20.500.12556/DKUM-71028 Razkroj nekaterih acetilacetonatov prehodnih kovin s termično in ultrazvočno metodo Decomposition of acetylacetonates of transition metals using thermal and ultrasonic method Glavni cilj magistrske naloge je bila določitev poteka razkroja nekaterih acetilacetonatov s termično in sonokemijsko metodo in identifikacija razkrojnih produktov. Ukvarjali smo se z bakrovim(II), barijevim, cinkovim, manganovim(III), nikljevim(II) in železovim(III) acetilacetonatom. Izbrane acetilacetonate smo najprej analizirali z rentgensko praškovno difrakcijo, nato pa je sledila analiza s termogravimetrično metodo v izbranih temperaturnih območjih. Delo smo nadaljevali s segrevanjem v izbranih topilih in s sonokemijsko metodo. Najprej smo izbrane acetilacetonate poskušali razkrojiti s termično metodo (segrevanje v čaši), nato pa še s sonokemijsko metodo. Pri termični metodi smo uporabljali naslednja topila: vodo, etanol, metanol, acetonitril in benzilalkohol. Sonokemijsko metodo smo izvajali pri vseh spojinah, večinoma eno uro s 50-odstotno amplitudo, pri čemer smo uporabljali topili vodo in etanol. Na koncu smo dobljene razkrojne produkte analizirali z rentgensko praškovno difrakcijo. Na podlagi rentgenskih analiz smo ugotovili, da je za razkroj bakrovega(II) in nikljevega(II) acetilacetonata termična metoda uspešnejša metoda od sonokemijske metode. Pri tem pa je potrebno uporabljati topila, ki imajo vrelišča višja od 100 °C. Pri razkroju barijevega acetilacetonata pa se je za uspešnejšo metodo izkazala sonokemijska metoda. Ugotovili smo še, da je za razkroj nekaterih acetilacetonatov potrebna nižja temperatura, če so raztopljene v topilu. Višja temperatura je potrebna v primeru, če so spojine termogravimetrično analizirane v dušikovi atmosferi – produkt v raztopini hitreje reagira oziroma razpade kot pa suh produkt. The main object of this master's thesis is to determine decomposition of some acetylacetonates by using thermal and ultrasonic method, as well to identify their decomposition products. We have studied copper(II), barium, zinc, manganese(III), nickel(II) and iron(III) acetylacetonates. Chosen acetylacetonates were first analysed by X-ray diffraction, which was followed by thermogravimetric analysis method within chosen temperature range. We continued our research work by heating in chosen solvents as well as by using ultrasonic method. First, we tried to decompose the acetylacetonates by thermal method (heating in a beaker), and then by ultrasonic method. While applying thermal method, we used the following solvents: water, ethanol, methanol, acetonitrile and benzyl alcohol. Ultrasonic method was applied on all compounds, mostly for an hour by 50 % amplitude, using water and ethanol as solvents. At the end of the procedure we analysed the resulting decomposition products by using X-ray diffraction. Based on the X-ray analyses thermal method proved to be more successful than ultrasonic method in the process of decomposition of copper(II) and nickel(II) acetylacetonates. It is necessary to use solvents with boiling points higher than 100 °C. On the other hand, ultrasonic method proved to be more successful when decomposing barium acetylacetonates. Moreover, it was found out that decomposition of some acetylacetonates requires lower temperature when they are dissolved in solvents. Higher temperatures are required in case when compounds are analysed by thermogravimetric method in nitrogen atmosphere – a product reacts or decomposes faster in a solvent compared to a dry product. termična metoda sonokemija ultrazvok acetilacetonati rentgenska praškovna difrakcija thermal method sonochemistry ultrasound acetylacetonates X-ray powder diffraction true true false [D. Lukač] Slovenski jezik Angleški jezik Magistrsko delo/naloga 2018-07-02 16:08:38 2018-07-13 13:25:02 2022-08-01 20:16:53 2019-07-11 18:27:50 2018 0 Maribor 0 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 543.579:544.576(043.2) 21601558 URN:SI:UM:DK:GTFGO3TG MAG_Lukac_Damjana_2018.pdf MAG_Lukac_Damjana_2018.pdf 1 0BCCE9C256B23EC344E09117BDCC3246 5e3f9b6f0b54907ef1f3ef7733ded6dd6f6778da47ec184c8c6dc8659be33275 145b6850-7c10-11eb-bb7a-00155d0001ca 20.500.12556/dkum/e39e7352-ec3d-4192-b3c9-072448484fdf https://dk.um.si/Dokument.php?lang=slv&id=126258 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0