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Wireless electrochemical preparation of gradient nanoclusters consisting of copper(II), stearic acid and montmorillonite on a copper wire for headspace in-tube microextraction of chlorobenzenes

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Abstract

This work introduces a new gradient fiber coating for microextraction of chlorobenzenes. Nanoclusters of organoclay-Cu(II) on a copper wire were fabricated by wireless electrofunctionalization. The resultant gradient coatings are more robust, and thermally and mechanically stable. Wireless electrofunctionalization was carried out in a bipolar cell under a constant deposition potential and using an ethanolic electrolyte solution containing stearic acid and montmorillonite. Stearic acid acts as an inexpensive and green coating while montmorillonite acts as a modifier to impart thermal stability. The gradient morphology of the nanoclusters was investigated by scanning electron microscopy, thermogravimetric analysis and energy dispersive X-ray spectroscopy. The coated wire was placed in a hollow needle and used for headspace in-tube microextraction (HS–ITME) of chlorobenzenes (CBs). Effects of various parameters affecting synthesis and extraction were optimized. Following extraction, the needles were directly inserted into the GC injector, and the CBs (chlorobenzene, 1,4-dichlorobenzene, 1,2-dichlorobenzene, 1,2,4-trichlorobenzene, 1,2,3,4-tetrachlorobenzene) were quantified by GC–MS. The limits of detection under optimized conditions range from 0.5 to 10 ng.L−1. The intra– and inter–day relative standard deviations (RSDs) (for n = 10, 5 respectively) using a single fiber are 6–10 and 10–15%, respectively. The fiber–to–fiber RSDs (for n = 3) is between 17 and 24%. The method was successfully applied to the extraction of CBs from real water samples, and relative recoveries are between 91 and 110%.

A gradient coating of organoclay–Cu nanoclusters was fabricated on a copper wire by wireless electrofunctionalization. The oxidation of copper takes place at the anodic pole (red) while dissolved oxygen in ethanol solution is reduced at the cathodic pole (blue).

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Authors and Affiliations

  1. Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran

    Marzieh Enteshari Najafabadi & Habib Bagheri

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  1. Marzieh Enteshari Najafabadi
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  2. Habib Bagheri
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Correspondence to Habib Bagheri.

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Enteshari Najafabadi, M., Bagheri, H. Wireless electrochemical preparation of gradient nanoclusters consisting of copper(II), stearic acid and montmorillonite on a copper wire for headspace in-tube microextraction of chlorobenzenes. Microchim Acta 185, 80 (2018). https://doi.org/10.1007/s00604-017-2549-9

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