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Cloud point extraction and spectrophotometric determination of mercury species at trace levels in environmental samples.

Talanta (2012-01-24)
Halil İbrahim Ulusoy, Ramazan Gürkan, Songül Ulusoy
ABSTRACT

A new micelle-mediated separation and preconcentration method was developed for ultra-trace quantities of mercury ions prior to spectrophotometric determination. The method is based on cloud point extraction (CPE) of Hg(II) ions with polyethylene glycol tert-octylphenyl ether (Triton X-114) in the presence of chelating agents such as 1-(2-pyridylazo)-2-naphthol (PAN) and 4-(2-thiazolylazo) resorcinol (TAR). Hg(II) ions react with both PAN and TAR in a surfactant solution yielding a hydrophobic complex at pH 9.0 and 8.0, respectively. The phase separation was accomplished by centrifugation for 5 min at 3500 rpm. The calibration graphs obtained from Hg(II)-PAN and Hg(II)-TAR complexes were linear in the concentration ranges of 10-1000 μg L(-1) and 50-2500 μg L(-1) with detection limits of 1.65 and 14.5 μg L(-1), respectively. The relative standard deviations (RSDs) were 1.85% and 2.35% in determinations of 25 and 250 μg L(-1) Hg(II), respectively. The interference effect of several ions were studied and seen commonly present ions in water samples had no significantly effect on determination of Hg(II). The developed methods were successfully applied to determine mercury concentrations in environmental water samples. The accuracy and validity of the proposed methods were tested by means of five replicate analyses of the certified standard materials such as QC Metal LL3 (VWR, drinking water) and IAEA W-4 (NIST, simulated fresh water).

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Triton X-405 solution, 70% in H2O
Sigma-Aldrich
1-(2-Pyridylazo)-2-naphthol, indicator grade
Sigma-Aldrich
IGEPAL® CA-630, viscous liquid
Sigma-Aldrich
IGEPAL® CA-630, for molecular biology
Sigma-Aldrich
Triton X-114, laboratory grade
Sigma-Aldrich
Triton X-165 solution
Supelco
IGEPAL® CA-630
Sigma-Aldrich
IGEPAL® CA-720, average Mn ~735
Sigma-Aldrich
Triton X-114