Headspace single-drop microextraction with in situ stibine generation for the determination of antimony (III) and total antimony by electrothermal-atomic absorption spectrometry
- 191 Downloads
A headspace-single drop microextraction method combined with electrothermal atomic absorption spectrometry (ETAAS) is developed for the extraction and preconcentration of antimony(III) and total antimony into a Pd(II)-containing aqueous drop after hydride generation. Experimental variables such as hydrochloric acid and sodium tetrahydroborate concentrations, sample volume, Pd(II) concentration in the acceptor phase and microextraction time were optimized. A 26-2 IV factorial fractional design was initially used for screening the effect of the variables, followed by an univariate approach. The method showed a great freedom from interferences caused by hydride-forming elements and transition metals. The detection limit of Sb(III) was 25 pg mL−1. A preconcentration factor of 176 is achieved in 3 min. The repeatability, expressed as relative standard deviation, was 4.7%. The method was validated against two certified reference materials (NWRI-TM 27.2 and NIST 2711) and applied to the determination of Sb(III) and total Sb in waters.
KeywordsSb(III) and total Sb Hydride generation Headspace-single drop microextraction Environmental samples Electrothermal-AAS
The financial support from the Spanish Education and Science Ministry (project CTQ2006-04111/BQU) and the Galician government (Xunta de Galicia) (project PGIDIT05PXIB31401PR) is gratefully acknowledged.
- 3.Council of the European Communities (1998) Council Directive Relating to the Quality of Water Intended for Human Consumption (98/83/CE)Google Scholar
- 10.Bosch Ojeda C, Sánchez Rojas F, Cano Pavón JM, Terrer Martín L (2005) Use of 1,5-bis(di-2-pyridyl)methylene thiocarbohydrazide immobilized on silica gel for automated preconcentration and selective determination of antimony(III) by flow injection electrothermal atomic absorption spectrometry. Anal Bioanal Chem 382:513CrossRefGoogle Scholar
- 11.Craig PJ, Sergeeva T, Jenkins RO (2001) Determination of inorganic Sb(V) and methylantimony species by HPLC with hydride generation-atomic fluorescence spectrometric detection. Mikrochim Acta 137:221Google Scholar
- 22.Figueroa R, García M, Lavilla I, Bendicho C (2005) Photoassisted vapor generation in the presence of organic acids for ultrasensitive determination of Se by electrothermal-atomic absorption spectrometry following headspace single-drop microextraction. Spectrochim Acta Part B 60:1556CrossRefGoogle Scholar
- 25.Shioji H, Tsunoi S, Harino H, Tanaka M (2004) Liquid-phase microextraction of tributyltin and triphenyltin coupled with gas chromatography-tandem mass spectrometry Comparison between 4-fluorophenyl and ethyl derivatizations. J Chromatogr A 1048:81Google Scholar
- 28.Box GEP, Hunter JS, Hunter WG (1989) Estadística para investigadores, 1st edn. Reverté, BarcelonaGoogle Scholar
- 35.Matusiewicz H, Kopras M (2003) Simultaneous determination of hydride forming elements (As, Bi, Ge, Sb, Se) and Hg in biological and environmental reference materials by electrothermal vaporization-microwave induced plasma-optical emission spectrometry with their in situ trapping in a graphite furnace. J Anal At Spectrom 18:1415CrossRefGoogle Scholar