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master's thesis
Istraživanje mehanokemijskih polimorfnih transformacija Ramanovom spektroskopijom in situ
Zagreb: University of Zagreb, Faculty of Chemical Engineering and Technology, 2021. urn:nbn:hr:149:376474
Vugrin, Leonarda
University of Zagreb
Faculty of Chemical Engineering and Technology

Institutional repository: Repository of Faculty of Chemical Engineering and Technology University of Zagreb

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Vugrin, L. (2021). Istraživanje mehanokemijskih polimorfnih transformacija Ramanovom spektroskopijom in situ (Master's thesis). Zagreb: University of Zagreb, Faculty of Chemical Engineering and Technology. Retrieved from https://urn.nsk.hr/urn:nbn:hr:149:376474

Vugrin, Leonarda. "Istraživanje mehanokemijskih polimorfnih transformacija Ramanovom spektroskopijom in situ." Master's thesis, University of Zagreb, Faculty of Chemical Engineering and Technology, 2021. https://urn.nsk.hr/urn:nbn:hr:149:376474

Vugrin, Leonarda. "Istraživanje mehanokemijskih polimorfnih transformacija Ramanovom spektroskopijom in situ." Master's thesis, University of Zagreb, Faculty of Chemical Engineering and Technology, 2021. https://urn.nsk.hr/urn:nbn:hr:149:376474

Vugrin, L. (2021). 'Istraživanje mehanokemijskih polimorfnih transformacija Ramanovom spektroskopijom in situ', Master's thesis, University of Zagreb, Faculty of Chemical Engineering and Technology, accessed 16 June 2024, https://urn.nsk.hr/urn:nbn:hr:149:376474

Vugrin L. Istraživanje mehanokemijskih polimorfnih transformacija Ramanovom spektroskopijom in situ [Master's thesis]. Zagreb: University of Zagreb, Faculty of Chemical Engineering and Technology; 2021 [cited 2024 June 16] Available at: https://urn.nsk.hr/urn:nbn:hr:149:376474

L. Vugrin, "Istraživanje mehanokemijskih polimorfnih transformacija Ramanovom spektroskopijom in situ", Master's thesis, University of Zagreb, Faculty of Chemical Engineering and Technology, Zagreb, 2021. Available at: https://urn.nsk.hr/urn:nbn:hr:149:376474

Metadata
TitleIstraživanje mehanokemijskih polimorfnih transformacija Ramanovom spektroskopijom in situ
Title (english)Mechanochemical polymorphic transformations studied by in situ Raman spectroscopy
AuthorLeonarda Vugrin
MentorMarica Ivanković (mentor)
Committee memberMarica Ivanković (predsjednik povjerenstva)
Committee memberHrvoje Ivanković (član povjerenstva)
Committee memberIvan Halasz (član povjerenstva)
GranterUniversity of Zagreb
Faculty of Chemical Engineering and Technology
Zagreb
Defense date and country2021-07-16, Croatia
Scientific / art field,
discipline and subdiscipline		NATURAL SCIENCES
Chemistry
Abstract
Ovaj diplomski rad doprinos je istraživanju mehanokemijskih polimorfnih transformacija. Kao modelni sustav odabran je derivat benzojeve kiseline te njegove transformacije u uvjetima suhog i tekućinom-potpomognutog mljevenja. U kemiji čvrstog stanja mnoga su istraživanja vezana uz temeljne karakteristike polimorfije i faznih prijelaza između polimorfa. Polimorfija je iznimno važna prilikom industrijske proizvodnje čvrstih tvari gdje je bitno da je konačna tvar u određenoj polimofnoj formi s ciljnim fizikalnim i kemijskim svojstvima. Glavni je predmet tih istraživanja priprava različitih polimorfa te određivanje njihovih svojstava uključujući i njihove relativne stabilnosti. U ovom radu istraživan je utjecaj tekućih aditiva na selektivnost i učinkovitost mehanokemijske priprave ciljnih polimorfa. Dobiveni polimorfi 4-nitrobenzojeve kiseline okarakterizirani su pomoću difrakcije rendgenskog zračenja na praškastom uzorku. Utjecaj dodatka malih količina različitih otapala na brzinu i nastanak specifičnog polimorfa istražen je Ramanovom spektroskopijom in situ, a kristalne strukture pripravljenih uzoraka identificirane su difrakcijom na prahu. Korištena su otapala različitih polarnosti odnosno različitih proton-donorskih i proton-akceptorskih svojstava. Prilikom mljevenja polaznog derivata benzojeve kiseline uz dodatak teške vode primijećena je izotopna izmjena vodika karboksilne skupine i deuterija stoga je u svrhu potpunije karakterizacije uz polimorfne transformacije paralelno analiziran i deuterijski kinetički-izotopni efekt. U radu se primjenjuje teorija funkcionala gustoće za optimizaciju struktura i izračun energija odgovarajućih polimorfa s ciljem usporedbe njihove stabilnosti i boljeg razumijevanja eksperimentalno dobivenih rezultata. Uočena je zadovoljavajuća korelacija između rezultata dobivenih računskim metodama i eksperimentalnih podataka što pruža smjernice za daljnje eksperimente i olakšava proučavanje faznih prijelaza odabranog sustava.
Abstract (english)
This work represents a contribution to the research of mechanochemical polymorphic transformations. Using benzoic acid derivatives as model systems, dry and liquid-assisted milling were studied. In solid-state chemistry, fundamental characteristics of polymorphism and their phase transitions have been in the focus of research for decades. Polymorphism is of utmost importance in industrial production of solids where it is essential that the final substance is formulated in the adequate crystalline form having desired physical and chemical properties. The main subject of these studies is the synthesis of different polymorphs and their stability. In this work we have studied the influence of liquid additives on selectivity and eficiency in targeted preparation of polymorphs. The prepared polymorphs were characterized by using powder X-ray diffraction and Raman spectroscopy. The influence of solvents of different polarities and different proton-donor and proton-acceptor properties on the rates and selctivities of polymorphic transformations was examined using in situ Raman spectroscopy, while all the crystal structures were characterised using powder X-ray diffraction data. During the grinding of the starting benzoic acid derivative with the addition of heavy water, an isotopic exchange of hydrogen of the carboxyl group and deuterium was observed. In this master thesis, density functional theory is applied to optimize the structures and calculate the energies of the corresponding polymorphs with the aim of comparing their stability and better understanding of the experimentally obtained results. A satisfactory correlation was observed between the results obtained by computational methods and experimental data, which provides guidelines for further experiments and facilitates the study of phase transitions of the selected system.
Keywords
Keywords (english)
Languagecroatian
URN:NBNurn:nbn:hr:149:376474
Study programmeTitle: Applied Chemistry - Graduate study; specializations in: Environmental chemistry and green technologies, Advanced materials and technologies, Applied organic chemistry
Course: Applied organic chemistry
Study programme type: university
Study level: graduate
Academic / professional title: magistar/magistra primijenjene kemije (magistar/magistra primijenjene kemije)
Type of resourceText
File originBorn digital
Access conditionsOpen access
Terms of useLicence In copyright icon
Created on2023-04-11 09:30:40