Analysis of benzene, toluene, ethylbenzene, xylenes and n-aldehydes in melted snow water via solid-phase dynamic extraction combined with gas chromatography/mass spectrometry

Autor(en): Sieg, Karsten
Fries, Elke
Puettmann, Wilhelm
Stichwörter: aldehydes; AROMATIC-HYDROCARBONS; Biochemical Research Methods; Biochemistry & Molecular Biology; BTEX; CHEMICALS; Chemistry; Chemistry, Analytical; GC/MS; HAIR SAMPLES; ICE; MATRICES; MICROEXTRACTION; NEEDLE; RAIN; snow; solid-phase dynamic extraction (SPDE); SORPTION; VOLATILE ORGANIC-COMPOUNDS
Erscheinungsdatum: 2008
Herausgeber: ELSEVIER SCIENCE BV
Journal: JOURNAL OF CHROMATOGRAPHY A
Volumen: 1178
Ausgabe: 1-2
Startseite: 178
Seitenende: 186
Zusammenfassung: 
The present study describes a method based on headspace-solid-phase dynamic extraction (HS-SPDE) followed by GC/MS for the qualitative and quantitative analysis of benzene, toluene, ethylbenzene, o-, m- and p-xylene (BTEX), and n-aldehydes (C-6-C-10) in water. To enhance the extraction capability of the HS-SPDE a new cooling device was tested that controls the temperature of the SPDE needle during extraction. Extraction and desorption parameters such as the number of extraction cycles, extraction temperature, desorption volume and desorption flow rate have been optimized. Detection limits for BTEX ranged from 19 ng/L (benzene) to 30 ng/L (m/p-xylene), while those for n-aldehydes ranged from 21 ng/L (n-heptanal) to 63 ng/L (n-hexanal). At a concentration level of 2 mu g/L, the relative standard deviations (RSDs) for BTEX ranged from 3.9% (benzene) to 15.3% (ethylbenzene), while RSDs for n-aldehydes were between 6.1% (n-octanal) and 16.5% (n-hexanal) (n=7). Best results were obtained when the analyzed water samples were heated to 50 degrees C. At a water temperature of 70 degrees C GC responses decreased for all analyzed compounds. At a defined water temperature, a significant improvement of the GC response was achieved by cooling of the SPDE fiber during water extraction in comparison to an extraction keeping the fiber at room temperature. Evaluating the extraction cycles, for BTEX, the sensitivity was almost similar using 20, 40 and 60 extraction cycles. In contrast, the highest GC responses for n-aldehydes were achieved by the use of 60 extraction cycles. Optimizing. the desorption parameters, best results were achieved using the smallest technical available desorption volume of 500 mu L and the highest technical desorption flow rate of 50 mu L/s. The method was applied to the analysis of melted snow samples taken from the Jungfraujoch, Switzerland (3580 m asl), revealing the presence of BTEX and aldehydes in snow. (c) 2007 Elsevier B.V. All rights reserved.
ISSN: 00219673
DOI: 10.1016/j.chroma.2007.11.025

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