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Comparison of three sequential extraction procedures for fractionation of arsenic from highly polluted mining sediments

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Abstract

Three sequential extraction procedures were evaluated for the study of fractionation of arsenic in environmental solid samples. The procedures considered were as follows: i) the standardized and widely recognised BCR procedure, conceived for the study of the partitioning of heavy metals; ii) the procedure developed by Manful, who adapted a phosphorus scheme for arsenic fractionation; and iii) a novel sequential extraction scheme especially devised for arsenic. The efficiency and suitability of these methods and the corresponding extraction steps for partitioning arsenic obtained from the most important solid forms were tested by application of the methods to real sediment samples heavily polluted by mining activity. Results showed the BCR scheme was inappropriate for arsenic fractionation. The procedure could, nevertheless, be a first approach for the assessment of arsenic partitioning, because its first extraction step can be regarded as adequate for the estimation of the most easily mobilizable arsenic. Although the Manful scheme results in a more differentiated arsenic pattern, some drawbacks arise from the lack of selectivity of some of the reagents used, for example overlapping of specific target phases, overestimation of adsorbed arsenate because of inadequate coprecipitation processes, and the inability to discriminate among amorphous and crystalline oxyhydroxides which are mainly responsible for arsenic retention. The novel procedure achieves the most suitable arsenic fractionation, because the main phases retaining arsenic are selectively targeted according to mobilization potential. In addition, the simplicity of its extraction steps would enable automation in a continuous flow scheme.

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Acknowledgements

The authors are very grateful to Jorge Loredo’s group from ETS de Ingenieros de Minas of the Universidad de Oviedo for providing the samples and minerals used in this study. The authors are also indebted to the staff of the División de Química of CIEMAT for their continuous assistance in the laboratory work. In addition, the authors would like to thanks the GEOCIMA project (CGL-2006-08192) and the FPI grant awarded to Raquel Larios by CIEMAT as financial support to perform this work.

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  1. División de Química, Departamento de Tecnología, CIEMAT, Unidad de Espectroscopía, Av. Complutense 40, 28040, Madrid, Spain

    Raquel Larios, Rodolfo Fernández-Martínez & Isabel Rucandio

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  1. Raquel Larios
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Correspondence to Isabel Rucandio.

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Larios, R., Fernández-Martínez, R. & Rucandio, I. Comparison of three sequential extraction procedures for fractionation of arsenic from highly polluted mining sediments. Anal Bioanal Chem 402, 2909–2921 (2012). https://doi.org/10.1007/s00216-012-5730-3

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