Online coupling of Lab-In-Syringe automated headspace extraction to gas chromatography has been studied. The developed methodology was successfully applied to surface water analysis using benzene, toluene, ethylbenzene, and xylenes as model analytes. The extraction system consisted of an automatic syringe pump with a 5 mL syringe into which all solutions and air for headspace formation were aspirated. The syringe piston featured a longitudinal channel, which allowed connecting the syringe void directly to a gas chromatograph with flame ionization detector via a transfer capillary. Gas injection was achieved via opening a computer-controlled pinch valve and compressing the headspace, upon which separation was initialized. Extractions were performed at room temperature; yet sensitivity comparable to previous work was obtained by high headspace to sample ratio VHS/VSample of 1.6:1 and injection of about 77% of the headspace. Assistance by in-syringe magnetic stirring yielded an about threefold increase in extraction efficiency. Interferences were compensated by using chlorobenzene as an internal standard. Syringe cleaning and extraction lasting over 10 min was carried out in parallel to the chromatographic run enabling a time of analysis of <19 min. Excellent peak area repeatabilities with RSD of <4% when omitting and <2% RSD when using internal standard corrections on 100 μg L-1 level were achieved. An average recovery of 97.7% and limit of detection of 1-2 μg L-1 were obtained in analyses of surface water.
- MeSH
- automatizace MeSH
- benzen analýza izolace a purifikace MeSH
- benzenové deriváty analýza izolace a purifikace MeSH
- limita detekce MeSH
- mikroextrakce na pevné fázi MeSH
- plamínková ionizace metody MeSH
- teplota MeSH
- toluen analýza izolace a purifikace MeSH
- voda chemie MeSH
- xyleny analýza izolace a purifikace MeSH
- Publikační typ
- časopisecké články MeSH
- MeSH
- chromatografie plynová * metody využití MeSH
- hippuráty izolace a purifikace metabolismus moč MeSH
- kyselina benzoová izolace a purifikace metabolismus moč MeSH
- lidé MeSH
- pára * analýza škodlivé účinky MeSH
- statistika jako téma MeSH
- xyleny * izolace a purifikace metabolismus škodlivé účinky MeSH
- Check Tag
- lidé MeSH
