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In-syringe magnetic-stirring-assisted liquid–liquid microextraction for the spectrophotometric determination of Cr(VI) in waters

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Abstract

A fully automated method for the determination of chromate is described. It is based on the selective reaction of Cr(VI) with diphenylcarbazide in acidic media to form a colored complex of Cr(III) with the oxidation product diphenylcarbazone. The reaction was performed within the syringe of an automatic burette containing a magnetic stirrer for homogenization of the sample and the required reagents. In-syringe stirring was made possible using a specially designed driving device placed around the syringe barrel to achieve a rotating magnetic field in the syringe, forcing the stirrer to spin. In a second step, the reaction mixture in the syringe was neutralized to allow in-syringe magnetic-stirring-assisted dispersive liquid–liquid microextraction of the complex into 125 μL of n-hexanol. After phase separation by droplet flotation over 30 s, the organic phase was propelled into a coupled spectrophotometric detection cell. The entire multistep procedure including in-system standard preparation was done within 270 s. The method was used for the analysis of natural waters, achieving average analyte recovery of 103 %, a limit of detection of 0.26 μg L-1, and a repeatability of less than 4 % relative standard deviation.

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Acknowledgments

The authors acknowledge the financial support from the Spanish Ministry of Science and Innovation through the project CTQ2010-15541 and from the Conselleria d’Economia, Hacienda, e Innovació of the Government of the Balearic Islands through the allowance to competitive groups (43/2011) through Feder Funds. C.H. is very grateful to the Conselleria d´Educació, Cultura I Universitat, and the European Social Fund for funding her PhD grant. B.H. was supported by a postdoctoral fellowship of the project CZ.1.07/2.3.00/30.0022 supported by the Education for Competitiveness Operational Program and co-financed by the European Social Fund and the state budget of the Czech Republic.

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Authors and Affiliations

  1. Laboratory of environmental Analytical Chemistry, University of the Balearic Islands, Carreterra de Valldemossa km 7.5, 07122, Palma de Mallorca, Spain

    Camelia Henríquez, Burkhard Horstkotte & Víctor Cerdà

  2. Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, 50005, Hradec Králové, Czech Republic

    Burkhard Horstkotte & Petr Solich

Authors
  1. Camelia Henríquez
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  2. Burkhard Horstkotte
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  3. Petr Solich
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  4. Víctor Cerdà
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Corresponding author

Correspondence to Víctor Cerdà.

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Henríquez, C., Horstkotte, B., Solich, P. et al. In-syringe magnetic-stirring-assisted liquid–liquid microextraction for the spectrophotometric determination of Cr(VI) in waters. Anal Bioanal Chem 405, 6761–6769 (2013). https://doi.org/10.1007/s00216-013-7111-y

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  • DOI: https://doi.org/10.1007/s00216-013-7111-y

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