National Repository of Grey Literature 31 records found  previous11 - 20nextend  jump to record: Search took 0.00 seconds. 
Synthesis and separation of arsenic-glutathione complexes
Balcárová, Barbora ; Petry-Podgórska, Inga (advisor) ; Červený, Václav (referee)
The arsenic-glutathione complexes are very unstable in solution and tend to decompose during separation in liquid chromatography. The aim of this work was to develop a relatively fast method of the synthesis and storage conditions for the arsenic-glutathione complexes. The thesis is focused on synthesis, stability in-solution and separation of arsenicglutathione complexes. The synthesis was carried out in solution of 2 mM TCEP (tris(2carboxyethyl)phosphine) in water and with excess of the glutathione. Solutions of 20 ppb arsenic-complexes were consecutively measured after 1h, 2h, 3h, 4h and 24 hours of synthesis. The results confirmed stability of the arsenic-complexes in the reaction mixtures over 24 h. The arsenic-glutathione complexes were separated using a reversed phase high performance liquid chromatography (RP-HPLC) coupled with inductively coupled plasma - mass spectrometry (ICP-MS). The chromatographic method was developed using Aeris widepore 3.6u XB-C18 250x2.10mm column. Isocratic and gradient elutions were compared using several compositions of mobile phases and time of the separation. Methods were tested using samples of synthesized arsenic-glutathione complex (DMAs(GS)). An application of the isocratic elution enabled elimination of time needed for the separation and conditioning of...
Mercury Content in Atmosphere and Wood-Decaying Mushrooms.
Švehla, Jaroslav ; Kratzer, Jan ; Lepšová, A. ; Svoboda, Karel
Polypores can serve as long-term bioindicators of air pollution by heavy metals. The aim of this work was to investigate their potential to monitor concentration of mercury species in the air.
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Speciation analysis of inorganic arsenic in seafood material
Pokorná, Nikola ; Matoušek, Tomáš (advisor) ; Musil, Stanislav (referee)
This thesis was focused on extraction of individual arsenic species from reference materials of fish protein DORM-3 and DORM-4. Extracts were then analyzed by a hydride generation method with detection by inductively coupled plasma mass spectrometry. Materials were extracted in two ways - in a microwave device and in a heating block. It was found that extraction with 2% nitric acid is not efficient. Extraction performed in 2% nitric acid with addition of hydrogen peroxide at various concentrations increased the extraction yield, but it caused conversion of arsenic species. This conversion would mean the overestimation of inorganic arsenic content.
Trace speciation analysis of arsenic in beverages
Fajgarová, Aneta ; Matoušek, Tomáš (advisor) ; Spěváčková, Věra (referee)
The aim of this bachelor thesis was to determine the toxicologically important arsenic species in beverages (beer, wine and apple juice) with minimal sample preparation. Determination of arsenic species was performed by selective hydride generation of arsenic hydrides with cryogenic collection under liquid nitrogen and detection by atomic absorption spectrometry. In all the samples only inorganic arsenic was found, methyl substituted species were below the limit of detection. The method is suitable for speciation analysis of arsenic in beverages. Detection limits are low enough, the determination is not influenced by the sample matrix. The results were also in good agreement with the determination of total arsenic after mineralization by ICP-MS. Since there is no specified maximum arsenic content in beverages, measured concentrations were compared with the limit for drinking water (10 μg l−1 ). All samples were under this limit, except for one sample of apple juice, which arsenic content was about twice higher. Key words speciation analysis, atomic absorption spektrometry, hydride generation, arsenic, beverages
Using of chemical mercury cold vapor generation for speciation analysis of selected mercury compounds employing HPLC and AAS
Králová, Pavlína ; Červený, Václav (advisor) ; Kratzer, Jan (referee)
The aim of this diploma thesis was to verify the usability of the chemical generation of mercury cold vapor for speciation analysis of selected mercury compounds using high - performance liquid chromatography coupled within atomic absorption spectrometry in the determination of mercury in real tap water samples. In this work, mercuric chloride, methylmercury, ethylmercury and phenylmercury were selected as model analytes. In the first part, the working conditions of chemical generation of mercury cold vapor for each of the selected specie of mercury were optimized. Optimized equipment was used to measure the calibration dependence for each specie and the basic characteristics of the method were established. After optimization of the chemical generation, HPLC column was connected prior this derivatization step and in resulted combined apparatus HPLC - CVG - QTAAS, the separation step was optimized . At optimized conditions, the calibration dependence was measured for each specie and the basic characteristics of the developed method including HPLC separation were established. In conclusion, the proposed analytical method was tested on real flowing tap water samples. Because of low content of mercury species in these samples, the recovery of the method was established when comparing the signal of...
Extraction of Selected Mercury Compounds from Real Samples for Speciation Analysis Employing RP-HPLC-UV-CVG-QTAAS
Kolorosová, Alžběta ; Červený, Václav (advisor) ; Kratzer, Jan (referee)
The extraction of mercury species (methylmercury, ethylmercury, phenylmercury and inorganic mercury(II)) from fish tissue, its determination by reverse phase HPLC, UV-photochemical generation of cold vapour, and detection by atomic absorption spectrometry is described in this work. Various extraction agents and digestion methods were compared in order to find the best alternative. The mixture of 6.25% tetramethylammonium hydroxide and 0.05 mol·l-1 hydrochloride acid was chosen as the best extraction agent. In addition to the high extraction efficiency, the solution involved positively not only UV-photochemical generation, but also separation of observed species. On the contrary, the poor repeatability was achieved with the microwave-assisted digestion due to the proved sorption of mercury species on the Teflon vessels. Therefore, the extraction by high temperature (50-60 řC) in glass bottles was preferred. The results of the determination of the mercury species after the extraction from the real samples were compared to the outcomes obtained by AMA 254. The proposed extraction technique together with the RP-HPLC-UV-CVG-QTAAS is suitable for the speciation analysis of mercury.
