期刊
MICROCHIMICA ACTA
卷 164, 期 1-2, 页码 77-83出版社
SPRINGER WIEN
DOI: 10.1007/s00604-008-0036-z
关键词
Sb(III) and total Sb; Hydride generation; Headspace-single drop microextraction; Environmental samples; Electrothermal-AAS
资金
- Spanish Education and Science Ministry [CTQ2006-04111/BQU]
- Galician government (Xunta de Galicia) [PGIDIT05PXIB31401PR]
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 2(6-2) (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.
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