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Detailed characterization of pyrolysis oil by separation techniques and mass spectrometry
Žvaková, Veronika ; Mravcová, Ludmila (referee) ; Čáslavský, Josef (advisor)
The aim of this work is detailed characterization of pyrolysis oil by advanced analytical separation methods and mass spectrometry. During the pyrolysis process decomposition of complex organic material take place in the presence of high temperatures and the absence of oxygen. Condensable part of vapours and aerosols forms viscous liquid called pyrolysis oil which is a complex mixture of large amount of compounds. In this work samples from microwave pyrolysis of woodchips and sewage sludge from wastewater treatment plant Brno-Modřice were analysed. Samples were provided by Bionic Laboratories company. Samples were separated by column chromatography on activated silica. For detailed characterization of each fraction gas chromatography with mass spectrometry detection and comprehensive two-dimensional gas chromatography with mass spectrometric detection with time of flight analyser were used. Substances that have been identified can be divided into several groups: alkanes, alkenes, aromatic hydrocarbons, polycyclic aromatic hydrocarbons, alcohols, aldehydes, esters, carboxylic acid and heterocycles.
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Study of Exposure PBDE and Perfluorinated Compounds into Aquatic Ecosystem
Vondráčková, Ilona ; Chýlková, Jaromíra (referee) ; Hroch, Martin (referee) ; Kráčmar, Stanislav (referee) ; Vávrová, Milada (advisor)
In the presented PhD. thesis, problems covering occurrence of polybrominated diphenyl ethers (PBDE) and perfluorinated compounds in the environment were solved. The study was focused on identification and further verification of optimal methods in order to determine PBDEs and perfluorinated compounds sampled from the aquatic ecosystem. Polybrominated diphenyl ethers belong to persistent compounds classified as main pollutants; within the environmental constituents, they have been observed particularly in the last decade. For these studies, there were selected surface water matrices and sediments taken in various localities within the river Svratka basin. The analyses were to demonstrate whether they accumulate and remain in these specific matrices for longer time. There we assessed the congeners of polybrominated diphenyl ethers as follows: BDE-28, 47, 66, 85, 99, 100, 153, 154 and 183. In order to isolate them from matrices, various extraction techniques were used, i.e., ultrasonic extraction, microwave extraction, and pressure solvent extraction. Gas chromatography method with electron capture detection (GC/ECD) was selected for determination. The accomplished studies also assessed basic chemical, physical and environmental characteristics of diphenyl ethers in the environmental constituents. The attention was also paid to perfluorooctanoic compounds (PFOA), (PFOS) and (FOSA); physico-chemical properties of these organic pollutants were characterised and their toxicological and environmental aspects were evaluated. Usability of extraction techniques (ultrasonic extraction, pressure solvent extraction, solid phase extraction) applied to PFCs isolation from sediments samples was assessed. Identification and quantification of these analytes were performed using a high performance liquid chromatography/mass spectrometry method (HPLC/MS). After that, the optimized methods applied to real samples. Surface water and sediments were sampled within the river Svratka basin, in particular, from 19 sampling localities. PBDE occurrence was confirmed in sediments samples from the Svratka river (g.kg-1), PBDE were not detected in the surface water samples, their concentrations were below the detection limit, resp.; perfluorinated compounds were not detected in sediments and water samples at all.
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Flame retardants and their penetration into the terrestrial ecosystem
Chytil, Václav ; Čáslavský, Josef (referee) ; Vávrová, Milada (advisor)
This diploma thesis was focused on the analysis of four compounds from brominated flame retardants group, namely pentabromoethylbenzene, hexabromocyclododecane, hexabromobenzene and tetrabromobisphenol A. Matrices were represented by four soil samples and four seat of fire samples. In addition, bisphenol A was also determined. First of all, process of extraction of analytes from matrices was optimized. Three different extraction techniques were tested (pressurized solvent extraction, microwave-assisted extraction and ultrasound-assisted extraction). Next step was to verify stability of target compounds in strongly acidic conditions and to optimize clean-up of extract by column chromatography. Gas chromatography with electron capture detection (GC-ECD) was chosen as an appropriate analytical method for the determination of brominated flame retardants. Bisphenol A was determined by gas chromatography with mass spectrometric detection (GC-MS). The derivatization of phenolic analytes before their final analytical determination was also essential.
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Non-target screening of organic pollutants in waters and sediments
Hamalčíková, Veronika ; Vávrová, Milada (referee) ; Čáslavský, Josef (advisor)
This master thesis deals with the potential influence of the waste dump Hrádek u Pacova and the wastewater treatment plant Brno – Modřice on surroundings using the optimized non-target screening method of organic pollutants in water and sediments. The experimental part is focused on the identification of organic compounds in samples of ground water from monitoring wells, the surface water from stream and pond and in sediment samples collected from streams in the vicinity of municipal waste dump. Organic compounds were also identified in water and sediment samples from the river Svratka near the municipal waste water treatment plant Modřice. The sequential liquid – liquid extraction was used for the isolation of organic compounds in water samples. Organic compounds in sediment samples were isolated by pressurized solvent extraction (PSE) with subsequent fractionation of the extract using column chromatography. Final analysis determination was performed using comprehensive orthogonal two-dimensional gas chromatography with mass spectrometric detection (GCxGC-TOF MS).
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Needles as bioindicators for assessing contamination levels of PAHs
Mikulíková, Iva ; Zlámalová Gargošová, Helena (referee) ; Vávrová, Milada (advisor)
Bioindicators are used to monitor the level of the environmental pollution. Plant bioindicators are most frequently used, particularly mosses, lichens and conifers. This thesis focuses of the monitoring of polycyclic aromatic hydrocarbons alkyl-derivates concentration in the needles, that were taken in different locations in the Czech Republic. Analytes were extracted by mixture of n-hexane and dichlormethane. The acquired extract was cleaned up by column chromatography with activated silicagel and florisil. Gas chromatography - mass spectrometry was used for final analysis.
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Analysis of tar formed by combustion of biomass
Chytil, Václav ; Čáslavský, Josef (referee) ; Vávrová, Milada (advisor)
This bachelor's thesis is focused on the analysis of the tar formed during combustion of biomass. Samples of the tar were provided by Energy Institute, Faculty of Mechanical Engineering, Brno University of Technology. BTEX, polycyclic aromatic hydrocarbons (PAHs) and n-alkanes were chosen as groups of target compounds. Samples (tar solutions in acetone) were refined before the final analysis. In the case of BTEX and n-alkanes, only filtration and dilution were used. In the case of polycyclic aromatic hydrocarbons, samples were filtered and then cleaned-up by column chromatography using silica gel. Gas chromatography with flame ionization detector (GC-FID) was chosen as an appropriate analytical method for the determination of target compounds from selected groups of BTEX and n-alkanes. Target compounds from the group of polycyclic aromatic hydrocarbons were determined by gas chromatography with mass spectrometric detection (GC-MS).
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