A micro-solid phase extraction procedure for the separation and preconcentration of antimony based in the use of magnetic particles covered with silver nanoparticles functionalized with the sodium salt of 2-mercaptoethane-sulphonate (MESNa) is discussed. After separation by means of a magnetic field, the solid phase is directly introduced into an electrothermal atomizer for antimony determination. Alternatively, the solid can be slurried and then injected into the atomizer. In all cases, palladium nitrate is used as a chemical modifier. The preconcentration factors are close to 205 and 325, with detection limits of 0.02 and 0.03µgL-1 antimony, for the slurry and solid sampling procedures, respectively. Speciation of Sb(III) and Sb(V) is achieved by means of two extractions carried out at different acidity. The results for total antimony are verified using certified reference materials. Water samples are analyzed for antimony speciation.
Keywords: Antimony; Electrothermal atomic absorption spectrometry; Magnetic-core particles; Speciation; Waters.
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