Selectivity assessment of an arsenic sequential extraction procedure for evaluating mobility in mine wastes

• Extraction efficiency and selectivity of phosphate and oxalate were tested.
• Pure As-bearing mineral phases and mine wastes were used.
• The reagents were found to be specific and selective for most major forms of As.
• An optimized sequential extraction scheme for mine wastes has been developed.
• It has been tested over a model mineral mixtures and natural mine waste materials.

An optimized sequential extraction (SE) scheme for mine waste materials has been developed and tested for As partitioning over a range of pure As-bearing mineral phases, their model mixtures, and natural mine waste materials. This optimized SE procedure employs five extraction steps: (1) nitrogen-purged deionized water, 10 h; (2) 0.01 M NH4H2PO4, 16 h; (3) 0.2 M NH4-oxalate in the dark, pH3, 2 h; (4) 0.2 M NH4-oxalate, pH3/80 °C, 4 h; (5) KClO3/HCl/HNO3 digestion. Selectivity and specificity tests on natural mine wastes and major pure As-bearing mineral phases showed that these As fractions appear to be primarily associated with: (1) readily soluble; (2) adsorbed; (3) amorphous and poorly-crystalline arsenates, oxides and hydroxosulfates of Fe; (4) well-crystalline arsenates, oxides, and hydroxosulfates of Fe; as well as (5) sulfides and arsenides. The specificity and selectivity of extractants, and the reproducibility of the optimized SE procedure were further verified by artificial model mineral mixtures and different natural mine waste materials. Partitioning data for extraction steps 3, 4, and 5 showed good agreement with those calculated in the model mineral mixtures (<15% difference), as well as that expected in different natural mine waste materials. The sum of the As recovered in the different extractant pools was not significantly different (89–112%) than the results for acid digestion. This suggests that the optimized SE scheme can reliably be employed for As partitioning in mine waste materials.

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