Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1238, Issue -, Pages 22-29Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2012.03.027
Keywords
Aniline-silica nanocomposite; Solid phase microextraction; Polycyclic aromatic hydrocarbons; Gas chromatography-mass spectrometry; Water analysis
Funding
- Research Council and Graduates School of Sharif University of Technology (SUT)
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A new unbreakable solid phase microextraction (SPME) fiber coating based on aniline-silica nanocomposite was electrodeposited on a stainless steel wire. The electropolymerization process was carried out at a constant deposition potential, applied to the corresponding aqueous electrolyte containing aniline and silica nanoparticles. The scanning electron microscopy (SEM) images showed the non-smooth and the porous surface structure of the prepared nanocomposite. The applicability of the new fiber coating was examined by headspace-solid phase microextraction (HS-SPME) of some environmentally important polycyclic aromatic hydrocarbons (PAHs), as model compounds, from aqueous samples. Subsequently, the extracted analytes were transferred into a gas chromatography (GC) by thermal desorption. Parameters affecting the synthesizing and extraction processes including the voltage of power supply, the weight ratio of components, the time of electrodeposition, extraction time and temperature, the ionic strength, and desorption temperature and time were optimized. Eventually, the developed method was validated by gas chromatography-mass spectrometry (GC-MS). At the optimum conditions, the relative standard deviation (%RSD) values for a double distilled water spiked with the selected PAHs at 40 ng L-1 were 6-13% (n = 3) while the limit of detection (LOD) results were between 1 and 3 ng L-1. The calibration graphs were linear in the concentration range from 20 to 4000 ng L-1 (R-2>0.995). Finally the developed method was applied to the analysis of Kalan dam, rain and tap water samples and the relative recovery values were found to be in the range of 76-109%, under optimized conditions. In addition, the synthesis of the nanocomposite coating was carried out conveniently while it is rather inexpensive, easy, simple, rapid and highly durable and can be used frequently. (C) 2012 Elsevier B.V. All rights reserved.
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