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Automated Single-Phase Liquid-Liquid Extraction for Determination of Cr(VI) Using Graphite Furnace Atomic Absorption Spectrophotometry without Wet Digestion of Samples

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Abstract

This paper proposes a method to perform rapid and sensitive graphite furnace atomic absorption spectrometry (GFAAS) determination of Cr(VI) in vinegar samples without wet digestion. Taking into account low levels of Cr(VI) and the presence of several concomitants in the sample matrix, the proposed method uses single-phase liquid-liquid extraction (SPLLE). The method is automated, employing a flow-batch analyzer (FBA) which uses a mixing chamber designed to emulate a separation funnel promoting the formation/break of the single-phase solution, reaction and extraction. The Cr(VI) extraction procedure was performed by proportioned mixing of the vinegar sample (aqueous phase), amyl alcohol (organic phase), and ethanol (consolute) to form a single-phase solution. The chelating reagent sodium diethyldithiocarbamate (DDTC) dissolved in the consolute reacts rapidly with Cr(VI), in the single phase to produce a stable Cr-DDTC complex. The single-phase break step is performed by adding an excess of Britton-Robinson buffer, and then the organic phase enriched with Cr(VI) was analyzed by GFAAS. Factors such as extraction steps, single-phase composition, pH, chelating agent concentration, and flow-batch parameters were optimized. The FBA-SPLLE-GFAAS was evaluated in vinegar samples showing satisfactory analytical features in terms of limit of quantification (0.86 μg L −1), precision (RSD <12 %), characteristic mass (m0 = 0.32 pg), high sampling rate (26 h −1), and accuracy (recovery rate = 82–108 %). The proposed method requires one-step extraction and is eco-friendly since it consumes low amounts of non-toxic chemicals and generates little waste (about 700 μL per determination).

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Acknowledgments

The authors gratefully acknowledge scholarships from the Brazilian funding agencies CAPES and CNPq.

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Authors and Affiliations

  1. Centro de Ciências Exatas e da Natureza, Departamento de Química, Universidade Federal da Paraíba, P.O. Box 5093, João Pessoa, PB, Zip Code 58051-970, Brazil

    Francisco Antonio S. Cunha, Anderson S. G. Pereira, Julys Pablo A. Fernandes, Wellington S. Lyra, Mario Cesar U. Araújo & Luciano F. Almeida

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  1. Francisco Antonio S. Cunha
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  2. Anderson S. G. Pereira
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  3. Julys Pablo A. Fernandes
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  4. Wellington S. Lyra
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  5. Mario Cesar U. Araújo
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  6. Luciano F. Almeida
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Correspondence to Luciano F. Almeida.

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This study was publicly funded by CNPq and CAPES.

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The authors Francisco Antonio da Silva Cunha, Anderson da Silva Gualberto Pereira, Julys Pablo Atayde Fernandes, Wellington da Silva Lyra, Mario Cesar Ugulino de Araújo, and Luciano Farias de Almeida declare no conflict of interest.

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Cunha, F.A.S., Pereira, A.S.G., Fernandes, J.P.A. et al. Automated Single-Phase Liquid-Liquid Extraction for Determination of Cr(VI) Using Graphite Furnace Atomic Absorption Spectrophotometry without Wet Digestion of Samples. Food Anal. Methods 10, 921–930 (2017). https://doi.org/10.1007/s12161-016-0651-y

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