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. 2014 Nov;5(6):685-93.
doi: 10.1016/j.jare.2013.11.003. Epub 2013 Nov 20.

Pseudo-stir Bar Hollow Fiber Solid/Liquid Phase Microextraction Combined With Anodic Stripping Voltammetry for Determination of Lead and Cadmium in Water Samples

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Free PMC article

Pseudo-stir Bar Hollow Fiber Solid/Liquid Phase Microextraction Combined With Anodic Stripping Voltammetry for Determination of Lead and Cadmium in Water Samples

Zarrin Es'haghi et al. J Adv Res. .
Free PMC article

Abstract

A new procedure is presented for the determination of low concentrations of lead and cadmium in water samples. Ligand assisted pseudo-stir bar hollow fiber solid/liquid phase microextraction using sol-gel sorbent reinforced with carbon nanotubes was combined with differential pulse anodic stripping voltammetry for simultaneous determination of cadmium and lead in tap water, and Darongar river water samples. In the present work, differential pulse anodic stripping voltammetry (DPASV) using a hanging mercury drop electrode (HMDE) was used in order to determine the ultra trace level of lead and cadmium ions in real samples. This method is based on accumulation of lead and cadmium ions on the electrode using different ligands; Quinolin-8-ol, 5,7-diiodo quinoline-8-ol, 4,5-diphenyl-1H-imidazole-2(3H)-one and 2-{[2-(2-Hydroxy-ethylamino)-ethylamino]-methyl}-phenol as the complexing agent. The optimized conditions were obtained. The relationship between the peak current versus concentration was linear over the range of 0.05-500 ng mL(-1) for Cd (II) and Pb (II). The limits of detection for lead and cadmium were 0.015 ng mL(-1) and 0.012 ng mL(-1), respectively. Under the optimized conditions, the pre-concentration factors are 2440 and 3710 for Cd (II) and Pb (II) in 5 mL of water sample, respectively.

Keywords: Anodic stripping; Cadmium; Hollow fiber solid liquid phase microextraction; Lead; Voltammetry.

Figures

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Fig. 1
Fig. 1
Scanning electron microscopy polypropylene hollow fiber structure.
Fig. 2
Fig. 2
(a) FT-IR spectra of untreated MWCNTs, (b) FT-IR spectra of acid-functionalized MWCNTs.
Fig. 3
Fig. 3
Simple scheme of pseudo-stir bar HF-SLPME device: (a) filled hollow fiber membrane by sol–gel and CNT mixture and (b) magnetic stoppers (iron pins; 2.5 mm × 0.6 mm).
Fig. 4
Fig. 4
Effect of feed solution pH on the extraction. Conditions: analytes concentration, 50 ng mL−1; donor phase volume, 5.0 mL; acceptor phase volume 3.0 μL; stirring speed, 150 rpm; extraction time, 60 min; room temperature.
Fig. 5
Fig. 5
Effect of stripping agent: Conditions: analytes concentration, 50 ng mL−1; molar concentration ratio of ligand to analyte, 10; pH, 5.0; donor phase volume, 5.0 mL; acceptor phase volume 3.0 μL; extraction time, 60 min; stirring speed, 200 rpm; room temperature.
Fig. 6
Fig. 6
Effect of functionalized MWCNTs concentration. Conditions: analytes concentration, 50 ng mL−1; molar concentration ratio of ligand (L2) to analyte, 10; pH, 5.0; donor phase volume, 5.0 mL; acceptor phase volume 3.0 μL; extraction time, 60 min; stirring speed, 200 rpm; room temperature.
Fig. 7
Fig. 7
Effect of donor phase volume on the extraction. Conditions: analytes concentration, 50 ng mL−1; molar concentration ratio of ligand (L2) to analyte, 10; pH, 5.0; acceptor phase volume 3.0 μL; stirring speed, 150 rpm; extraction time, 60 min; room temperature.
Fig. 8
Fig. 8
Differential pulse voltammograms of Cd (II) and Pb (II) obtained from (a) the blank voltammogram, (b) River water sample and (c) the same sample after microextraction under optimal conditions.

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