Antimony(V) volatilization with bromide and determination by inductively coupled plasma atomic emission spectrometry

Abstract Antimony(V) is volatilized by reaction with potassium bromide in concentrated sulfuric acid media. After volatilization, the gases can be transported to an inductively coupled plasma spectrometer for atomic emission of antimony and its analytical determination. The influent factors, concentrated sulfuric acid volume, concentration and volume of the potassium bromide aqueous solution and carrier gas flow were investigated and optimized using different alternatives. A detection limit of 48 ng ml −1 of Sb was achieved under the optimized conditions with a precision of 7.6% and the calibration graph was linear from 0.10 to 10.0 μg ml −1 for a sample injection of 130 μl. The study of interferences from common cations and anions revealed a good tolerance for most ions, although there was a significant improvement in Sb(V) volatility when As(III) was present. Furthermore, the As(III) sensitization was only produced with Sb(V) species, while the volatility of the Sb(III) bromide species was unaltered. The method was applied to the determination of Sb in real river waters. The results were checked using alternative atomic spectroscopy methods.