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Ordoñes J, Fernández L, Romero H, et al. Electrochemical generation of antimony volatile species, stibine, using gold and silver mercury amalgamated cathodes and determination of Sb by flame atomic absorption spectrometry. Talanta. 2015;141:259-66doi: 10.1016/j.talanta.2015.04.025.
Ordoñes, J., Fernández, L., Romero, H., Carrera, P., & Alvarado, J. (2015). Electrochemical generation of antimony volatile species, stibine, using gold and silver mercury amalgamated cathodes and determination of Sb by flame atomic absorption spectrometry. Talanta, 141259-66. https://doi.org/10.1016/j.talanta.2015.04.025
Ordoñes, Jessenia, et al. "Electrochemical generation of antimony volatile species, stibine, using gold and silver mercury amalgamated cathodes and determination of Sb by flame atomic absorption spectrometry." Talanta vol. 141 (2015): 259-66. doi: https://doi.org/10.1016/j.talanta.2015.04.025
Ordoñes J, Fernández L, Romero H, Carrera P, Alvarado J. Electrochemical generation of antimony volatile species, stibine, using gold and silver mercury amalgamated cathodes and determination of Sb by flame atomic absorption spectrometry. Talanta. 2015 Aug 15;141:259-66. doi: 10.1016/j.talanta.2015.04.025. Epub 2015 Apr 16. PMID: 25966412.
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Talanta. 2015 Aug 15;141:259-66. doi: 10.1016/j.talanta.2015.04.025. Epub 2015 Apr 16.

Electrochemical generation of antimony volatile species, stibine, using gold and silver mercury amalgamated cathodes and determination of Sb by flame atomic absorption spectrometry.

Talanta

Jessenia Ordoñes, Lenys Fernández, Hugo Romero, Patricio Carrera, José Alvarado

Affiliations

  1. Facultad de Ciencias Químicas y de la Salud, Universidad Técnica de Machala, Apartado, 070151 Machala, Ecuador.
  2. Departamento de Química, Universidad Simón Bolívar, Apartado 89000, Caracas 1080-A, Venezuela. Electronic address: [email protected].
  3. Hidroecuador, Apartado, EC1701 Quito, Ecuador.
  4. Departamento de Química, Universidad Simón Bolívar, Apartado 89000, Caracas 1080-A, Venezuela.

PMID: 25966412 DOI: 10.1016/j.talanta.2015.04.025

Abstract

The electrochemical generation of antimony volatile species (stibine) using Au and Ag mercury amalgamated cathodes is described. Compared with some other cathode materials commonly used for electrochemical hydride generation, performance of the amalgamated cathodes is substantially better in the following aspects: higher interference tolerance, higher erosion resistance and longer useful working time. Using the amalgamated cathodes, it could be shown that interferences from major constituents at high concentrations, especially from transition metals, affecting stibine generation are not as significant as they are using other cathode types in regards to sensitivity and useful working time. Results obtained using the Ag/Hg amalgamated cathode showed a slightly higher sensitivity than the corresponding results obtained using the Au/Hg cathode. The Au/Hg cathode, which to our knowledge has not previously been used to generate stibine, showed considerably longer useful working time than the Ag/Hg one. The optimum catholytes for electrolytic generation of stibine (SbH3) from Sb(III) and Sb(V) using the Au/Hg electrode were aqueous solutions containing 0.5mol L(-1) H2SO4 and 0.5mol L(-1)HCl, respectively. Under optimized conditions, using the Au/Hg cathode and comparing to aqueous standards calibration curves, detection limits (3σ) of 0.027µg L(-1) for Sb(III) and 0.056µg L(-1) for Sb(V), were obtained. To check accuracy a marine sediment reference material (PACS-2, NRC) was analyzed using a method purportedly developed for this task. Good agreement, 95% confidence, was found between the certified and the experimental values for Sb. The proposed method was also applied to the determination of Sb in aqueous solutions of marine sediments samples from Comuna de Bajo Alto Provincia de El Oro-Ecuador. Recoveries of five replicate determinations of these samples were in the range of 98-103% thus showing acceptable accuracy in the analysis of real samples.

Copyright © 2015 Elsevier B.V. All rights reserved.

Keywords: Atomic absorption spectrometry; Electrochemical antimony hydride generation; Marine sediment samples; Stibine

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