Publication Details

Category Text Publication
Reference Category Journals
DOI 10.1016/j.chroma.2005.11.010
Title (Primary) Miniaturized membrane-assisted solvent extraction combined with gas chromatography/electron-capture detection applied to the analysis of volatile organic compounds
Author Schellin, M.; Popp, P.
Source Titel Journal of Chromatography A
Year 2006
Department ANA
Volume 1103
Issue 2
Page From 211
Page To 218
Language englisch
Keywords Membrane-assisted solvent extraction; Volatile organic compounds; Extraction conditions; Real samples; Headspace-analysis; Semi volatiles
Abstract A new module of membrane-assisted solvent extraction (MASE) with miniaturized membrane bags was applied to the determination of seven volatile organic compounds (VOCs): chloroform, 1,1,1-trichloroethane, trichloroethylene, 1,1,2-trichloroethane, tetrachloroethene, 1,1,1,2-tetrachloroethane, 1,1,2,2-tetrachloroethane with boiling points between 61 and 147 °C in aqueous samples. Different from the known procedure the new, shortened membrane bags were filled with 100 μl of an organic solvent. The membrane bags were placed in a 20 ml headspace vial and filled with 15 ml of the aqueous sample. The vial was transferred into an autosampler where it was stirred for a definite time at elevated temperature. After the extraction, 1 μl of the organic extract was transferred into the spilt/splitless injector of a GC system equipped with an electron-capture detector. This work included optimization of the membrane device, the determination of the optimized extraction conditions such as stirring rate, extraction time and the impact of salt addition. The validation of the method involved repeatability, recovery and detection limit studies, followed of its application towards real water samples. The repeatability, expressed as the relative standard deviation of the peak areas of six extractions was below 10%. The detection limits (LODs) were between 5 ng/l (tetrachloroethene) and 50 ng/l (chloroform). Calibration was performed in a range from 5 ng/l to 150 μg/l, since the concentration in the aqueous samples was expected quite various in this concentration range. Five river water samples of Bitterfeld, Saxony-Anhalt, Germany were analyzed with miniaturized-MASE and the results were compared with those obtained with Headspace-Analysis. The method can be fully automated and moreover, it allows the simultaneous determination of volatile and semi volatile compounds.
Persistent UFZ Identifier https://www.ufz.de/index.php?en=20939&ufzPublicationIdentifier=2988
Schellin, M., Popp, P. (2006):
Miniaturized membrane-assisted solvent extraction combined with gas chromatography/electron-capture detection applied to the analysis of volatile organic compounds
J. Chromatogr. A 1103 (2), 211 - 218 10.1016/j.chroma.2005.11.010