Optimization of headspace experimental factors to determine chlorophenols in water by means of headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry and parallel factor analysis |
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Authors: | Rocío Morales M Cruz Ortiz Luis A Sarabia |
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Institution: | 1. Department of Chemistry, Faculty of Science, University of Burgos, Pza. Misael Bañuelos s/n, 09001 Burgos, Spain;2. Department of Mathematics and Computation, Faculty of Science, University of Burgos, Pza. Misael Bañuelos s/n, 09001 Burgos, Spain |
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Abstract: | In this work an analytical procedure based on headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry (HS-SPME–GC/MS) is proposed to determine chlorophenols with prior derivatization step to improve analyte volatility and therefore the decision limit (CCα). After optimization, the analytical procedure was applied to analyze river water samples. The following analytes are studied: 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TrCP), 2,3,4,6-tetrachlorophenol (2,4,6-TeCP) and pentachlorophenol (PCP). A D-optimal design is used to study the parameters affecting the HS-SPME process and the derivatization step. Four experimental factors at two levels and one factor at three levels were considered: (i) equilibrium/extraction temperature, (ii) extraction time, (iii) sample volume, (iv) agitation time and (v) equilibrium time. In addition two interactions between four of them were considered. The D-optimal design enables the reduction of the number of experiments from 48 to 18 while maintaining enough precision in the estimation of the effects. As every analysis took 1 h, the design is blocked in 2 days. |
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Keywords: | Chlorophenols D-optimal design Parallel factor analysis River water samples Headspace solid-phase microextraction Gas chromatography&ndash mass spectrometry |
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