Tungsten coil atomic emission spectrometry combined with dispersive liquid-liquid microextraction: A synergistic association for chromium determination in water samples

Author(s)

Vidal, Lorena ^{[1, 2]} ; Silva, Sidnei G. ^[3] ; Canals, Antonio ^{[1, 2]} ; Nobrega, Joaquim A. ^[3]

Affiliation

^[1] Univ Alicante, Dept Quim Analit Nutr & Bromatol, E-03080 Alicante - Spain

^[2] Univ Alicante, Inst Univ Mat, E-03080 Alicante - Spain

^[3] Univ Fed Sao Carlos, Dept Chem, Grp Appl Instrumental Anal, BR-13560970 Sao Carlos, SP - Brazil

• Document type: Journal article
• Source: Talanta; v. 148, p. 602-608, FEB 1 2016.
• Web of Science Citations: 16

Abstract

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 mu g L-1, respectively. This is a 233-fold improvement when compared with chromium determination by WCAES without using pre-concentration. The repeatability of the proposed method was evaluated at two different spiking levels (10 and 50 mu g 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 mu g L-1 were the recovery (trueness) and standard deviation values, respectively. Tap, bottled mineral and natural mineral water samples were analyzed at 60 mu g 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. (C) 2015 Elsevier B.V. All rights reserved. (AU)

• FAPESP's process: 11/13288-7 - Development of vaporization and atomization systems using a infrared radiation and tungsten coil
• Grantee: Sidnei Gonçalves da Silva
• Support Opportunities: Scholarships in Brazil - Post-Doctoral