Hydride generation atomic fluorescence spectrometry (HG-AFS) as a sensitive detector for Sb(III) and Sb(V) speciation in water

A procedure for the separation and determination of inorganic species of an timony based on the use of coupled high-performance liquid chromatography ( HPLC) hydride generation (HG) atomic fluorescence spectrometry (AFS) is des cribed. Sb(III) and Sb(V) were separated on a miniaturized anion-exchange c olumn (Supelcosil LC-SAX 1, 2 cm x 4.6 mm id) using a 0.06 mol l(-1) ammoni um tartrate aqueous solution at pH 6.9 as eluent. The retention times were 0.45 and 3.5 min for Sb(V) and Sb(III), respectively. The hydrides were gen erated on-line with 3% m/v NaBH4 and 2 mol l(-1) HNO3 aqueous solutions. Th e intensity of emission was linearly related to the concentration of the Sb (V) species in the range 1.0-50.0 mu g l(-1) (r(2) = 0.9976) and of Sb(III) in the range 3.0-200 mu g l(-1), with detection limits of 0.8 and 1.9 mu g l(-1), for Sb(v) and Sb(III), respectively. The precision evaluated using the relative standard deviation (RSD) was 4.4 and 2.5% (n = 10) for Sb(V) a nd Sb(III) at concentrations of 10 mu g l(-1), respectively. The method has a sensitivity suitable for monitoring drinking and surface water according to the regulations established by the EU directives for antimony (10 mu g l(-1)) and has been applied to the speciation of inorganic antimony in seve ral spiked water samples.