Use of Experimental Design to Develop a Method for Analysis of 1,3-Dichloropropene Isomers in Water by HS-SPME and GC–ECD
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A simple and reliable method has been established for determination of cis and trans-1,3-dichloropropene (1,3-DCP) in water by headspace solid-phase microextraction (HS-SPME) then GC–ECD. An experimental design with two steps was performed to determine the best experimental conditions for extraction of the 1,3-DCP isomers. First, a 26−2 fractional factorial design was conducted to screen for significant conditions. Second, a central composite design (CCD) was performed to optimise the variables. The best experimental extraction conditions were: polydimethylsiloxane–divinylbenzene (PDMS–DVB)-coated fibre, 20-min extraction time, 12 °C extraction temperature, 300 g L−1 NaCl, and 20 mL headspace volume in 40-mL vial. Under these conditions the method detection limit (MDL) was 0.5 ng L−1 for cis-1,3-DCP and 1.0 ng L−1 for trans-1,3-DCP. The method quantification limit (MQL) was 1.2 ng L−1 for cis-1,3-DCP and 3.0 ng L−1 for trans-1,3-DCP. For both isomers the relative standard deviation (RSD) for analysis of 50 ng L−1 or 0.5 μg L−1 of the isomer mixture was less than 8%. When the proposed method was applied to surface (river) water and tapwater samples from Gipuzkoa province (Spain) the target analytes were not detected. The method was also used to investigate the presence of the isomers in leachates from agricultural soil. A mixed solution was added to samples of two different soils and 1,3-DCP isomers were quantified in leachate obtained from the samples.
KeywordsGas chromatography Headspace solid-phase microextraction Experimental design 1,3-Dichloropropene River water and tapwater Soil leachate
The authors wish to thank the University of the Basque Country (UPV/EHU) for financial support through project UPV05/65.
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