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Piston-cylinder based micro liquid-liquid extraction with GC-qMS for trace analysis of targeted chlorinated organic compounds in water
journal contribution
posted on 2015-01-01, 00:00 authored by J Luong, R Gras, K Gras, Robert ShellieRobert ShellieA fast and reliable approach for the measurement of sub parts-per-billion levels of targeted chlorinated compounds like tetrachloroethane, hexachloroethane, hexachlorobutadiene, pentachlorobenzene, and hexachlorobenzene in various water matrices such as waste water is described. The method employed a novel piston-cylinder-based micro liquid-liquid extraction technique using hexane as an extraction solvent. The device, known commercially as the MIXXOR, substantially accelerates extraction time by a factor of more than 100 times and reduces solvent consumption by a factor of 25 times when compared with the solvent extraction technique using wrist-action mechanical agitation. A recently introduced 6% cyanopropylphenyl-94% dimethylpolysiloxane capillary column offering a high degree of inertness was used for the separation of the analytes. A quadrupole mass spectrometer equipped with a triple-axis detector was also employed to enhance the instrument detection limit. With this technique, a complete separation for the analytes in water can be conducted in less than 10 min using a three-port SilFlow planar microfluidic device for back-flushing. Repeatability of retention times for all compounds were found to be less than 0.04% (n = 10). The compounds cited can be analyzed from 1 ng/mL to 10 μg/mL, with a detection limit and correlation coefficient of at least 0.5 ng/mL and 0.999, respectively. A relative precision of less than 1.2% relative standard deviation (RSD) (n = 20) at the 50 ng/mL level, with analyte recovery of greater than 99% (n = 3) from 10 ng/mL to 10 μg/mL, was obtained.
History
Journal
Canadian journal of chemistryVolume
93Issue
11Pagination
1283 - 1289Publisher
Canadian Science PublishingLocation
Ottawa, Ont.Publisher DOI
ISSN
0008-4042Language
engPublication classification
C1 Refereed article in a scholarly journalCopyright notice
2015, Published by NRC Research Press.Usage metrics
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No categories selectedKeywords
micro liquid-liquid extractionpiston-cylinder based extractionScience & TechnologyPhysical SciencesChemistry, MultidisciplinaryChemistryDB-624UI columnplanar microfluidicstriple-axis detectorSOLID-PHASE MICROEXTRACTIONGROUNDWATER QUALITYGAS-CHROMATOGRAPHYHEXACHLOROBENZENELANDFILLPHOTOIONIZATIONCONTAMINANTSIMPACTSSYSTEMSSITE
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