National Repository of Grey Literature 64 records found  1 - 10nextend  jump to record: Search took 0.01 seconds. 
Derivatization of the micro-samples of natural polymers with similar composition for FTIR analysis
Dudičová, Dorota ; Červený, Václav (advisor) ; Dian, Juraj (referee)
in English This master thesis is focused on verifying the possibility of optimizing FTIR spectrometric analysis of terpenic resins using derivatized (fluorinated) samples using XtalFluor-E in combination with triethylamine trihydrofluoride as an agent. Terpenic resins have very similar FTIR spectra, so for their better differentiation, they need to be derivatized to minimize the influence of overlapping spectral bands in FTIR spectra. This work aimed to create a methodology for derivatization of samples of natural polymers for the National Technical Museum in Prague, where the work was performed. Samples of terpenic resins were measured non-fluorinated by the ATR crystal method and by transmission, after fluorination, only the ATR crystal method was used. Different fluorination conditions, different times (2, 4, 6, 24 and 96 hours), the effect of sample rinsing (diethyl ether, ethylene tetrachloride) and the effect of matrix on the sample (KBr pellet) were tested. Fluorination has shown to be effective. Four hours of fluorination and the need to rinse the sample with diethyl ether were chosen as the optimal fluorination conditions. After testing the resins themselves, fluorinated samples of violin varnishes and samples of historical varnishes from harp and piano were analyzed. Their spectra before...
Study of properties of UV-photochemical generation of volatile compounds od antimony
Adámková, Dominika ; Červený, Václav (advisor) ; Hraníček, Jakub (referee)
The master thesis deals with comparison of atomic fluorescence spektrometry and high resolution continuum source atomic absorption spektrometry for three methods generation of volatile compounds Antimony. In both methods of atomic antimony detection, it compares the most common chemical generation of volatile compounds (hydrides) with two alternative methods - electrochemical and UV - photochemical. The values of performance parameters for the determination of Sb(III) and Sb(V) were determined for all the above combinations. In the case of chemical generation, a surprisingly almost four times higher limit of detection of Sb(III) was found in connection with AFS detection than AAS detection. The final part was devoted to UV - photochemical vapor generation, with AAS detection for Sb(III) reaching limit of detection 4,96 ppb, for Sb(V) 8,63 ppb. Although UV - photochemical generation of volatile antimony compounds did not reach such performance parameters as chemical or electrochemical generation, it was observed that the sensitivity of antimony determination increased greatly when introducing oxygen into the apparatus. The interference study also found a significant positive effect of Fe(II) on the generation efficiency, and this modification partially persisted without further introduction of these...
Determination of lead and cadmium in fruits and vegetables extracts by atomic absorption spectrometry
Záškodová, Terezie ; Hraníček, Jakub (advisor) ; Červený, Václav (referee)
The content of this thesis was to analyse fruit and vegetable extracts. In the samples, the concentration of lead and cadmium was determine by atomic absorption spectrometry. First, it was necessary to conduct an optimalization study to find the optimal conditions of the method and select the appropriate method of atomization of the sample. It was chosen between flame and electrothermal atomization. For optimization, the following parameters were studied for atomization in flame: beam height above the burner, fuel flow rate, horizontal burner position, spectral interval width and lamp supply current. An optimization study for electrothermal atomization included the effect of atomization a pyrolysis temperature on signal size. Standard lead and cadmium solutions were used to determine the detection limits of the instruments used. The limit of detection in flame atomization was for lead respectively cadmium 0,002 mg/l, resp. 0,003 mg/l. In electrothermal atomization the detection limit was for lead, resp. cadmium 0,026 μg/l, resp. 0,029 μg/l. The experimentally determined values were statistically processed and the lead and cadmium contents were compared with the lead and cadmium limit values that may be contained in a sample of fruit and vegetables according to Commission Regulation (EC) No...
Comparison of mercury determination by electrochemical or UV-photochemical vapor generation with detection by atomic fluorescence
Šandlová, Petra ; Červený, Václav (advisor) ; Nováková, Eliška (referee)
~ 5 ~ Abstract The functionality of the add-on Millennium Merlin Satellite module towards the PSA Millennium Excalibur atomic fluorescence spectrometer for determination of mercury has been proven. At the same time, the ratios of the average signal to the sample standard deviations of the results of repeated measurements of this module were compared with the mercury determination using an atomic absorption spectrometer ContrAA700 with a radiation source with continuous spectrum and high resolution. In model experiments performed on an atomic absorption spectrometer, the experimental conditions of the cold vapor detection above the level of the elemental mercury were optimized. The flow rate of argon and hydrogen, the temperature of the detection cell and the storage bottle and the mercury evaporation time were optimized. It has been shown that the reduction environment in the detection tube reduces the signal. The need to heat the detection tube up to 650 řC has been surprising. The causes of this phenomenon were discussed and confronted with data from the available literature. Subsequently, the mercury signal was monitored unde roptimal conditions found on the AAS, using an atomic fluorescence PSA Millennium Excalibur spectrometer with an additional Millennium Merlin Satellite unit for mercury...
