Nanovlákenné sorbenty pro analytické extrakce
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Disertační práce je zaměřena na vývoj a využití nanostrukturovaných sorbentů, konkrétně nanovlá-ken s použitím v analytické chemii pro metodu mikroextrakce tuhou fází (SPME). Nanovlákna byla pro tyto účely připravena z tepelně odolných polymerů metodou elektrostatického zvlákňování z jehly. Jako tepelně odolné polymery vhodné pro elektrospinning byly vybrány polyetherimid, polyethersulfon a polysulfon. Pro zhotovená nanovlákna byl vyvinut speciální nosič, který umožňuje jejich zachycení a současně je kompatibilní s běžnými autosamplery plynových chromatografů.Na připravených nanovláknech byly provedeny materiálové testy pro ověření vhodnosti je-jich použití. Na zhotovených SPME nosičích s nanovlákny byly realizovány rozsáhlé aplikační testy s cílem ověřit jejich vlastnosti při reálném použití. Pro výsledné reálné porovnání jejich provozních vlastností byly do těchto testů zahrnuty i dvě nejpoužívanější komerční vlákna - polydimethylsi-loxan (100 ?m PDMS) a polydimethylsiloxan/divinylbenzen (65 ?m PDMS/DVB). Testování pro-běhlo metodou headspace SPME (HS-SPME) na plynovém chromatografu s hmotnostní detekcí (GC/MSMS), kde jako modelové polutanty byly použity izomery hexachlorcyklohexanu (HCH). Testy byly koncipovány tak, aby byla postihnuta kinetika sorpce, ověření linearity, testy životnosti, testy parametrů ovlivňujících sorpci a stanovení limitů detekce a stanovitelnosti. Na základě výsledků realizovaných testů v rámci disertační práce se ukazuje aplikační po-tenciál připravených nanovláken jako sorbentu v analytické chemii. Jejich využití směřuje k použití v analytické technice HS-SPME pro stanovení těkavých a především semi-těkavých organických látek. Díky vysoké tepelné odolnosti nanovláken, které jsou naneseny na SPME nosičích, jsou tato zařízení primárně určena pro použití ve spojení s plynovým chromatografem, kde v jeho injektoru dochází k tepelné desorpci analytů.
The dissertation thesis is focused on the development and utilization of nanostructured sorbents - specifically nanofibres used in analytical chemistry for the solid phase microextraction (SPME) method. For this purpose, nanofibres were prepared from heat-resistant polymer solutions by the method of needle electrospinning. Polyetherimide (PEI), polyethersulfone (PES) and polysulfo-ne (PSU) have been selected as heat-resistant polymers suitable for electrospinning. A special carrier has been developed for the produced nanofibers, which enables their storage and they are also compatible with conventional autosamplers of gas chromatographs.Material tests were performed on prepared nanofibres to verify their intended use. Extensive application tests were carried out on SPME carriers with nanofibers to verify their properties in real use. In order to achieve a real comparison of their operational properties, the two most commonly used commercial fibers - polydimethylsiloxane (100 ?m PDMS) and polydimethylsiloxa-ne/divinylbenzene (65 ?m PDMS/DVB) were also included in these tests. Testing was carried out by the headspace SPME (HS-SPME) method on gas chromatograph with mass detection (GC/MSMS) using hexachlorocyclohexanes (HCH) as model pollutants. The tests were designed to cover sorption kinetics, linearity verification, durability tests, sorption-affecting parameters and limit od detection and quantification.Based on the results of tests carried out in this thesis, the application potential of prepared nanofibers as a sorbent in analytical chemistry is shown. Their use is intended for use in the analyti-cal technique HS-SPME for the determination of volatile and mainly for semi-volatile organic com-pounds. Due to the high heat resistance of nanofibres deposited on SPME carriers, these devices are primarily intended for use in conjunction with a gas chromatograph where the analytes are thermally desorbed.
The dissertation thesis is focused on the development and utilization of nanostructured sorbents - specifically nanofibres used in analytical chemistry for the solid phase microextraction (SPME) method. For this purpose, nanofibres were prepared from heat-resistant polymer solutions by the method of needle electrospinning. Polyetherimide (PEI), polyethersulfone (PES) and polysulfo-ne (PSU) have been selected as heat-resistant polymers suitable for electrospinning. A special carrier has been developed for the produced nanofibers, which enables their storage and they are also compatible with conventional autosamplers of gas chromatographs.Material tests were performed on prepared nanofibres to verify their intended use. Extensive application tests were carried out on SPME carriers with nanofibers to verify their properties in real use. In order to achieve a real comparison of their operational properties, the two most commonly used commercial fibers - polydimethylsiloxane (100 ?m PDMS) and polydimethylsiloxa-ne/divinylbenzene (65 ?m PDMS/DVB) were also included in these tests. Testing was carried out by the headspace SPME (HS-SPME) method on gas chromatograph with mass detection (GC/MSMS) using hexachlorocyclohexanes (HCH) as model pollutants. The tests were designed to cover sorption kinetics, linearity verification, durability tests, sorption-affecting parameters and limit od detection and quantification.Based on the results of tests carried out in this thesis, the application potential of prepared nanofibers as a sorbent in analytical chemistry is shown. Their use is intended for use in the analyti-cal technique HS-SPME for the determination of volatile and mainly for semi-volatile organic com-pounds. Due to the high heat resistance of nanofibres deposited on SPME carriers, these devices are primarily intended for use in conjunction with a gas chromatograph where the analytes are thermally desorbed.
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Mikroextrakce tuhou fází; nanovlákna; sorpce; hexachlorcyklohexany; SPME vlákna; plynová chromatografie, Solid Phase Microextraction; nanofibers; sorption; hexachlorocyclohexanes; SPME fibres; gas chromatography