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Piston-cylinder based micro liquid–liquid extraction with GC–qMS for trace analysis of targeted chlorinated organic compounds in water


Luong, J and Gras, R and Gras, K and Shellie, RA, Piston-cylinder based micro liquid-liquid extraction with GC-qMS for trace analysis of targeted chlorinated organic compounds in water, Canadian Journal of Chemistry, 93, (11) pp. 1283-1289. ISSN 0008-4042 (2015) [Refereed Article]

DOI: doi:10.1139/cjc-2015-0307


A 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.

Item Details

Item Type:Refereed Article
Keywords:micro liquid-liquid extraction, piston-cylinder based extraction, DB-624UI column, planar microfluidics, triple-axis detector
Research Division:Chemical Sciences
Research Group:Analytical chemistry
Research Field:Separation science
Objective Division:Expanding Knowledge
Objective Group:Expanding knowledge
Objective Field:Expanding knowledge in the chemical sciences
UTAS Author:Luong, J (Mr Jim Luong)
UTAS Author:Gras, R (Ms Ronda Gras)
UTAS Author:Shellie, RA (Associate Professor Robert Shellie)
ID Code:106674
Year Published:2015
Web of Science® Times Cited:4
Deposited By:Austn Centre for Research in Separation Science
Deposited On:2016-02-17
Last Modified:2017-10-30

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