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Challenges of Mechanochemistry : Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation. / Michalchuk, Adam A.L.; Tumanov, Ivan A.; Konar, Sumit et al.

In: Advanced Science, Vol. 4, No. 9, 1700132, 01.09.2017, p. 1700132.

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Michalchuk AAL, Tumanov IA, Konar S, Kimber SAJ, Pulham CR, Boldyreva EV. Challenges of Mechanochemistry: Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation. Advanced Science. 2017 Sept 1;4(9):1700132. 1700132. doi: 10.1002/advs.201700132

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Michalchuk, Adam A.L. ; Tumanov, Ivan A. ; Konar, Sumit et al. / Challenges of Mechanochemistry : Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation. In: Advanced Science. 2017 ; Vol. 4, No. 9. pp. 1700132.

BibTeX

@article{2dc0e6a590b94567adb56a57e6c23a98,
title = "Challenges of Mechanochemistry: Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation",
abstract = "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.",
keywords = "kinetics, mechanochemistry, organic salts, X-ray powder diffraction, ACTIVATION, ACID, X-RAY-DIFFRACTION, OPPORTUNITIES",
author = "Michalchuk, {Adam A.L.} and Tumanov, {Ivan A.} and Sumit Konar and Kimber, {Simon A.J.} and Pulham, {Colin R.} and Boldyreva, {Elena V.}",
note = "Publisher Copyright: {\textcopyright} 2017 The Authors. Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim",
year = "2017",
month = sep,
day = "1",
doi = "10.1002/advs.201700132",
language = "English",
volume = "4",
pages = "1700132",
journal = "Advanced Science",
issn = "2198-3844",
publisher = "Wiley-VCH Verlag",
number = "9",

}

RIS

TY - JOUR

T1 - Challenges of Mechanochemistry

T2 - Is In Situ Real-Time Quantitative Phase Analysis Always Reliable? A Case Study of Organic Salt Formation

AU - Michalchuk, Adam A.L.

AU - Tumanov, Ivan A.

AU - Konar, Sumit

AU - Kimber, Simon A.J.

AU - Pulham, Colin R.

AU - Boldyreva, Elena V.

N1 - Publisher Copyright: © 2017 The Authors. Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

PY - 2017/9/1

Y1 - 2017/9/1

N2 - 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.

AB - 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.

KW - kinetics

KW - mechanochemistry

KW - organic salts

KW - X-ray powder diffraction

KW - ACTIVATION

KW - ACID

KW - X-RAY-DIFFRACTION

KW - OPPORTUNITIES

UR - http://www.scopus.com/inward/record.url?scp=85019110441&partnerID=8YFLogxK

U2 - 10.1002/advs.201700132

DO - 10.1002/advs.201700132

M3 - Article

C2 - 28932677

AN - SCOPUS:85019110441

VL - 4

SP - 1700132

JO - Advanced Science

JF - Advanced Science

SN - 2198-3844

IS - 9

M1 - 1700132

ER -

ID: 9049343