Razvoj modula za prijenos analita u dvodimenzijskoj fluidnoj kromatografiji pri superkritičnim uvjetima

doctoral thesis

• Title (english): Development of analyte transfer module in two dimensional supercritical fluid chromatography
• Author: Orjen Petković
• Mentor: Dragana Mutavdžić Pavlović (mentor)
• Mentor: Čedomila Milin (mentor)
• Committee member: Šime Ukić (predsjednik povjerenstva)
• Committee member: Bruno Zelić (član povjerenstva)
• Committee member: Dalibor Broznić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Chemical Engineering and Technology; Zagreb
• Defense date and country: 2018-10-12, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry; Analytic Chemistry
• Universal decimal classification (UDC): 54 - Chemistry. Crystallography. Mineralogy

Abstract

Kromatografija superkritičnim fluidom (SFC) doživljava novi uspon zbog potreba analize sve kompleksnijih uzoraka. SFC analitički sustavi dopuštaju korištenje širokog raspona nepokretnih faza i detektora. Kao pokretna faza najčešće je korišten CO2. Upravo ta sloboda izbora detektora i nepokretnih faza čini SFC vrlo pogodnom tehnikom u razvoju višedimenzijskih kromatografskih sustava. Dobro su poznati SFC × GC i SFC × HPLC dvodimenzijski sustavi, dok su SFC × SFC sustavi još u fazi razvoja. Jedna od osnovnih zapreka bržem razvoju dvodimenzijskih kromatografija upravo je međudimenzijski prijenos analita. Kako bi se omogućilo dublje i kvalitetnije upoznavanje problematike međudimenzijskog prijenosa analita, razvijen je novi modul međudimenzijskog prijenosa analita. Glavna odrednica modula je mogućnost neovisnog upravljanja vrijednostima protoka i tlaka pokretne kromatografske faze. Modul je korišten za utvrđivanje utjecaja tih vrijednosti na kvalitetu dvodimenzijske fluidne kromatografije pri superkritičnim uvjetima. Hipoteza o potrebi neovisne kontrole stanja pokretne faze u tijeku prijenosa pokazala se točnom te su korištena nova saznanja u razvoju metode za analize stvarnih uzoraka. Razvijena metoda koristi velik protok uz nizak tlak pokretne faze pri međudimenzijskom prijenosu analita, što dovodi do kompresije analita u drugoj dimenziji čime se povećava razlučivost u drugoj dimenziji pa tako i u cijelom analitičkom sustavu. Razvijena metoda primijenjena je u analizi stvarnih uzoraka pri čemu su se potvrdila poboljšanja u kvaliteti analitičkog podatka te primjenjivost metode u analizi složenih uzorka.

Abstract (english)

The supercritical fluid chromatography (SFC) is experiencing a revival due to the need to analyze samples of groving complexitiy. Such analytical systems allow for the use of a wide range of stationary phases and detectors, while commonly used mobile phase is CO2.
The variety of choice of detectors and stationary phases makes SFC a good basis for the development of multi-dimensional chromatographic systems. SFC × GC and SFC × HPLC two-dimensional systems are well known, while SFC × SFC systems are still under development. One of the main obstacles to the faster development of two-dimensional chromatography is the analyte transfer between dimensions. A new module for the
inter-dimensional transfer of the analyte was constructed, to allow a better insight to the problem of inter-dimensional transfer of the analyte. The principal characteristics of the module is the ability to control the flow values and the pressure values of the mobile chromatographic phase. The module was used to determine the influence of these values on the quality of two-dimensional fluid chromatography under supercritical conditions.
The hypothesis of the need for independent control of the mobile phase during the transfer has proven correct and new approach, in developing the actual sample analysis method, has been tried. The developed method uses a high flow rate with a low mobile phase pressure during interdimensional transfer of analyte leading to compression analites in the second dimension, thus increasing the resolution in the second dimension and in the entire analytical system. The developed method was applied in the analysis of actual samples, confirming the improvements in the quality of the analytical data and the applicability of the method in the analysis of complex samples.

• Keywords: instrumentacijski modul; kromatografija; superkritični fluid; CO2; međudimenzijski prijenos analita
• Keywords (english): instrumentation module; chromatography; supercritical fluid; CO2; interdimensional analite transfer
• Language: croatian
• URN:NBN: urn:nbn:hr:149:144922
• Promotion: 2018
• Study programme: Title: Engineering Chemistry - Doctoral Course; 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: 95 str. ; 30 cm
• File origin: Born digital
• Access conditions: Open access
• Created on: 2023-12-13 09:53:13