Microchimica Acta

, Volume 164, Issue 1–2, pp 77–83 | Cite as

Headspace single-drop microextraction with in situ stibine generation for the determination of antimony (III) and total antimony by electrothermal-atomic absorption spectrometry

  • Francisco Pena-Pereira
  • Isela Lavilla
  • Carlos BendichoEmail author
Original Paper


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.


Sb(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.

Supplementary material

604_2008_36_MOESM1_ESM.pdf (39 kb)
ESM Supplementary section (PDF 40 KB)


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Copyright information

© Springer-Verlag 2008

Authors and Affiliations

  • Francisco Pena-Pereira
    • 1
  • Isela Lavilla
    • 1
  • Carlos Bendicho
    • 1
    Email author
  1. 1.Departamento de Química Analítica y Alimentaria, Area de Química Analítica, Facultad de QuímicaUniversidade de VigoVigoSpain

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