O presente estudo consistiu em caracterizar quimicamente amostras de sedimentos da represa Billings, braço Rio Grande, na região Metropolitana de São Paulo, por meio da determinação da concentração de metais e outros elementos de interesse. Os parâmetros químicos escolhidos para esta caracterização, foram as concentrações de Alumínio, Arsênio, Bário, Cádmio, Chumbo, Cobre, Cromo, Ferro, Manganês, Mercúrio, Níquel, Selênio e Zinco. Esses parâmetros são também utilizados na determinação do Índice de Qualidade das Águas (com exceção do Selênio). As determinações foram efetuadas pelas técnicas analíticas de espectrometria de absorção atômica (FAAS, GFAAS e CVAAS), espectrometria de emissão ótica (ICP OES) e análise por ativação neutrônica (AAN). Essas metodologias analíticas foram avaliadas quanto à precisão, exatidão e limite de detecção e/ou quantificação para os elementos determinados, nas amostras de sedimentos. Foram discutidas também as vantagens e desvantagens de cada técnica utilizada, para cada elemento, dependendo de sua concentração. A partir dessa análise, selecionou-se a técnica mais apropriada para a determinação de cada elemento, para a implementação em análise de rotina de amostras de sedimentos. Dessa forma verificou-se que a digestão efetuada assistida por microondas em sistema fechado com ácido nítrico é eficiente para a quantificação da concentração de metais extraíveis de interesse ambiental. Verificou-se também que as técnicas escolhidas para as determinações dos metais eram igualmente eficientes. No caso dos metais Cd e Pb, com a técnica de FAAS obteve-se resultados melhores do que a técnica de ICP OES, por não apresentar interferência de matriz. Os valores de concentração para os metais As, Cd, Cu, Cr, Hg, Ni, Pb e Zn nas amostras de sedimentos foram comparados com os valores orientadores (TEL e PEL) do Canadian Council of Minister of the Environment (CCME). Esse projeto definiu as técnicas analíticas e parâmetros, para um melhor monitoramento dos níveis de contaminação de sedimentos por metais, fornecendo dados que possam ser utilizados para direcionar atitudes e manejos de sistemas aquáticos. / The present study chemically characterized sediment samples from the Billings reservoir, Rio Grande tributary, in the Metropolitan region of São Paulo, by determining metal concentration and other elements of interest. The chosen chemical parameters for this characterization were Aluminum, Arsenic, Barium, Cadmium, Copper, Chromium, Iron, Lead, Manganese, Mercury, Nickel, Selenium and Zinc. These parameters are also used in the water quality index, with the exception of Selenium. The concentrations were determined through different analytical techniques such as atomic absorption spectrometry (FAAS, GFAAS and CVAAS), optical emission spectrometry (ICP OES) and neutron activation analysis. These analytical methodologies were assessed for precision, accuracy and detection and/or quantification limits for the sediment elements in question. Advantages and disadvantages of each technique for each element and its concentration were also discussed. From these assessment the most adequate technique was selected for the routine analysis of sediment samples for each element concentration determination. This assessment verified also that digestion in a closed microwave system with nitric acid is efficient for the evaluation of extracted metals of environmental interest. The analytical techniques chosen were equally efficient for metals determination. In the case of Cd and Pb, the FAAS technique was selected due to better results than ICP OES, as it does not present matrix interference. The concentration values obtained for metals As, Cd, Cu, Cr, Hg, Ni, Pb and Zn in the sediment samples were compared to Canadian Council of Minister of the Environment (CCME) TEL and PEL values.

No description available.

