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Preconcentration of Trace Analytes on Modified Sorbents and their Determination on Waters
Holubová, Zuzana ; Čelechovská, Olga (referee) ; Holoubek,, Ivan (referee) ; Otruba,, Vítězslav (referee) ; Sommer, Lumír (advisor)
The work has been focused on the preconcentration techniques for determination of 9Be, 51V, 59Co, 60Ni, 89Y, 111Cd, 208Pb, 232Th and 238U on the modified sorbents, all measurements were performed on ICP-MS. The instrument setup was optimized. The solution of internal standard (200 µg•l-1) was used during all measurements. The internal standard were chosen as follows: 6Li for 9Be, 45Sc (51V), 72Ge (59Co, 60Ni, 89Y), 103Rh (111Cd), 209Bi (206Pb, 207Pb, 208Pb, 232Th and 238U). Another parameters such as influence of mineral acids (HCl, HNO3), surfactant (Septonex®, Zephyramin, Ajatin, Brij 35 and Sodium dodecyl sulphate) and organic reagents (Ammonium pyrrolidinedithiocarbamate, 8-Hydroxyquinoline-5-sulphonic acid, 1,2-Dihydroxyanthraquinone-3-sulphonic acid and 4-(2-Pyridylazo)resorcinol) and the effect of some matrix components on intensity of instrument signal determination was investigated. For preconcentration polar Silicagel and modified nonpolar Silicagels (Silicagel-C18, C8 nad Phenyl) were used. Another experimantal part was dedicated to preconcentration on nonpolar Amberlite XAD-16 and Strata SDB-L and intermediately polar sorbent Amberlite XAD-7. Recoveries of sorption process were observed in the presence of all testing types of surfactants in certified concentration 5•10-4 mol•l-1. Surfactants were always applied in the conditioning step. The suitable combinations of surfactant and organic reagent were tested for increasing of recoveries of analytes. Testing organic reagents were added in five times mass excess againts concentration of analytes, the concentration of the organic reagents was 900 µg•l-1. The organic reagent was always added to the solution for preconcentration before this solution was led on the sorbent. The composition and a necessary volume of elution mixture for quantitative elution were tested, too. Only one sorbent was chosen from each group of sorbents with similar properties. The chosen sorbent showed the best recoveries in majority of target analytes. The highest recoveries from silica-group was reached for Silicagel-C18, from nonpolar Amberlite was chosen Strata SDB-L and intermediately polar Amberlite XAD-7. The influence of some matrix components (anionts and cations) on recoveries of analytes was investigated for chosen sorbent. The optimized process was applied on real samples of nature water and industry water. In experimental part all analytes are marked as specific izotopes, which were measured by ICP-MS. Of course, all izotopes of analytes undergo preconcentration techniques.
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Preconcentration Techniques for Determination of Uranium Using the Modified Sorbents.
Moos, Martin ; Řehůřková, Irena (referee) ; Kanický, Viktor (referee) ; Kráčmar, Stanislav (referee) ; Sommer, Lumír (advisor)
The work has been focused on the preconcentration techniques for determination of uranium on the modified sorbent, with the final use of ICP-OES and ICP-MS. First ICP-OES at a wavelength of 385.958 nm was used for determination of uranium. Parameters were optimized and the effect of mineral acids (HCl, HNO3), tensides (Septonex, Ajatin) and organic reagents like (4-(2-pyridylazo)resorcinol, ammonium pyrrolidinedithiocarbamate, 8-hydroxyquinoline-5-sulphonic acid and 1,2-dihydroxyanthraquinone-3-sulphonic acid) was observed. For ICP-MS an isotope 238U was chosen. As an internal standard 209Bi (200 ?g•l-1) was used. Modified silica gel was used (Silicagel tethered with C18, C8 alkyls and phenyl) and two types of Amberlite XAD 4 and XAD 16 for the preconcentration of uranium (VI). Commercially produced Amberlite was modified as follows: Drying at 100 °C (24 hours), milled, minced sorbent was selected and fractionated to particles size ranging from 0.32 to 0.63 ?m and finally activated in methanol. The deionised water and Septonex (5•10-3 mol•l-1) at pH 8 were used for Amberlite conditioning. The optimal sorption of uranium (VI) proceeded at pH 8 in the presence of 4-(2-pyridylazo)resorcinol or ammonium pyrrolidinedithiocarbamate with Amberlite XAD-16 moreover with 1,2-dihydroxyanthraquinone-3-sulphonic acid. All organic reagents have mass concentration five time larger than uranium . For the elution of uranium the mixture of 1 mol•l-1 HNO3 with acetone (ratio of 1:1) was used. Acetone was evaporated and the final analysis performed using ICP-OES. The preconcentration of uranium (VI) using Silicagel-C18 conditioning was performed with ethanol, deionised water and Zephyraminu (5•10-4 mol•l-1) at pH 8. For the Silica-C8 and Silicagel-Phenyl the same conditioning procedure without zephyramin was used. Silica-C18 had the highest sorption efficiency with 1,2-dihydroxyanthraquinone-3-sulphonic acid, Silicagel-C8 with ammonium pyrrolidinedithiocarbamate and Silicagel-Phenyl with 8-hydroxyquinoline-5-sulfonic acid, all organic reagents have mass concentration five time larger than uranium concentration. As an optimal elution mixture acetone and ethanol (ratio of 1:1) in the presence of 1 mol•l-1 HCl was evaluated. Acetone and ethanol was evaporated and the final analysis was performed using ICP-MS. Silicagel-C18 was evaluate as the most effective in the presence of zephyramin and 1,2-dihydroxyanthraquinone-3-sulphonic acid. Sorption was also tested in the presence of 20 ?g•l-1 microelements (Be, V, Co, Ni, Y, Pb, Th, Cd) and in the presence of a defined concentrations of K, Na, Ca, Mg, Al and Fe. Direct analysis of uranium was carried out on samples of water from the river Ploucnice and Turonian aquifers containing uranium, 3,5 and 19,3 ?g•l-1. Different type of water required preconcentration of uranium (VI) on Silica-C18 in the presence of 1,2-dihydroxyanthraquinone-3-sulphonic acid and zephyramin. The analysis results gave statistically satisfactory results, which were confirmed using standard addition of 20 ?g•l-1.
