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

Institutional repository: Repository of the Faculty of Science

Cite this document

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

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

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

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 22 November 2024, https://urn.nsk.hr/urn:nbn:hr:217:083226

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 2024 November 22] Available at: https://urn.nsk.hr/urn:nbn:hr:217:083226

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

Metadata
TitleMethod 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
AuthorStipe Lukin
MentorIvan Halasz (mentor)
Committee memberIvica Đilović (predsjednik povjerenstva)
Committee memberCarsten Bolm https://orcid.org/0000-0001-9415-9917 (član povjerenstva)
Committee memberDarko Babić (član povjerenstva)
GranterUniversity of Zagreb
Faculty of Science
(Department of Chemistry)
Zagreb
Defense date and country2019-09-30, 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)
Languageenglish
URN:NBNurn:nbn:hr:217:083226
Study programmeTitle: 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 resourceText
Extent251 str. ; 30 cm
File originBorn digital
Access conditionsOpen access
Embargo expiration date: 2021-10-01
Terms of useLicence In copyright icon
Created on2019-12-05 13:17:36