Análise de especiação redox de arsênio in situ usando a técnica de difusão de filmes finos por gradiente de concentração
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Data
2013-09-18
Autores
Rolisola, Ana Marta Cavinato Marchini [UNESP]
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
A técnica de difusão em filmes finos por gradiente de concentração (DGT - diffusive gradients in thin films) está entre as ferramentas analíticas usadas para análise de especiação de metais e semimetais. Esta técnica é capaz de fornecer as concentrações médias por tempo, pré-concentração do elemento e amostragem in situ. Nesta pesquisa, a determinação de As(V) pela técnica DGT foi realizada usando a resina de troca aniônica fortemente básica Amberlite IRA 910, seletiva para a retenção do mesmo; enquanto que o hidróxido férrico foi utilizado para a determinação do arsênio total. A concentração de As(III) foi obtida pela diferença entre ambos. Foram também avaliadas, a membrana de troca aniônica fracamente básica DE81 e a resina de troca aniônica fortemente básica Amberlite IRA 410. A resina de troca aniônica fortemente básica Amberlite IRA 910 apresentou melhor desempenho nas condições testadas. O DAs(V) em agarose 1,5 % (m/v), na presença de cloreto de sódio obtido por curva de imersão foi de 4,59 ± 0,43 x 10-6 cm2 s-1 e, o obtido pela câmara de difusão foi de 6,33 ± 0,21 x 10-6 cm2 s-1. A retenção de As(V) pela resina Amberlite IRA 910, apresentou melhor linearidade para um tempo de imersão de 8 h. Do mesmo modo, a melhor retenção de As(V) foi observada na faixa de pH entre 5,0 e 9,0 e, força iônica entre 0,001 mol L-1 a 0,05 mol L-1. Dentre os potenciais interferentes aniônicos, o sulfato demonstrou ser o ânion que mais interferiu na retenção de As(V), enquanto o carbonato apresentou menor interferência. A metodologia desenvolvida foi aplicada para análise de especiação de arsênio inorgânico em amostras sintéticas com diferentes concentrações de As(III) e As(V) e os resultados obtidos pela DGT ficaram próximos aos valores esperados. Para a análise de amostras coletadas no Córrego Furnas, a recuperação...
The diffusive gradients in thin films (DGT) technique is among the analytical tools used for speciation analysis of metals and semimetals. The DGT is able to provide average concentrations by time, pre-concentration of the element and in situ sampling. In this research, the determination of As(V) by DGT technique was possible using a strongly basic anion exchange resin, Amberlite IRA 910, selective for accumulating As(V), while ferrihydrite was used for measuring the total arsenic. The As(III) concentration was obtained by the difference between both. The DE81 weakly basic anion exchange membrane and strongly basic anion exchange resins Amberlite IRA 410 were also investigated for selective sampling of As (V). The resin Amberlite IRA 910 has shown the best performance. Diffusion coefficients of the As(V) obtained by immersion curves and diffusion cell were 4.59 ± 0.43 x 10-6 cm2 s-1 e 6.33 ± 0.21 x 10-6 cm2 s-1 respectively. Both experiments were carried out using 1.5 % m/v agarose as diffusive layer and sodium chloride as ionic strength electrolyte. The As(V) accumulated by IRA 910 shown the best linear range for immersion times of up to 8 hours. While the range of pH 5.0 – 9.0 and ionic strength from 0.001 mol L-1 to 0.05 mol L-1 were the best working conditions. These rates are among the common values found in surface water. Among the potential interfering anions, the sulfate anion interfere the most in the As(V) retention while carbonate showed the least interference. The proposed methodology was applied to speciation analysis of inorganic arsenic on synthetic samples with different concentrations of As(III) and As(V), and the obtained results by DGT were close to expected values. For the analysis of spiked samples collected in Furnas Stream, the recoveries for total arsenic were between 103.9 % and 118.8 %... (Complete abstract click electronic access below)
The diffusive gradients in thin films (DGT) technique is among the analytical tools used for speciation analysis of metals and semimetals. The DGT is able to provide average concentrations by time, pre-concentration of the element and in situ sampling. In this research, the determination of As(V) by DGT technique was possible using a strongly basic anion exchange resin, Amberlite IRA 910, selective for accumulating As(V), while ferrihydrite was used for measuring the total arsenic. The As(III) concentration was obtained by the difference between both. The DE81 weakly basic anion exchange membrane and strongly basic anion exchange resins Amberlite IRA 410 were also investigated for selective sampling of As (V). The resin Amberlite IRA 910 has shown the best performance. Diffusion coefficients of the As(V) obtained by immersion curves and diffusion cell were 4.59 ± 0.43 x 10-6 cm2 s-1 e 6.33 ± 0.21 x 10-6 cm2 s-1 respectively. Both experiments were carried out using 1.5 % m/v agarose as diffusive layer and sodium chloride as ionic strength electrolyte. The As(V) accumulated by IRA 910 shown the best linear range for immersion times of up to 8 hours. While the range of pH 5.0 – 9.0 and ionic strength from 0.001 mol L-1 to 0.05 mol L-1 were the best working conditions. These rates are among the common values found in surface water. Among the potential interfering anions, the sulfate anion interfere the most in the As(V) retention while carbonate showed the least interference. The proposed methodology was applied to speciation analysis of inorganic arsenic on synthetic samples with different concentrations of As(III) and As(V), and the obtained results by DGT were close to expected values. For the analysis of spiked samples collected in Furnas Stream, the recoveries for total arsenic were between 103.9 % and 118.8 %... (Complete abstract click electronic access below)
Descrição
Palavras-chave
Water - Composition, Agua - Composição, Arsênio - Especiação química, Águas superficiais, Arsênio - Toxicologia, Filmes finos, Difusão, Corumbataí, Rio, Bacia (SP), Gradiente de concentração, Arsênio
Como citar
ROLISOLA, Ana Marta Cavinato Marchini. Análise de especiação redox de arsênio in situ usando a técnica de difusão de filmes finos por gradiente de concentração. 2013. 97 f. Dissertação (mestrado) - Universidade Estadual Paulista Júlio de Mesquita Filho, Instituto de Geociências e Ciências Exatas, 2013.