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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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Determination of toxic elements in wines
Hajdučková, Iva ; Vespalcová, Milena (referee) ; Diviš, Pavel (advisor)
The aim of this study was to determine the occurrence of selected toxic elements in wine. The theoretical part described technology of wine production and selected toxic elements (cadmium, lead, copper, zinc, nickel and chromium) in the terms of their impact on wine quality and their effects on the human organism. It provides an overview of instrumental analytical methods, which can be used for the analysis of toxic metals. In the experimental part inductively coupled mass spektrometry technique was used for the analysis of wine samples. The measured values are statistically processed and compared with current legislation.
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Possibilities of determining the origin of the wine from the element composition
Škařupa, Přemysl ; Gregor,, Tomáš (referee) ; Diviš, Pavel (advisor)
The aim of this diploma thesis was to evaluate the possibility of determining the origin of the wine on the basis of elemental composition. For this purpose an analysis of major and minor elements was accomplished in selected varieties of wines. In total, 48 parameters for six wine subregions in Bohemia and Moravia was determined and used. The sum of 35 parameters represented the concentration of selected elements and other 13 parameters were created from the measured values. The concentration of elements was determined by inductively coupled plasma mass spectrometry (ICP-MS). For the purpose of classification of samples into groups multivariate statistical methods were used. The measured data set was firstly separated using analysis of variance (ANOVA) and discriminant analysis (DA). It has been proved that the selected variables influence the distribution of wines into categories according to their geographic location. Canonical discriminant analysis, principal component analysis (PCA) and cluster analysis has been used for graphical projection. Simultaneously the model based on our analysis was created to enable classify an unknown sample of wine according to the origin.
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Determination of selected metals in unconventional fruit species
Křížová, Soňa ; Dočekalová, Hana (referee) ; Diviš, Pavel (advisor)
The aim of this diploma thesis is determination of selected metals in unconventional fruit species, specifically in cornelian cherry (Cornus mas), sea buckthorn (Hippophae rhamnoides) and medlar (Mespilus germanica).There is informationabout 16 analysed metals – As, B, Be, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Se, Sn, Pb, V, Zn. There are described analytical techniques for elemental analysis and methods for destruction biological material. Samples for analysis are prepared by using microwave mineralization and ICP-MS for detection. This is described in the experimental part of the diploma thesis. Analysis confirmed that unconventional fruits are rich sources of trace elements.
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Determination of selected metals in fruit squashs
Drobilová, Marcela ; Vránová, Dana (referee) ; Diviš, Pavel (advisor)
The theoretical part of the thesis deals with the technology of fruit juices production and characteristics of the known varieties of elderberry. There are also summarized available information on the presence and properties of minerals in food. In the practical part of the thesis 17 different varieties of elderberry juice and commercially available juice sold as food supplements were analyzed using ICP-MS technique. The concentrations of 15 selected essential and toxic elements were determined in these juices.
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Determination of alergenic and potential alergenic metals in cosmetics
Krakovková, Lenka ; Zemanová, Jana (referee) ; Diviš, Pavel (advisor)
The aim of the diploma thesis was to provide an overview of the prevalence of allergenic and potentially allergenic metals in eye shadows. The diploma thesis gives an overview of the legislation on cosmetics and description of the types of allergenic reactions caused by allergenic and potential allergenic metals in eye shadows. Listed below are the preparation methods of the samples for analysis and the list of the methods by which can the selected metals be analyzed. The experimental part of the diploma thesis deals with an analysis of selected allergenic and potentially allergenic metals in eye shadows. In the experimental part of diploma thesis method of sample preparation for analysis of eye shadows and a method of analysis of sample of eye shadows by ICP-MS have been optimized. Monitored analytes were selected metals. Altogether 6 samples of eye shadows from different manufacturers were chosen. Measured results have been statistically processed, confronted with the applicable legislation and assessed in terms of possible allergic reactions.
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Representation of selected elements in human hair
Jochimová, Eva ; Janoušková, Eva (referee) ; Zemanová, Jana (advisor)
Hair is an excellent matrix for monitoring trace elements and minerals in the body. To long-term changes in concentration of elements in the body are reflected in their value in her hair, so the assessment of the organism from the mineral analysis of hair is a very suitable method. This method is widely used in toxicological testing and forensics. This work deals with the analysis of Mg, K, Fe, Zn, Mn, Se, As, Cd and Pb in 100 samples by ICP-MS. It is a male hair samples with the age range 19 – 74 years. Analysis of hair revealed that concentrations of individual elements are moving in a narrow range of values. Values of older age category are in some case significantly deflective.
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