title: A novel approach in dispersive liquid-liquid microextraction based on the use of an auxiliary solvent for adjustment of density UV-VIS spectrophotometric and graphite furnace atomic absorption spectrometric determination of gold based on ion pair formation.
abstract: This paper presents a novel approach to dispersive liquid-liquid microextraction (DLLME), based on the use of an auxiliary solvent for the adjustment of density. The procedure utilises a solvent system consisting of a dispersive solvent, an extraction solvent and an auxiliary solvent, which allows for the use of solvents having a density lower than that of water as an extraction solvent while preserving simple phase separation by centrifugation. The suggested approach could be an alternative to procedures described in the literature in recent months and which have been devoted to solving the same problem. The efficiency of the suggested approach is demonstrated through the determination of gold based on the formation of the ion pair [Au(CN)(2)](-) anion with Astra Phloxine (R) reagent and its extraction using the DLLME procedure with subsequent UV-VIS spectrophotometric and graphite furnace atomic absorption spectrometric detection. The optimum conditions were found to be: pH 3; 0.8 mmol L(-1) K(4)[Fe(CN)(6)]; 0.12 mmol L(-1) R; dispersive solvent, methanol; extraction solvent, toluene; auxiliary solvent, tetrachloromethane. The calibration plots were linear in the ranges 0.39-4.7 mg L(-1) and 0.5-39.4 μg L(-1) for UV-VIS and GFAAS detection, respectively; thus enables the application of the developed method in two ranges differing from one from another by three orders of magnitude. The presented approach can be applied to the development of DLLME procedures for the determination of other compounds extractable by organic solvents with a density lower than that of water.
authors.affiliation: Department of Analytical Chemistry, University of P.J. Safárik, SK-04154 Kosice, Slovak Republic.
authors.forename: Lívia
authors.initials: L
authors.lastname: Kocúrová
authors.forename: Ioseph S
authors.initials: IS
authors.lastname: Balogh
authors.forename: Jana
authors.initials: J
authors.lastname: Skrlíková
authors.forename: József
authors.initials: J
authors.lastname: Posta
authors.forename: Vasil
authors.initials: V
authors.lastname: Andruch
mesh_terms: D002251:Carbon Tetrachloride / Q000737:chemistry; D005591:Chemical Fractionation / Q000379:methods*; D003485:Cyanates / Q000737:chemistry*; D006046:Gold / Q000737:chemistry*; D006108:Graphite / Q000737:chemistry*; D007477:Ions; D000432:Methanol / Q000737:chemistry; D012997:Solvents / Q000737:chemistry*; D013054:Spectrophotometry, Atomic / Q000379:methods*; D013056:Spectrophotometry, Ultraviolet / Q000379:methods*; D014050:Toluene / Q000737:chemistry
chemical_list: D003485:Cyanates; D007477:Ions; D012997:Solvents; C043041:gold cyanide; D014050:Toluene; D006046:Gold; D006108:Graphite; D002251:Carbon Tetrachloride; D000432:Methanol