Este trabalho de mestrado tem o intuito de caracterizar plasmas do tipo indutivo (ICP). Para a caracterização do plasma, foram usadas técnicas de espectroscopia e medidas elétricas. Foram analisados plasmas de Argônio, por ser um gás inerte, oxigênio, por ser um pouco eletronegativo, SF6, por ser um gás muito eletronegativo e útil para a corrosão de silício, misturas de oxigênio e SF6 com Ar, CF4 e misturas de CF4 com Ar. Observou-se que obtêm-se plasmas indutivamente acoplados quando se cria uma condição de concentração mínima de elétrons livres no plasma. Isso acontece quando há uma certa potência aplicada no eletrodo e outra potência aplicada na bobina. Quanto menos eletronegativo o gás, menores são estas potências. Nos casos estudados significa que é mais fácil obter acoplamento indutivo com Ar puro, depois com as misturas dos gases. Em nosso reator foi mais difícil conseguir obter plasmas indutivamente acoplados com O2 e SF6 puros, pois não tivemos condições de “hardware" para aplicar as potências altas as suficientes para criar o plasma indutivo. Também estudamos dois materiais como material de eletrodo, estanho e alumínio e observamos que para o SF6 há uma maior concentração de F com eletrodo de Sn enquanto para CF4 a concentração de F e maior com eletrodo de Al. / In this work, inductively coupled plasmas have been studied, using optical emission spectroscopy and electrical measurements. Four gases were analysed : argon, being an inert gas, oxygen because it is slightly electronegative, SF6 because it is very eletronegative and also etches silicon and its compounds and CF4 because it also etches silicon and its compounds and is slightly electronegative. Also the mixtures of oxygen, SF6, important to silicon etching and CF4 with argon were studied. The studies indicated that it is necessary to have a minimum concentration of free electrons in the plasma to obtain an inductively coupled plasma. This depends very strongly on the power levels applied to the cathode and the coil of the reactor, The less electronegative the gas, the lower these power levels. Hence it was easiest to obtain argon inductively coupled plasmas, followed by the argon mixtures and with the pure gases it more difficult to obtain ICP plasmas with the available hardware. Two materials were studied as cathode material: tin and aluminium. When using SF6, the highest F concentration was obtained with the tin electrode, but for CF4 gases, the highest fluorine concentration was obtained with the aluminium electrode.

Paderborn, Universiẗat-GH, Diss., 1993. / Paderborn, Univ. Gesamthochsch., Diss., 1993.

Este trabalho de mestrado tem o intuito de caracterizar plasmas do tipo indutivo (ICP). Para a caracterização do plasma, foram usadas técnicas de espectroscopia e medidas elétricas. Foram analisados plasmas de Argônio, por ser um gás inerte, oxigênio, por ser um pouco eletronegativo, SF6, por ser um gás muito eletronegativo e útil para a corrosão de silício, misturas de oxigênio e SF6 com Ar, CF4 e misturas de CF4 com Ar. Observou-se que obtêm-se plasmas indutivamente acoplados quando se cria uma condição de concentração mínima de elétrons livres no plasma. Isso acontece quando há uma certa potência aplicada no eletrodo e outra potência aplicada na bobina. Quanto menos eletronegativo o gás, menores são estas potências. Nos casos estudados significa que é mais fácil obter acoplamento indutivo com Ar puro, depois com as misturas dos gases. Em nosso reator foi mais difícil conseguir obter plasmas indutivamente acoplados com O2 e SF6 puros, pois não tivemos condições de “hardware” para aplicar as potências altas as suficientes para criar o plasma indutivo. Também estudamos dois materiais como material de eletrodo, estanho e alumínio e observamos que para o SF6 há uma maior concentração de F com eletrodo de Sn enquanto para CF4 a concentração de F e maior com eletrodo de Al. / In this work, inductively coupled plasmas have been studied, using optical emission spectroscopy and electrical measurements. Four gases were analysed : argon, being an inert gas, oxygen because it is slightly electronegative, SF6 because it is very eletronegative and also etches silicon and its compounds and CF4 because it also etches silicon and its compounds and is slightly electronegative. Also the mixtures of oxygen, SF6, important to silicon etching and CF4 with argon were studied. The studies indicated that it is necessary to have a minimum concentration of free electrons in the plasma to obtain an inductively coupled plasma. This depends very strongly on the power levels applied to the cathode and the coil of the reactor, The less electronegative the gas, the lower these power levels. Hence it was easiest to obtain argon inductively coupled plasmas, followed by the argon mixtures and with the pure gases it more difficult to obtain ICP plasmas with the available hardware. Two materials were studied as cathode material: tin and aluminium. When using SF6, the highest F concentration was obtained with the tin electrode, but for CF4 gases, the highest fluorine concentration was obtained with the aluminium electrode.

