112 resultados para Extração em fase sólida


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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Pós-graduação em Química - IQ

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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This study evaluated the bioaccumulation of tributyltin (TBT) by the blue crab (Callinectes sapidus). Animals were fed with contaminated food containing 30 µg g-1 of TBT expressed as Sn. The analytes were determined in the gills, hepatopancreas and muscle. Acid digestion was used in the total Sn determination, and a solid-phase extraction technique was used for the selective determination of TBT. Limits of detection of 44.6 and 4.46 ng g-1 were found for HG-ICP OES (hydride generation-inductively coupled plasma optical emission spectroscopy) and ICP-MS (ICP-mass spectrometry), respectively. The results for non-contaminated animals were below 50 ng g-1, while the animals subjected to the contaminated food showed higher tissue concentrations of Sn (until 6229 ng g-1) and TBT (until 3357 ng g-1) related to the number of exposure days. According to the results, Sn is bioaccumulated by the blue crab in higher concentrations in the hepatopancreas. For most of these animals, the results suggest that Sn is bioaccumulated as TBT.

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Pós-graduação em Química - IQ

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In order to enable the reuse of the large surplus volume of petroleum produced water for irrigation of crops inedible, the quality evaluation of this water is very important. This work aimed to evaluate the effectiveness of the diffusive gradient in thin films technique (DGT) for the determination of labile Cu (II), Mn (II) and Zn (II) in petroleum produced water destined to reuse in agriculture. Samples were collected at the exit of the wastewater treatment plant (WWTP) (after separation oil/water and flotation) of a Petrobrás onshore production region. Basically, the laboratory experiments with DGT devices involved the evaluation of the behavior of the main variables of the technique for determination of analytes in the samples (diffusion coefficients, immersion time, fractionation of organic and inorganic species, and performance of diffusion gels with different porosities, among others). Also, experiments were conducted based on the solid phase extraction (SPE) protocol with Chelex- 100 resin using previously established protocols to support the study. During the project the possibility of in situ immersions in water treatment plants was evaluated. The DGT technique presented satisfactory results for determination of Mn in produced water, and can be used for in situ determinations. However, the results obtained for Cu and Zn show the need of additional studies

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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The studies of this work aimed to determine the labile fractions of manganese (Mn) in natural and drainage water samples collected around the Osamu Utsumi uranium mine, located in the municipality of Caldas, south-central region of Poços de Caldas- MG, using the technique of diffusion gradient in thin films (DGT). The DGT devices were mounted with Chelex-100 resin, polyacrylamide-agarose hydrogel (conventional porosity) and cellulose acetate membrane. The device were deployed up to 48 hours in six water samples collected from different areas around the uranium mine (075, 076, 022-E, 025-E, 014, and 041). The DGT devices immersed in each sample were gradually removed after 4, 8, 12, 24 and 48 hours. The pH of the samples ranged from 3.0 to 10.5, which influenced the lability and the sampling of the analyte by the Chelex-100 resin. The results showed a linear relationship between accumulated mass and sampling time (immersion curve) for samples 014 and 025-E (pH between 6 and 8) suggesting the ability of the DGT technique for sampling the analyte. The results obtained for samples 075 and 076 (pH<5) and samples 041 and 022-E (pH around 10) were characterized by nonlinear relationships. The values obtained by DGT were compared with Solid Phase Extraction (SPE) technique using Chelex-100. For samples 014 and 025-E, there was a good agreement between the results obtained by both techniques

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Métodos comparativos foram desenvolvidos para detectar e quantificar o corante solvente azul 14 (SA-14) em amostras de combustíveis. O método eletroanalítico foi baseado na técnica de voltametria de onda quadrada (VOQ) com detecção em +0,60 V vs. Ag/AgCl sobre o eletrodo de carbono vítreo, usando tampão Britton-Robinson e N, N-dimetilformamida (1:1, v/v) como eletrólito suporte. Para metodologia, envolvendo a cromatografia líquida de alta performance (CLAE) foi empregada uma fase móvel composta de acetonitrila e cloreto de lítio (85:15, v/v) e a detecção eletroquímica foi realizada em um potencial de oxidação em +0,65 V vs. Ag/AgCl. Sob as melhores condições de trabalho curvas de calibração foram obtidas, para ambos os métodos, as quais foram lineares na faixa de concentração de 5,0Ã10 -7 a 6,0Ã10 -6 mol L-1 (VOQ) e 8,0Ã10 -8 a 3,0Ã10 -6 mol L-1 (CLAE). Os métodos foram aplicados para quantificar o corante em amostras de álcool e querosene após um simples processo de extração em fase sólida com resultados de recuperação satisfatórios.