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Determination of heavy metals in waste energetic materials with using sequential extraction
Kořínková, Alena ; Sommer, Lumír (referee) ; Doležalová Weissmannová, Helena (advisor)
Tato diplomová práce pojednává o stanovení vybraných kovů v energetických odpadech, jako je úletový popílek, škvára, struska, ložový popel, produkt odsíření apod., které pocházejí ze čtyř moravských tepláren. Extrakce kovů z energetických materiálů byla provedena Tessierovou extrakcí. Za tímto účelem byla použita extrakční činidla chlorid hořečnatý (MgCl2), octan sodný (CH3COONa), hydroxylamin hydrochlorid v kyselině octové (NH2OH.HCl v CH3COOH), peroxid vodíku v kyselině dusičné (H2O2 v HNO3) a kyselina fluorovodíková (HF). Extrakce probíhala při teplotách 25°C a 40°C. Ve všech frakcích byly stanoveny olovo, měď a kadmium s využitím atomové absorpční spektrometrie (F AAS, ET AAS) a rtuť metodou AMA 254.
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Monitoring of mercury and methylmercury content in fish meat and evaluation of risks associated with the consumption of this meat
Křížová, Lucie ; Pořízka, Jaromír (referee) ; Diviš, Pavel (advisor)
Mercury and its compounds are one of the most toxic global pollutants in the environment. It occurs in all segments of the environment, and it attains the food chain ang human body by people consuming fish. The theoretical part of this thesis examines the characteristics of mercury, its occurrence, the roots of its pollution, and the toxicity of various forms of mercury. Consequently, the thesis delineates analytical methodologies applied to determine the overall level of mercury and chemical forms of mercury. The practical part focuses on monitoring the level of mercury and methylmercury in 12 extracts of fish meat. The analyzer AMA 254 has been used to determine the level of mercury and methylmercury in these extracts. Based on the level that resulted from the measurements, the thesis concludes a risk that correlates with consuming this type of meat.
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Contamination of soil and sediment by hazardous metals
Pidima, Tomáš ; Komendová, Renata (referee) ; Doležalová Weissmannová, Helena (advisor)
This bachelor thesis deals with soil and sediments from the environmental perspective. For selected heavy metals – cadmium, lead and mercury are given information about their occurrence, characteristics and potential sources of environmental contamination. It is also mentioned legislation dealing with the topic. The limit concentrations in soil and sediments, determination methodology and principles of the most commonly used instrumental analytical methods for these elements are described.
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Spectrophotometric determination of Chromium(III) with organic reagents
Nevrlá, Jana ; Komendová, Renata (referee) ; Sommer, Lumír (advisor)
The theoretical part of this master’s thesis is mainly focused on the physical and chemical properties of chromium, its toxicity and possibility of entering of various forms of chromium into the environment. There are also described the most common analytical methods for determination of chromium in water, including ways of modification and preconcentration water samples. The aim of experimental part is the optimalization and assessing the conditions spectrophotometric determination of Cr(III) by selected organic reagents (chromazurol S, eriochromcyanine R, 4-(2-thiazolylazo)resorcinol) and their comparison with the determination of total chromium, as Cr(III), using atomic absorption spectrometry with electrothermic atomization. The analytical procedure for spectrophotometric determination of chromium with chromazurol S, which was found to be most suitable and ET-AAS, were applied to real water samples.
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Determination of platinum in Brno's agglomeration
Dvořák, Rostislav ; Řezáčová, Veronika (referee) ; Komendová, Renata (advisor)
This thesis is focused on the determination of platinum in samples of road dust and soil by atomic absorption spectrometry. The theoretical part describes the basic physical and chemical properties of platinum, platinum function in automotive converters and its behavior in the environment. In the experimental section summarizes the methods used to decompositions samples, concentration of the analyte and the main results of the measurements.
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Generation of volatile zinc chelates from aqueous matrix
Kračmarová, Aneta ; Nováková, Eliška (advisor) ; Červený, Václav (referee)
The topic of this work was optimization of the conditions for the generation of volatile zinc chelates. The aim was to develop an alternative method for generating volatile Zn speciates to its reduction by sodium tetrahydridoborate. Detection was carried out by atomic absorption spectrometry. Optimization of the conditions of the chelation reaction itself included the selection of a suitable chelating agent and appropriate modifiers, pH adjustment, suitable reagent and carrier gas flow rates, and appropriate apparatus arrangement. The following method characteristics were obtained under optimal conditions: LOD 1.55 mg L-1 , LOQ 5.17 mg L-1 and sensitivity 0.245 s L mg-1 . The repeatability was 13,7 %. The addition of modifiers was then tested to increase the efficiency of generation of volatile zinc chelates. Potential modifiers included transition metals, organic solvents, heterocyclic organic compounds, compounds from the carbamate group and surfactants. The heterocyclic 1,10-phenanthroline and the carbamate NaPDC were included in the optimal conditions because without them it was not possible to distinguish the signal from noise. Acetonitrile proved to be the most effective modifier, increasing the efficiency to 1547 %. With the addition of acetonitrile, the LOD decreased to 0.191 mg L-1 , the...
