Tungsten coil atomic emission spectrometry combined with dispersive liquid-liquid microextraction: a synergistic association for chromium determination in water samples
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A novel and environment friendly analytical method is reported for total chromium determination and chromium speciation in water samples, whereby tungsten coil atomic emission spectrometry (WCAES) is combined with in situ ionic liquid formation dispersive liquid-liquid microextraction (in situ IL-DLLME). A two stage multivariate optimization approach has been developed employing a Plackett-Burman design for screening and selection of the significant factor involved in the in situ IL-DLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were complexant concentration: 0.5% (or 0.1%); complexant type: DDTC; IL anion: PF6(-); [Hmim][Cl] IL amount: 60 mg; ionic strength: 0% NaCl; pH: 5 (or 2); centrifugation time: 10 min; and centrifugation speed: 1000 rpm. Under the optimized experimental conditions the method was evaluated and proper linearity was obtained with a correlation coefficient of 0.991 (5 calibration standards). Limits of detection and quantification for both chromium species were 3 and 10 µg L(-1), respectively. This is a 233-fold improvement when compared with chromium determination by WCAES without using preconcentration. The repeatability of the proposed method was evaluated at two different spiking levels (10 and 50 µg L(-1)) obtaining coefficients of variation of 11.4% and 3.6% (n=3), respectively. A certified reference material (SRM-1643e NIST) was analyzed in order to determine the accuracy of the method for total chromium determination and 112.3% and 2.5 µg L(-1) were the recovery (trueness) and standard deviation values, respectively. Tap, bottled mineral and natural mineral water samples were analyzed at 60 µg L(-1) spiking level of total Cr content at two Cr(VI)/Cr(III) ratios, and relative recovery values ranged between 88% and 112% showing that the matrix has a negligible effect. To our knowledge, this is the first time that combines in situ IL-DLLME and WCAES.
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The strategy of diluting the IL phase before injection has been extended to other instrumental techniques, including tungsten coil atomic emission spectrometry for Cr detection and HPLC-UV determination of Pb, Cd, Co and Ni after extraction in DES trihexyl(tetradecyl)phosphonium chloride and thiosalicylic acid.
“The strategy of diluting the IL phase prior injection has been extended to other instrumental techniques, as tungsten coil atomic emission spectrometry for Cr detection [17], or HPLC-UV determination of Pb, Cd, Co and Ni after extraction in DES trihexyl(tetradecyl)phosphonium chloride and thiosalicylic acid [38].”
From Advances in ionic liquids and deep eutectic solvents-based liquid phase microextraction of metals for sample preparation in Environmental Analytical Chemistry (2021) · cites this paper as [17]
Experimental — accuracy not yet measuredIn both cases (tungsten coil AES for Cr and HPLC-UV for Pb, Cd, Co, Ni), acetonitrile was used as a diluent.
“In both cases acetonitrile was used as a diluent.”
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- Authors
- Vidal, L., Silva, S. G., Canals, A., & Nóbrega, J. A.
- Affiliations
- University of Alicante (ES)
- Universidade Federal de São Carlos (BR)
- Corresponding author
- Vidal, Lorena
- Venue
- Talanta
- Publisher
- Elsevier BV
- Published
- 2016-02
- Volume
- 148
- Pages
- 602-608
- ISSN
- 0039-9140 (ISSN-L)
- OpenAlex
- W1993097247
- Semantic Scholar
- 6eb18256906623d0fc4ffd56a8b8ba7d3c275634
- Cited by
- 29
- References
- 33
- Citations by year
- 2025: 3 · 2024: 1 · 2023: 2 · 2022: 1 · 2021: 2 · 2020: 3 · 2019: 2 · 2018: 9 · 2017: 1 · 2016: 5
- FWCI
- 3.91
- Type
- journal article
- Language
- en
- Open access
- bronze
- doi.org
- Licence
- Locations
- Talanta (publishedVersion)
- PubMed (publishedVersion)
- LA Referencia (Red Federada de Repositorios Institucionales de Publicaciones Científicas) (submittedVersion)
- RUA, Repositorio Institucional de la Universidad de Alicante (Universidad de Alicante) (submittedVersion)
- Funders
- Fundação de Amparo à Pesquisa do Estado de São Paulo
- Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (2011/13288-7, 243/11, HBP-2010-0030)
- Ministerio de Educación, Cultura y Deporte (PHB2010-0018-PC)
- Generalitat Valenciana (ACOMP/2013/072)
- Ministerio de Ciencia e Innovación (CTQ2011-23968)
- Topics
- Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
- Physical Sciences › Environmental Science › Water Science and Technology › Environmental and Analytical Chemistry Studies
- Physical Sciences › Engineering › Mechanics of Materials › Laser-induced spectroscopy and plasma
- Keywords
- dispersive liquid-liquid microextraction, ionic liquids, chromium speciation, total chromium determination, water samples, preconcentration, mineral water, tap water, bottled water
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