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.

No description available.

[pt] Os elementos de maior interesse no biodiesel são os resíduos de catálise do processo produtivo (Na e K), os delimitados por legislação ambiental vigente (S, por exemplo) e os elementos venenosos aos catalisadores automotivos (Pb, V, P e Hg); porém, pesquisas orientadas no sentido de produzir metodologias analíticas para a realização de determinações em biodiesel vêm buscando um mapeamento elementar mais completo do combustível. Técnicas como ICP OES, ICP-MS com célula de reação/colisão, FAAS, GFAAS têm sido usualmente empregadas em determinações diretas ou não, mas ainda existem combinações de preparo de amostra e técnica analítica a ser pesquisadas. O presente trabalho teve como objetivo a avaliação de um sistema de decomposição ácida de amostra de biodiesel, visando à decomposição ácida da maior quantidade possível de matéria orgânica presente na matriz e a consequente determinação em ICP-MS. O processo de decomposição ácida, avaliado pela concentração de carbono residual, determinado em ICP OES, não requer grandes quantidades nem de energia térmica e nem do agente oxidante e ainda permite, após processo de redução da matriz nítrica remanescente, uma determinação direta em ICP-MS utilizando padrões aquosos na confecção das curvas e sem a necessidade de célula de colisão/reação. Foram determinados Ag, Ba, Cu, Mn, Mo, Ni, Ti e Zn em amostras de biodiesel de 4 matérias-primas diferentes e em duas amostras certificadas de biodiesel (NIST) e, tanto os resultados de recuperação, que variaram entre 90 e 110 por cento, quanto o comparativo realizado com as metodologias por ICP OES, validaram os resultados. / [en] Biodiesel appeared in this scenario as an alternative short-term, compatible with the current technologies and without the necessity of major modifications. The elements of greatest interest are the residue of catalyst of the production process (Na, K), those limited by environmental regulations (S) and those that act like poisons for the catalyst system of vehicles (Pb, V, P and Hg), but researches aimed to produce analytical methodologies for determinations in Biodiesel, have sought to achieve a multielement mapping of the fuel (Woods ET AL, 2007). Techniques like ICP OES, ICP-MS with reaction cell, FAAS, GFAAS have been usually used in direct or indirect determinations, but still there are combinations of sample preparation and analytical techniques to be studied. This present work sought to evaluate an analyzing system in ICP-MS after a digestion procedure looking for the minimal quantity of organic matter at the final sample. The preliminary results showed that the digestion process, evaluated by the concentration of residual carbon determined by ICP OES, it can be fast and does not require large amounts of energy and oxidizing agent. And still allow, after reducing the nitric matrix, the use of aqueous standards at the calibration curve. It was monitored Ag, Ba, Cu, Mn, Mo, Ni, Ti and Zn in 4 different sources of raw material for biodiesel, and the method was validated by the analysis of two NIST standards by the comparison with ICP OES results and by the recover results ranged between 90 and 110 per cent.

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Determination of metal in milk powder and soil by slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry

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