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Atomization of hydride forming elements in dielectric barrier plasma discharges
Baranová, Barbora
The aim of this diploma thesis was to optimize the atomization conditions of two hydride forming elements - bismuth and tellurium in dielectric barrier discharge (DBD) plasma atomizers using atomic absorption spectrometry (AAS) as a detector. Two types of electrode constructions of planar DBD atomizers were studied: glued and sputtered electrodes while two construction of high voltage power supply sources were investigated employing either a sinusoidal or square wave modulation of high voltage function. The effect of the gas phase dryer included in the apparatus upstream the atomizer was also investigated. A nafion membrane tube dryer was identified as the most effective one. Its efficiency was verified using optical emission spectrometry. With the nafion tube included in the apparatus, two main parameters of DBD atomizers were optimized: the voltage of the power supply source and argon flow rate, which served as a discharge gas. Using optimal conditions, analytical characteristics were determined for all atomizers used and these were subsequently compared with those achieved in an externally heated quartz (multi)atomizer (MM)QTA. In the case of bismuth, the optimal argon flow rate was determined to be 75 cm3 min-1 for all atomizers. The optimal value for the power supply source with sinusoidal...
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Sewage sludge – a secondary source of environmental contamination with heavy metals
Sysel, Petr ; Zlámalová Gargošová, Helena (referee) ; Komendová, Renata (advisor)
This work deals with the elementary trace analysis of sewage sludge as a potential source of risk elements when applied to agricultural land. A total of 24 samples were analyzed, divided into two sets with different collection dates. The total content of zinc, copper, chromium, lead, mercury and cadmium in sewage sludge, as well as amount of risk elements that are extracted from sludge to water in 24 hours, was determined. Atomic absorption spectrometry was chosen for the analysis. It was found that the risk elements are in sewage sludge in amounts and order Zn (254.68 – 3084.53 mg/kg) > Cu (6.18 – 961.89 mg/kg) > Cr (26.95 – 387 .91 mg/kg) > Pb (0.84 – 155.30 mg/kg) > Hg (0.50 – 4.12 mg/kg) > Cd (0.06 – 2.61 mg/kg). A lower amounts of analyzed metals in the aqueous extracts than their total amounts in sludges were observed. The concentration of mercury and cadmium in the aqueous extracts was below the detection limits. It was evaluated that the risk elements in sewage sludge are found in less water soluble compounds. The results also show that the concentration of risk elements in the sludge does not depend on the number of equivalent inhabitants for which the treatment plant is dimensioned.
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UV-photochemical generation of volatile species of tellurium and other transition metals
Jeníková, Eva
This dissertation thesis is focused on UV-photochemical generation of volatile species of tellurium, ruthenium, rhenium and iridium coupled to methods of atomic spectrometry. In the first part, attention was paid to the optimization of parameters of UV-photochemical generation of volatile tellurium species and its application for speciation analysis of Te(IV) and Te(VI) in water samples. UV-photochemical generation was carried out in a UV-photoreactor, which consisted of a low-pressure mercury lamp wrapped with a polytetrafluoroethylene reaction coil that served as a reactor. Atomic absorption spectrometry with a continuum source of radiation and high resolution and atomization in a miniature diffusion flame were used to optimize the conditions of generation, which included the composition of the reaction medium, irradiation time and the addition of transition metals as modifiers. In order to achieve a higher sensitivity of determination, the generator was coupled to a triple quadrupole inductively coupled plasma mass spectrometer. Since efficient UV-photochemical generation of volatile species was achieved only from Te(IV), with no response from Te(VI), the feasibility of this technique for simple "non-chromatographic" speciation analysis was tested and a method for determination of Te(IV) and...
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UV-photochemical generation of volatile species of tellurium and other transition metals
Jeníková, Eva ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee) ; Kanický, Viktor (referee)
This dissertation thesis is focused on UV-photochemical generation of volatile species of tellurium, ruthenium, rhenium and iridium coupled to methods of atomic spectrometry. In the first part, attention was paid to the optimization of parameters of UV-photochemical generation of volatile tellurium species and its application for speciation analysis of Te(IV) and Te(VI) in water samples. UV-photochemical generation was carried out in a UV-photoreactor, which consisted of a low-pressure mercury lamp wrapped with a polytetrafluoroethylene reaction coil that served as a reactor. Atomic absorption spectrometry with a continuum source of radiation and high resolution and atomization in a miniature diffusion flame were used to optimize the conditions of generation, which included the composition of the reaction medium, irradiation time and the addition of transition metals as modifiers. In order to achieve a higher sensitivity of determination, the generator was coupled to a triple quadrupole inductively coupled plasma mass spectrometer. Since efficient UV-photochemical generation of volatile species was achieved only from Te(IV), with no response from Te(VI), the feasibility of this technique for simple "non-chromatographic" speciation analysis was tested and a method for determination of Te(IV) and...
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