Os sedimentos possuem propriedades de acumulação de poluentes e a determinação de elementos tóxicos nessas amostras permite avaliar o seu ciclo geoquímico. Arsênio e mercúrio foram determinados em 28 amostras de sedimento da Bacia do Rio São Francisco, Minas Gerais, Brasil, por geração de hidretos acoplada à espectrometria de absorção atômica (HG AAS). Foram empregados procedimentos de digestão pseudo-total empregando HCl:HNO 3 (3:1 v/v) e extração parcial com HCl 1 mol L -1 . Realizou-se ainda a determinação de Hg nas amostras sólidas, utilizando-se um analisador direto de mercúrio. Observou-se que 46% das amostras apresentaram concentrações de As acima do limite de nível 1 estabelecido pela Resolução 344/2004 do CONAMA e que 14% excederam o limite de nível 1 para Hg. As amostras com altas concentrações de Hg foram também analisadas por termodessorção acoplada à espectrometria de absorção atômica (TDAAS) para especiação e os termogramas apontaram somente a presença da espécie Hg(II).Sediments have metal accumulation properties, then, an evaluation of their geochemistry cycle is feasible via toxic element determination of these samples. Arsenic and mercury determinations were accomplished in 28 sediment samples from the São Francisco River Basin, Minas Gerais, Brazil. For sample pretreatment were employed a pseudo-total digestion procedure with HCl:HNO 3 (3:1 v/v) and a partial extraction procedure with 1 mol L -1 HCl. Arsenic and mercury were analysed by hydride generator atomic absorption spectrometry (HG AAS). Mercury determination was realized in the solid samples by direct mercury analyzer (DMA). It was observed that 46% of the samples presented arsenic concentrations above Brazil's legal limits, and 14% of samples exceeded the established mercury limit. The samples with high mercury content were also analysed by thermodesorption coupled to atomic absorption spectrometry (TDAAS) and only Hg(II) was identified.Keywords: arsenic, mercury, sediment samples, environmental monitoring, São Francisco River IntroductionIn most aquatic environments, dissolved metal concentrations in overlying water are low due to the precipitation of solids or the adsorption of suspended particles and the deposition of these particles as sediments. 1 Sediment is a matrix comprising inorganic and organic particles. It is relatively heterogeneous in terms of its physical, chemical, and biological characteristics. Sediments have an important role in the transport and storage of contaminants, being of high relevance in the identification of contaminant sources and in the determination of dispersion pathways. Sediment quality determines the biodiversity and the ecological health in aquatic systems as well as being economically important in the environmental assessment of coastal areas. 2 São Francisco is the third largest hydrographic basin in Brazil. It is responsible for drainage of a 640.000 km² area, corresponding to 8% of land in the country of Brazil. About 40% of the basin is located in the state of Minas Gerais and it is divided ...

Paracatu River Basin, Minas Gerais, Brazil, houses long areas of irrigated agriculture and gold-, lead-, and zinc-mining activities. This region has a prevalence of sulfide minerals and a natural occurrence of high levels of arsenopyrite. In this work, surface water, groundwater, sediments and local vegetable samples were collected in October 2010 and November 2011 and were analyzed to evaluate arsenic (As) distribution, mobility, and transport in these environmental compartments. All sediment samples (738-2,750 mg kg(-1)) and 37 % of the water samples [less than the limit of detection (LOD) to 110 µg L(-1)] from the rivers and streams of Paracatu had As concentrations greater than the quality standards established by national and international environmental organizations (5.9 mg kg(-1) for sediments and 10 µg L(-1) for water). Most vegetable samples had As concentrations within the normal range for plants (lower than the LOD to 120 mg kg(-1)). A correlation among As concentrations in water, sediment, and vegetable samples was verified.

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