStChem School of Chemistry and Centre for Science at Extreme Conditions (CSEC) University of Edinburgh Edinburgh EH9 3FJ, UK
3	EPSRC Centre for Continuous Manufacturing and Crystallisation (CMAC), Joseph Black Building, King’s Buildings, David Brewster Rd. Edinburgh EH9 3FJ, UK
4	Institute of Solid State Chemistry and Mechanochemistry SB RAS Kutateladze 18, 630128 Novosibirsk, Russian Federation
5	European Synchrotron Radiation Facility 71 avenue des Martyrs, 38000 Grenoble, France

Funding (5)

1	The Ministry of Education and Science of the Russian Federation	1828
2	Russian Foundation for Basic Research	16-33-60086 (АААА-А15-115121840103-1)
3	Federal Agency for Scientific Organizations	0301-2014-0002
4	Engineering and Physical Sciences Research Council	CMAC 1/1033459/1
5	The University of Edinburgh

Mechanochemical methods offer unprecedented academic and industrial opportunities for solvent‐free synthesis of novel materials. The need to study mechanochemical mechanisms is growing, and has led to the development of real‐time in situ X‐ray powder diffraction techniques (RI‐XRPD). However, despite the power of RI‐XRPD methods, there remain immense challenges. In the present contribution, many of these challenges are highlighted, and their effect on the interpretation of RI‐XRPD data considered. A novel data processing technique is introduced for RI‐XRPD, through which the solvent‐free mechanochemical synthesis of an organic salt is followed as a case study. These are compared to ex situ studies, where notable differences are observed. The process is monitored over a range of milling frequencies, and a nonlinear correlation between milling parameters and reaction rate is observed. Kinetic analysis of RI‐XRPD allows, for the first time, observation of a mechanistic shift over the course of mechanical treatment, resulting from time evolving conditions within the mechanoreactor.

Michalchuk A.A.L. , Tumanov I.A. , Konar S. , Kimber S.A.J. , Pulham C.R. , Boldyreva E.V.
Challenges of Mechanochemistry: Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation

Advanced Science. 2017. V.4. N9. 1700132 :1-7. DOI: 10.1002/advs.201700132 WOS Scopus РИНЦ AN OpenAlex

Full text from publisher

Submitted:	Mar 22, 2017
Published online:	May 8, 2017
Published print:	Sep 1, 2017

Web of science:	WOS:000411148100014
Scopus:	2-s2.0-85019110441
Elibrary:	31021610
Chemical Abstracts:	2017:1512933
OpenAlex:	W2612038360

DB	Citing
Scopus	52
Web of science	54
OpenAlex	65