Separation and determination of antimony(III) and antimony(V) species by high-performance liquid chromatography with hydride generation atomic absorption spectrometric and inductively coupled plasma mass spectrometric detection

Abstract

Methods are described for the effective separation and determination of inorganic antimony species by high-performance liquid chromatography (HPLC)–hydride generation (HG) atomic absorption spectrometry (AAS), HPLC–inductively coupled plasma (ICP) mass spectrometry (MS) and HPLC–HG–ICP-MS. Sb^III and Sb^V were separated on a strong anion-exchange column using phthalic acid as the mobile phase. The optimum conditions for the separation of the antimony species by HPLC and the hydride generation conditions for the determination by AAS were established. Then, the HPLC system was connected to an ICP-MS system using either nebulization or hydride generation sample introduction to improve the detection limits. The detection limits were 5 and 0.6 ng per 100 µl sample for Sb^III and Sb^V, respectively (HPLC–HGAAS). For the HPLC–ICP-MS determination these limits were 0.75 and 0.09 ng and 0.04 and 0.008 ng for the HPLC–HG-ICP-MS coupling. The proposed methods for the simultaneous separation of inorganic antimony species were applied to the determination of Sb^III and Sb^V in spiked and natural water samples. Agreement within the statistical uncertainty was obtained in all instances.