Speciation analysis of arsenic-glutathione complexes by ion-pairing HPLC-ICP-MS
Zušťáková, Veronika ; Matoušek, Tomáš (advisor) ; Červený, Václav (referee)
The thesis has focused on the separation of arsenic-glutathione species using ion-pairing high performance liquid chromatography with detection by inductively coupled plasma mass spectrometry. Species were separated on chromatographic column Prodigy ODS (3) using an aqueous mobile phase containing 4.7mM tetrabutylammonium hydroxide (TBAH), 2mM malonic acid and 4% methanol at pH 5.85 in the isocratic mode. Simple arsenic species - arsenite (iAsIII), arsenate (iAsV) monomethylarsenic acid (MAsIII), monomethylarsenous acid (MAsV), dimethylarsenic acid (DMAsIII) and dimethylarsenous acid (DMAsV), which served as arsenic standards to determine retention times, were successfully separated under these conditions. Arsenic-glutathione complexes As(GS)3, MAs(GS)2 and DMAs (GS) were not successfully separated. These complexes provided peaks of simple arsenic species. Peak broadening was observed in the first analysis of As(GS)3 and MAs(GS)2 complexes, which disappeared in subsequent analyses. This broadening probably represents a residual of glutathion complex which disintegrated to single species. Powered by TCPDF (
Optimization of generation and atomization of arsines for speciation analysis by atomic fluorescence spectrometry
Marschner, Karel ; Dědina, Jiří (advisor) ; Komárek, Josef (referee)
Speciation analysis of arsenic based on selective hydride generation and detection by atomic fluorescence spectrometry have been studied in this work. It was found that under optimum conditions of atomization in the flame in gas shield atomizer, sensitivity was approximately twice higher and detection limit was about four times lower compared to miniature diffusion flame, which is a standard atomizer for atomic fluorescence spectrometry. The conditions to generate hydrides from both inorganic forms of the arsenic, i.e. from arsenite and arsenate, with the same efficiency have been found in the batch arrangement, by using 1 mol dm-3 hydrochlorid acid and 1% solution of tetrahydridoborate. To determine only trivalent form, TRIS buffer at pH 6.00 was used together with 1% sodium tetrahydridoborate. The detection limits found for inorganic arsenic, i.e. for arsenite and arsenate, respectively, were 15 ng dm-3 and 9 ng dm-3 . It was found that in the batch arrangement under these conditions it is possible to generate corresponding hydrides methylarsonate and dimethylarsonate with the same efficiency as from the inorganic form. Finally, it was found when slightly changing the gas-liquid separator design in order to introduce the mixture of tetrahydridoborate with hydrochloric acid to the bottom of the...
Contribution to optimization of parameters of speciation analysis of As based on selective hydride generation in direct transfer mode and detection by atomic absorption spectrometry
Vyvadilová, Tereza ; Dědina, Jiří (advisor) ; Korunová, Vlasta (referee)
The presented thesis deals with optimization of parameters speciation analysis based on a selective hydride generation in a direct transfer mode of hydrides and on-line atomization in an atomic absorption spectrometer. In the first part of the thesis processes during generation were investigated. Important indicator of a reactions taking place in a generator is volume of hydrogen (created by decomposition of NaBH4) which is subsequently introduced to the atomizer. In this part of the thesis a new approach to determine a flow rate of hydrogen delivered to the atomizator was developed. An influence of relevant paremeters of the atomizers and atomic absorption spectrometers on basic analytical characteristics of arsenic determination based on hydride generation was performed in the second part. Three atomic absorption spectrometers were used and three sources of radiation were compared. The most important analytic characteristic was the limit of detection which is influenced by standard deviation of measurement values of blank samples and by sensitivity. The best values of the limit of detection were achieved with electrodeless discharge lamps. Key words: hydride generation, arsenic, speciation analysis, atomic absorption spectrometry
Speciation Analysis of Selected Mercury Compounds Using HPLC, UV-Photochemical Cold Mercury Vapor Generation and its AAS Detection
Linhart, Ondřej ; Červený, Václav (advisor) ; Spěváčková, Věra (referee)
The mercury occurs in the environment in a variety of forms. Mercury compounds can be found in the soil, atmosphere, water and living organisms. Although some of the mercury substances are very toxic, they are often used in various sectors of industry, agriculture and medicine. Mercury compounds differ in their toxicity, so it is necessary to do speciation analysis. The aim of this diploma thesis was to develop and validate a new analytical method for the determination of mercury compounds in different samples. This method involves the combination of high performance liquid chromatography, UV-photochemical cold vapor mercury generation and atomic absorption spectrometry. Effective separation of mercury(II), methylmercury(I), ethylmercury(I) and phenylmercury(I) ions and subsequent comparable efficient of mercury cold vapor generation from all of forms was achieved using these techniques. The reached detection limits were 8 µg l-1 , 31 µg l-1 , 16 µg l-1 and 38 µg l-1 . At the end of experimental work, the proposed method of RP-HPLC-UV-CVG- QTAAS was used for the determination of mercury compounds in real samples (fish tissue and water samples: Labe, Vltava and tap water) and in certified reference materials (DORM-3 and DOLT-4). Several methods for extraction of mercury species from solid samples...

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