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Multicomponental Preconcentration of As, Sb, Se and Te on Modified Silica, Their Determination by ICP-AES (ICP-MS) and Application for Waters
Urbánková, Kristýna ; Řehůřková, Irena (referee) ; Kanický, Viktor (referee) ; Ventura, Karel (referee) ; Sommer, Lumír (advisor)
The determination of inorganic speciations of arsenic, antimony, selenium and tellurium in natural waters demands often separation and preconcentration. Solid phase extraction is a very effective method for these purposes. In this paper the separation and preconcentration of these microelements is realised on the basis of modified silica Separon SGX C18, SGX C8, SGX CN, SGX NH2, SGX Phenyl and strongly basic anion Exchanger SGX AX. The sorption was provided in the presence of cationic surfactants such as benzyldimethyl dodecylammonium bromide (Ajatin), benzyldimethyltetradecylammonium chloride (Zephyramine), 1-ethoxycarbonylpentadecyltrimetrhylammonium bromide (Septonex) and selected complexing agents 4-(2-pyridylazo)resorcinol (PAR), 8-hydroxyquinoline-5-sulphonic acide (8-HQS), 1,2-dihydroxybenzene (PYR), amonium 1-pyrrolidinecarbodithioate (APDC), sodium diethyldithiocarbamate (DTC) or thiourea(Thur). The interactions of the formed ion associate with the sorbent shows a complicated character which has not been cleared as yet. The previous conditioning of the sorbent plays an outstanding role. Thus, the sorption efficiency was studied in the presence and absence of surfactant and of selected organic complexing agents. Moreover, the influence of pH of the sorbed solution as well as the speed and the volume of the solution running through the sorbent and the type and volume of the eluent on the resulting sorption efficiency was evaluated. The sorption was successfully carried out from 50-1000 ml of solution which allows the 100 fold increase of the preconcentration factor and the determination of the microelements in g.l-1 instead of mg.l-1 by using the common ICP-AES. The influence of macroelements occurring in waters as well as B, Be, Bi, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Sr, Ti, V and Zn in comparable concentrations involve less than 5% error. After the quantitative elution of microelements, the organic solvents were evaporated under IR lamps prior to the determination by ICP-AES and |ICP-MS. The conditions for the direct determination of arsenic, antimony, selenium and tellurium in g.l-1 with ICP-MS were also described in detail in the absence and presence of internal standards Ge and Bi. However, even in this case the preconcentration on silica in the presence of surfactant and selected organic complexants was also tested. When the sorption was followed from 500 ml a 50 fold enrichment factor is reached and the sensitivity for the microelements is improved. The direct determination and the sorption of microelements were applied on synthetic and real waters (dirinking, surface, mineral and sea waters). Instrumental and practical detection limits for various water samples were evaluated according to IUPAC. The results from 1000 ml solution of real waters after sorption on modified silica and the final determination of microelements with ICP-AES were compared with those from ICP-MS without sorption using the method of standards addition in the presence of suitable internal standards. By comparison of results for synthetic and real water samples the error of the determination of microelements was evaluated.
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Optimization and using mercury determination in air.
POSPÍCHAL, Aleš
In this master thesis, during 2009, 2010 and 2011, has been done measurement of total content of mercury in ambient air and soil air in urban and rural locations agglomeration of České Budějovice. The goal was to develop suitable method in order to provide sampling of air to evaluate rate of contamination from chosen locations. The aquaristic compressor was used for admission of air, thus collected air could pass through external amalgamator, which secured pre-concentration of mercury from air. Consecutively, captured mercury has been determined in laboratory by atomic absorption spectrometer AMA-254. In urban background locations has been found total average concentration of mercury in rate 4,01 +/- 3,5 ng.m-3 and urban locations influenced by traffic in rate 29,5 +/- 50,07 ng.m-3. The concentration of mercury in soil air taken from filter bed of constructed wetland (CW) was 16 +/- 9,44 ng.m-3 with average mercury flux 14,5 +/- 8,3 ng.m-2.h-1. In rural compared location has been concentration of mercury in rate 15,4 +/- 7,83 ng.m-3 and mercury flux in soil air was 16 +/- 9,3 ng.m-2.h-1 at this location. Significant differences in contamination of mercury among partial locations have not been ascertained to the exception. The statutory limit for amount of mercury in atmosphere is 50 ng.m-3, whose value has not been mostly reached in any of measured locations. Thus, it has been proved that air contamination is low at selected locations.
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