Determination of cadmium and copper in bood of great tits
Adamová, Simona ; Hraníček, Jakub (advisor) ; Červený, Václav (referee)
EN Monitoring of the environment is one of the most important activities nowadays. This monitoring includes, for example, monitoring the concentration levels of heavy metals in organisms with a defined relationship to the environment. Great tit (Parus major) was evaluated as a suitable indicator of the environment especially for its abundance and presence near human settlements. The target of this bachelor thesis is to determine cadmium and copper in dried blood samples of these birds from several parts of Europe. All samples were prepared using microwave digestion and analyzed using the inductively coupled plasma mass spectrometry, which is known for its ability to determine simultaneously metals in biological samples even at very low concentrations. Key words Inductively coupled plasma mass spectrometry, heavy metals, copper, cadmium, great tit, blood
Analysis of unstable complexes for study of enzymatic methylation of arsenic
Albrecht, Michal ; Petry-Podgórska, Inga (advisor) ; Červený, Václav (referee)
The main aim of this thesis was the development of conjugation of existing methods for analysis of arsenic-glutathione complexes (As-GS complexes) together with simple arsenic species (iAs, MMAs, DMAs) during simple run. The basic technique for analysis of As-GS complexes was the HPLC-ICP-MS method with a reverse phase separation column (C18). The separation problem of simple species has been overcome by extending of system by postcolumn hydride generation with cryotrapping system (HG-CT). The resulting HPLC/HG-CT-ICP-MS system provides a complex analysis of all the above-mentioned analytes. According to the currently available resources, it is an innovative system, where for the first time all the simple arsenic species (iAs, MMAs, DMAs) and the As-GS complexes were separated. Under the given conditions, the detection limit for the As-GS complexes of 1.9 pg cm-3 in the RP-HPLC-ICP-MS system (a quantification limit of 6.5 pg cm-3 ) was achieved at a sensitivity of 468 CPS s pg-1 . The HG-CT-ICP-MS system provided a detection limit for iAs of 1.2 pg cm-3 at a sensitivity of 1121 CPS s pg-1 , for MMAs of 0.043 pg cm-3 at a sensitivity of 895 CPS s pg-1 and for DMAs of 0.076 pg.cm-3 at a sensitivity of 926 CPS s pg-1 . This method was applied to achieve another aim, studying the pathways of enzymatic...
UV-photochemical generation of cadmium volatile compounds with atomic spectrometric detection
Horová, Kateřina ; Nováková, Eliška (advisor) ; Červený, Václav (referee)
The aim of this master's thesis has been to develop and optimize the method of UV- photochemical vapor generation of cadmium volatile compounds for atomic fluorescence spectrometry. Two configurations with different materials wrapped around the low-pressure mercury vapor lamp were tested. I experimentally determined optimal conditions for both systems; the optimalized parametres included selection of photochemical reagent and its concentration, flow rate of liquids and gases, and the lenghth of the reaction coil. After finding the optimal parametres I determined the figures of merit of the method. I found from the measured data that UV-photoreactor with the quartz capillary provided lower limits of detection and thus was more suitable for generation of cadmium volatile compounds. With this arrangement and using the ferrous sulphate heptahydrate as the chemical modifier I obtained limit of detection 2,0 µg·l-1 , limit of determination 7,0 µg·l-1 , linear dynamic rate LOD-50 µg·l-1 and repeatibility 0,35 %. I also carried out the interference study in my thesis and determined the generation effeciency of cadmium volatile compounds. The interference study shows the influence of mineral acids (HCl, H2SO4, HNO3), their salts (NaNO2, NaNO3) and transition metals (Co, Ni, Cu). Based on literature review I also...
Speciation analysis of arsenic and mercury using postcolumn generation of their volatile compounds for needs of atomic spectroscopic methods
Linhart, Ondřej ; Červený, Václav (advisor) ; Spěváčková, Věra (referee) ; Šíma, Jan (referee)
The presented dissertation thesis deals with the use of UV-photochemical generation of volatile compounds (UV-PVG) as a derivatization technique for the combination of high-performance liquid chromatography (HPLC) and atomic absorption spectrometry (AAS) detection. Two model elements arsenic and mercury and their compounds were selected for the speciation analysis. The work was divided into several parts that follow. In the first part of the research, the apparatus for the UV-photochemical generation of the volatile mercury compounds and their detection with a new continuum source and high-resolution atomic absorption spectrometer (HR-CS AAS) with an externally heated detection tube was constructed. The analytical method was adapted for use with atomic fluorescence detection with the aim to improve sensitivity of the determination. Furthermore, apparatus for the electrochemical generation of cold mercury vapor with AAS detection was built. The construction of the apparatus was followed by optimization of the reaction conditions (concentration and flow of electrochemical reagents: sulfuric and hydrochloric acid, mobile phase, carrier medium, flow rate of the carrier gas and localization of its introduction), determination of the analytical figures of merit, and comparation of the methods. Both...

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