High-energy ion beam based proton induced x-ray (PIXE) is an ideal analytical tool suitable for simultaneous quantification of trace elements with high accuracy. The quantification of trace elements in solids using PIXE has been well established for over two decades. The main objective of this study is to extend this capability to solids with an inhomogeneous internal structure. In this study, pure GAC and PAC samples were soaked in known concentration of arsenic (As) solution and the trace amount of As uptake was determined during these exposures using PIXE, neutron activation analysis (NAA) and atomic absorption spectroscopy (AAS). There is a good agreement between the values and adsorption mechanisms derived from the NAA and pelletised PIXE measurements and some AAS measurements. Micro-PIXE was used to understand the discrepancies in the As adsorption on the pore and flat surfaces of GAC samples. / Master of Science (Hons) (Physics)

Thesis (Ph. D.)--Ohio State University, 2007. / Title from first page of PDF file. Includes bibliographical references (p. 361-380).

<p> </p><p>Correlation between production method and mineral-, cadmium- and protein content were sought for Swedish winter wheat. The wheat was grown according to conventional, organic or biodynamic principles. The minerals; iron, zinc, magnesium, copper and the heavy metal cadmium were analyzed with atomic absorption spectroscopy. Protein was analyzed with elemental combustion analysis. All together, 17 samples were analyzed; nine from the still ongoing Bollerup field trial in Skåne and eight from four different farm pairs in the midst of Sweden.</p><p>The Bollerup field trials showed that organic wheat had a higher concentration of iron than conventional. Both organic and biodynamic wheat had a higher concentration of zinc than conventional. Magnesium concentration was higher in biodynamic wheat than in conventional grown wheat. Differences between production methods were in the range of 7.5 and 17%.</p><p>No unmistakable connections were found between any of the parameters and production method for the farm pairs. However, a tendency for more minerals in organic/biodynamic wheat was seen for all minerals but iron.</p><p>Due to unclean equipment, analyzing of cadmium contents could not be completed.</p>

Correlation between production method and mineral-, cadmium- and protein content were sought for Swedish winter wheat. The wheat was grown according to conventional, organic or biodynamic principles. The minerals; iron, zinc, magnesium, copper and the heavy metal cadmium were analyzed with atomic absorption spectroscopy. Protein was analyzed with elemental combustion analysis. All together, 17 samples were analyzed; nine from the still ongoing Bollerup field trial in Skåne and eight from four different farm pairs in the midst of Sweden. The Bollerup field trials showed that organic wheat had a higher concentration of iron than conventional. Both organic and biodynamic wheat had a higher concentration of zinc than conventional. Magnesium concentration was higher in biodynamic wheat than in conventional grown wheat. Differences between production methods were in the range of 7.5 and 17%. No unmistakable connections were found between any of the parameters and production method for the farm pairs. However, a tendency for more minerals in organic/biodynamic wheat was seen for all minerals but iron. Due to unclean equipment, analyzing of cadmium contents could not be completed.

Electrochemical hydride generation is an alternative technique to the chemical hydride generation by NaBH4 which is widely used for atomic spectrometric determination of volatile elements such as As, Bi, Ge, Pb, Sb, Se, Sn and Te. The aim of this research has been to develop an analytical technique at the level of ng/L for determination of antimony by using a simple and inexpensive AA spectrometer and the other parts that can be built in any laboratory. Carbon rod and platinum foil were used as cathode and anode materials, respectively, for the generation of antimony hydride. Argon was used as the carrier gas. Zr coated W-coil was used for on-line preconcentration of generated hydrides. A new apparatus independent from quartz T-tube atomizer was constructed and used to contain the atom trap. Zr coated W-trap was heated to the collection temperature for trapping the analyte species generated electrochemically. For the revolatilization of the trapped species, the trap was further heated to the revolatilization temperature. Revolatilized species were transported to a flame-heated quartz tube atomizer where the analytical signal was recorded. Duringcollection and revolatilization steps hydrogen gas was introduced into the system to prevent the oxidation of atom trap. The experimental operation conditions for electrochemical hydride generation and atom trapping were optimized. 3&amp / #963 / limit of detections were found to be 0.012 ng/mL and 0.41 ng/mL with and without using trap, respectively. The trap has provided 34 fold sensitivity improvement as compared with the electrochemical hydride generation alone. The interferences of some hydride forming elements and some transition metals on electrochemical hydride generation with and without employing the trap were investigated. Analysis of standard reference material was performed to check the accuracy of the proposed method.

