Method development for in situ monitoring of mechanochemical reactions by Raman spectroscopy and powder X–ray diffraction

Lukin, Stipe

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doctoral thesis

Method development for in situ monitoring of mechanochemical reactions by Raman spectroscopy and powder X–ray diffraction

Zagreb: University of Zagreb, Faculty of Science, 2019. urn:nbn:hr:217:083226

Lukin, Stipe

University of Zagreb
Faculty of Science
Department of Chemistry

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APA 6th Edition

Lukin, S. (2019). Method development for in situ monitoring of mechanochemical reactions by Raman spectroscopy and powder X–ray diffraction (Doctoral thesis). Zagreb: University of Zagreb, Faculty of Science. Retrieved from https://urn.nsk.hr/urn:nbn:hr:217:083226

MLA 8th Edition

Lukin, Stipe. "Method development for in situ monitoring of mechanochemical reactions by Raman spectroscopy and powder X–ray diffraction." Doctoral thesis, University of Zagreb, Faculty of Science, 2019. https://urn.nsk.hr/urn:nbn:hr:217:083226

Chicago 17th Edition

Harvard

Lukin, S. (2019). 'Method development for in situ monitoring of mechanochemical reactions by Raman spectroscopy and powder X–ray diffraction', Doctoral thesis, University of Zagreb, Faculty of Science, accessed 24 January 2025, https://urn.nsk.hr/urn:nbn:hr:217:083226

Vancouver

Lukin S. Method development for in situ monitoring of mechanochemical reactions by Raman spectroscopy and powder X–ray diffraction [Doctoral thesis]. Zagreb: University of Zagreb, Faculty of Science; 2019 [cited 2025 January 24] Available at: https://urn.nsk.hr/urn:nbn:hr:217:083226

IEEE

S. Lukin, "Method development for in situ monitoring of mechanochemical reactions by Raman spectroscopy and powder X–ray diffraction", Doctoral thesis, University of Zagreb, Faculty of Science, Zagreb, 2019. Available at: https://urn.nsk.hr/urn:nbn:hr:217:083226

Cite this item: https://urn.nsk.hr/urn:nbn:hr:217:083226

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Metadata

Title	Method development for in situ monitoring of mechanochemical reactions by Raman spectroscopy and powder X–ray diffraction
Title (croatian)	Razvoj metoda za praćenje in situ mehanokemijske sinteze Ramanovom spektroskopijom i difrakcijom na praškastom uzorku
Author	Stipe Lukin
Mentor	Ivan Halasz (mentor)
Committee member	Ivica Đilović (predsjednik povjerenstva)
Committee member	Carsten Bolm https://orcid.org/0000-0001-9415-9917 (član povjerenstva)
Committee member	Darko Babić (član povjerenstva)
Granter	University of Zagreb Faculty of Science (Department of Chemistry) Zagreb
Defense date and country	2019-09-30, Croatia
Scientific / art field, discipline and subdiscipline	NATURAL SCIENCES Chemistry
Universal decimal classification (UDC)	54 - Chemistry. Crystallography. Mineralogy
Abstract	Milling reactions are conducted in high-energy ball mills in a closed assembly comprising of a milling jar, sample, and a milling media. So far, monitoring a reaction course of such reactions required periodic disruption of the milling process and sampling for further ex situ analysis. Thus, information obtained in that way might not reflect the true nature of milling reactions. Recently introduced in situ approach based on synchrotron powder X-ray diffraction and Raman spectroscopy for monitoring milling reactions have been superior to the already established ex situ analysis. This thesis represents a further development of methods for uninterrupted real-time and in situ monitoring of milling reactions. Here, a detail description of experimental setup and data analysis is given, and developed methods were used for studying solid-state synthesis of metal-organic frameworks ZIF-6 and ZIF-8, Knoevenagel condensation between barbituric acid and vanillin, isotope-exchange reactions between benzoic acid and deuterated water, 2-pyridone, or paracetamol, and finally, competitive cocrystallization reactions between nicotinamide and benzoic, anthranilic, or salicylic acid.
Abstract (croatian)	Reakcije mljevenjem odvijaju se u specijaliziranim mlinovima unutar zatvorenih posuda u kojima se nalaze reaktanti i kuglice. Praćenje takvih reakcija je zahtjevalo periodičko zaustavljanje mljevenja i uzorkovanje reakcijske smjese za daljnu anlizu ex situ. Stoga, informacije dobivene na ovaj način ne moraju nužno odgovarati stvarnim kemijskim i fizikalnim procesima koji se odvijaju tijekom reakcije. Nedavno uvedene metode praćenja reakcija mljevenja, temeljene na difrakciji na praškastom uzorku i Ramanovoj spektroskopiji in situ, pokazale su se superiornim u usporedbi s dosad korištenim metodama ex situ. U ovoj disertaciji prikazan je daljnji razvoj metoda za neprekidno praćenje reakcija mljevenja, te je dan detaljan opis eksperimentalnog postava i obrade prikupljenih podataka. Razvijene metode iskorištene su u proučavanju sinteze u čvrstom stanju metalo-organskih mreža ZIF-6 i ZIF-8, Knoevenagelovoj kondenzaciji između barbiturne kiseline i vanilina, reakcijama izmjene izotopa između benzojeve kiseline i deuterirane vode, 2-piridona ili paracetamola, i kompetitivnim reakcijama kokristalizacije između nikotinamida i benzojeve, antranilne ili salicilne kiseline.
Keywords
Keywords (croatian)
Language	english
URN:NBN	urn:nbn:hr:217:083226
Study programme	Title: Doctoral study in chemistry Study programme type: university Study level: postgraduate Academic / professional title: doktor/doktorica znanosti, područje prirodnih znanosti, polje kemija (doktor/doktorica znanosti, područje prirodnih znanosti, polje kemija)
Type of resource	Text
Extent	251 str. ; 30 cm
File origin	Born digital
Access conditions	Open access Embargo expiration date: 2021-10-01
Terms of use
Repository	Repository of the Faculty of Science
Created on	2019-12-05 13:17:36