Determination of traces of Sb(III) using ASV in Sb-rich water samples affected by mining

• Antimony speciation affects the toxicity of this element.
• A simple method for Sb(III) analyses in Sb-rich waters was developed.
• Sb(III) was determined by ASV in water stabilized with tartaric and nitric acids.
• Pre-concentration and/or separation of Sb(III) prior to analysis are not required.

Chemical speciation [Sb(V) and Sb(III)] affects the mobility, bioavailability and toxicity of antimony. In oxygenated environments Sb(V) dominates whereas thermodynamically unstable Sb(III) may occur. In this study, a simple method for the determination of Sb(III) in non acidic, oxygenated water contaminated with antimony is proposed. The determination of Sb(III) was performed by anodic stripping voltammetry (ASV, 1–20 μg L−1 working range), the total antimony, Sb(tot), was determined either by inductively coupled plasma mass spectrometry (ICP-MS, 1–100 μg L−1 working range) or inductively coupled plasma optical emission spectrometry (ICP-OES, 100–10,000 μg L−1 working range) depending on concentration. Water samples were filtered on site through 0.45 μm pore size filters. The aliquot for determination of Sb(tot) was acidified with 1% (v/v) HNO3. Different preservatives, namely HCl, L(+) ascorbic acid or L(+) tartaric acid plus HNO3, were used to assess the stability of Sb(III) in synthetic solutions.The method was tested on groundwater and surface water draining the abandoned mine of Su Suergiu (Sardinia, Italy), an area heavily contaminated with Sb. The waters interacting with Sb-rich mining residues were non acidic, oxygenated, and showed extreme concentrations of Sb(tot) (up to 13,000 μg L−1), with Sb(III) <10% of total antimony. The stabilization with L(+) tartaric acid plus HNO3 appears useful for the determination of Sb(III) in oxygenated, Sb-rich waters. Due to the instability of Sb(III), analyses should be carried out within 7 days upon the water collection. The main advantage of the proposed method is that it does not require time-consuming preparation steps prior to analysis of Sb(III).

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