Antimony is a toxic element which is mostly found in two oxidation states (III and V) in environmental, biological and geological samples. Antimony may form various inorganic and organic compounds that exhibit differences in analytical behavior, toxicity and mobility / inorganic compounds of antimony are more toxic than organic forms and toxicity of Sb(III) has been shown to be 10 times higher than that of Sb(V). Therefore selective determination of Sb(III) and Sb(V) is required in environmental and biological samples. Hydride generation atomic absorption spectrometry is a sensitive, fast and economical technique for the determination of antimony at trace level. A possible non-chromatographic method for antimony speciation is hydride generation atomic absorption spectrometry that is based on the relatively slow kinetics of hydride formation from Sb(V). In this study, continuous flow hydride generation method for the determination of antimony was developed and hydride generation conditions were optimized. Analyte solution was prepared in 0.050 mol/L HCl and 1.2% (w/v) NaBH4 stabilized in 0.30% (w/v) NaOH was used as a reductant solution. Inorganic antimony speciation conditions were determined by continuous flow HGAAS system. For the pre-reduction of Sb(V) to Sb(III), 8.0% (w/v) potassium iodide (KI) and 0.10% (w/v) ascorbic acid were used. Further speciation study was also carried out using Ir coated W-coil Atom Trap Hydride Generation Atomic Absorption Spectrometry. Tungsten coil atom trap was used to enhance the sensitivity. Tungsten coil surface was treated with Ir and totally 250 &amp / #956 / g 1000 mg/L Ir stock solution was used for coating of tungsten coil. LOD and LOQ values were calculated as 152 pg/mL and 508 pg/mL according to 120 seconds trapping. 128 and 37 fold enhancement were obtained for 120 seconds collection with respect to W-coil-ETAAS and ETAAS, respectively.

Determination of thallium is important due to its toxic effects on the environment and human health. Extremely low abundance of thallium in earth crust requires very sensitive and accurate methods for determination of this element. Although volatile compound generation is a sensitive, fast and economical method, thallium determination by this method has not been sufficiently investigated in literature, because of the fact that the formation of volatile forms of this element is a difficult task. A continuous flow volatile compound generation system was developed and parameters that affect the analytical signal were optimized. Sample solutions were acidified with 0.5 mol/L HNO3 and prepared in 0.0005% (v/v) rhodamine B and 1.0 mg/L Pd while 0.5% (m/v) NaBH4 stabilized in 0.5% (m/v) NaOH was used as reductant. Fast decomposition and unstability of thallium volatile species affected system performance negatively. Flow injection volatile compound generation studies were carried out with a special system. After optimizations, LOD and LOQ values were calculated as 12 ng/mL and 40 ng/mL according to peak height values in HNO3 medium. Similarly, in HCl medium LOD and LOQ values were calculated as 14 ng/mL and 45 ng/mL. Addition of Te and Pd to the sample solution containing co-enhancement reagent rhodamine B improved volatile compound generation efficiency in peak height by 3.6 and 9.3, respectively. Type of the acid used was affected peak heights and peak shapes of Tl+ and Tl3+ volatile species and HNO3 medium gave better results. By changing the location of introduction for Ar gas, the sources of memory effects and reasons of peak broadening were investigated. Most of the memory effects were coming from the gas-liquid separator (GLS) or before the GLS, as well as T-tube atomizer. Nature and behavior of Tl volatile species were also investigated and it was found that Tl and also Pd were generated in the form of nanoparticles. Transmission electron microscopic (TEM) measurements prove the presence of Tl nanoparticles in the analyte species transported to the atomizer by the effect of carrier Ar gas.

Thesis (MTech. degree in Chemistry)--Tshwane University of Technology, 2010.