Electrochemical In Situ Fabrication of Titanium Dioxide Nanotubes on a Titanium Wire as a Fiber Coating for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons

A novel titanium dioxide nanotube (TiO<sub>2</sub>NTS) coated fiber for solid-phase microextraction (SPME) was prepared by in situ anodization of titanium wire in electrolyte containing ethylene glycol and ammonium fluoride (NH<sub>4</sub>F). The effects of different electrol...

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Autores principales: Mingguang Ma, Yunxia Wei, Jie Chen, Qiong Shang
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Publicado: MDPI AG 2021
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spelling oai:doaj.org-article:04feb5def203457d993aeb7345fd19b32021-11-25T17:19:13ZElectrochemical In Situ Fabrication of Titanium Dioxide Nanotubes on a Titanium Wire as a Fiber Coating for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons10.3390/cryst111113842073-4352https://doaj.org/article/04feb5def203457d993aeb7345fd19b32021-11-01T00:00:00Zhttps://www.mdpi.com/2073-4352/11/11/1384https://doaj.org/toc/2073-4352A novel titanium dioxide nanotube (TiO<sub>2</sub>NTS) coated fiber for solid-phase microextraction (SPME) was prepared by in situ anodization of titanium wire in electrolyte containing ethylene glycol and ammonium fluoride (NH<sub>4</sub>F). The effects of different electrolyte solutions (NH<sub>4</sub>F and ethylene glycol) and oxidation voltages on the formation and size of TiO<sub>2</sub>NTs was studied. It was obtained from the experiment that TiO<sub>2</sub>NTs arrays were arranged with a wall thickness of 25 nm and the diameter of 100 nm pores in ethylene glycol and water (<i>v</i>/<i>v</i>, 1:1) containing NH<sub>4</sub>F of 0.5% (<i>w</i>/<i>v</i>) with a voltage of 20 V at 25 °C for 30 min. The TiO<sub>2</sub>NTs were used as solid-phase microextraction fiber coatings coupled with high-performance liquid chromatography (HPLC) in sensitive determination of polycyclic aromatic hydrocarbons (PAHs) in spiked real samples water. Under the optimized SPME conditions, the calibration curve has good linearity in the range of 0.20–500 μg·L<sup>−1</sup>, and the correlation coefficient (R<sup>2</sup>) is between 0.9980 and 0.9991. Relative standard deviations (RSDs) of 3.5–4.7% (<i>n</i> = 5) for single fiber repeatability and of 5.2% to 7.9% for fiber-to-fiber reproducibility (<i>n</i> = 3) was obtained. The limits of detection (LOD) (S/N = 3) and limits of quantification (LOQ) (S/N = 10) of PAHs were 0.03–0.05 µg·L<sup>−1</sup> and 0.12–0.18 µg·L<sup>−1</sup>. The developed method was applied to the preconcentration and determination of trace PAHs in spiked real samples of water with good recoveries from 78.6% to 119% and RSDs from 4.3 to 8.9%, respectively.Mingguang MaYunxia WeiJie ChenQiong ShangMDPI AGarticlesolid-phase microextractiontitanium dioxide nanotubehigh-performance liquid chromatographypolycyclic aromatic hydrocarbonsCrystallographyQD901-999ENCrystals, Vol 11, Iss 1384, p 1384 (2021)
institution DOAJ
collection DOAJ
language EN
topic solid-phase microextraction
titanium dioxide nanotube
high-performance liquid chromatography
polycyclic aromatic hydrocarbons
Crystallography
QD901-999
spellingShingle solid-phase microextraction
titanium dioxide nanotube
high-performance liquid chromatography
polycyclic aromatic hydrocarbons
Crystallography
QD901-999
Mingguang Ma
Yunxia Wei
Jie Chen
Qiong Shang
Electrochemical In Situ Fabrication of Titanium Dioxide Nanotubes on a Titanium Wire as a Fiber Coating for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons
description A novel titanium dioxide nanotube (TiO<sub>2</sub>NTS) coated fiber for solid-phase microextraction (SPME) was prepared by in situ anodization of titanium wire in electrolyte containing ethylene glycol and ammonium fluoride (NH<sub>4</sub>F). The effects of different electrolyte solutions (NH<sub>4</sub>F and ethylene glycol) and oxidation voltages on the formation and size of TiO<sub>2</sub>NTs was studied. It was obtained from the experiment that TiO<sub>2</sub>NTs arrays were arranged with a wall thickness of 25 nm and the diameter of 100 nm pores in ethylene glycol and water (<i>v</i>/<i>v</i>, 1:1) containing NH<sub>4</sub>F of 0.5% (<i>w</i>/<i>v</i>) with a voltage of 20 V at 25 °C for 30 min. The TiO<sub>2</sub>NTs were used as solid-phase microextraction fiber coatings coupled with high-performance liquid chromatography (HPLC) in sensitive determination of polycyclic aromatic hydrocarbons (PAHs) in spiked real samples water. Under the optimized SPME conditions, the calibration curve has good linearity in the range of 0.20–500 μg·L<sup>−1</sup>, and the correlation coefficient (R<sup>2</sup>) is between 0.9980 and 0.9991. Relative standard deviations (RSDs) of 3.5–4.7% (<i>n</i> = 5) for single fiber repeatability and of 5.2% to 7.9% for fiber-to-fiber reproducibility (<i>n</i> = 3) was obtained. The limits of detection (LOD) (S/N = 3) and limits of quantification (LOQ) (S/N = 10) of PAHs were 0.03–0.05 µg·L<sup>−1</sup> and 0.12–0.18 µg·L<sup>−1</sup>. The developed method was applied to the preconcentration and determination of trace PAHs in spiked real samples of water with good recoveries from 78.6% to 119% and RSDs from 4.3 to 8.9%, respectively.
format article
author Mingguang Ma
Yunxia Wei
Jie Chen
Qiong Shang
author_facet Mingguang Ma
Yunxia Wei
Jie Chen
Qiong Shang
author_sort Mingguang Ma
title Electrochemical In Situ Fabrication of Titanium Dioxide Nanotubes on a Titanium Wire as a Fiber Coating for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons
title_short Electrochemical In Situ Fabrication of Titanium Dioxide Nanotubes on a Titanium Wire as a Fiber Coating for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons
title_full Electrochemical In Situ Fabrication of Titanium Dioxide Nanotubes on a Titanium Wire as a Fiber Coating for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons
title_fullStr Electrochemical In Situ Fabrication of Titanium Dioxide Nanotubes on a Titanium Wire as a Fiber Coating for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons
title_full_unstemmed Electrochemical In Situ Fabrication of Titanium Dioxide Nanotubes on a Titanium Wire as a Fiber Coating for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons
title_sort electrochemical in situ fabrication of titanium dioxide nanotubes on a titanium wire as a fiber coating for solid-phase microextraction of polycyclic aromatic hydrocarbons
publisher MDPI AG
publishDate 2021
url https://doaj.org/article/04feb5def203457d993aeb7345fd19b3
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