Analysis of benzene, toluene, ethylbenzene, xylenes and n-aldehydes in melted snow water via solid-phase dynamic extraction combined with gas chromatography/mass spectrometry.
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 microg/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 microL and the highest technical desorption flow rate of 50 microL/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.
Institute of Atmospheric and Environmental Sciences, Department of Analytical Environmental Chemistry, Johann Wolfgang Goethe-University Frankfurt/Main, Altenhöferallee 1, 60438 Frankfurt am Main, Germany. k.sieg@iau.uni-frankfurt.de
Karsten
K
Sieg
Elke
E
Fries
Wilhelm
W
Püttmann
D001554:Benzene / Q000032:analysis* / Q000302:isolation & purification; D001555:Benzene Derivatives / Q000032:analysis* / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D012914:Snow / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D014050:Toluene / Q000032:analysis* / Q000302:isolation & purification; D014867:Water / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis; D014992:Xylenes / Q000032:analysis* / Q000302:isolation & purification
D001555:Benzene Derivatives; D014874:Water Pollutants, Chemical; D014992:Xylenes; D014867:Water; D014050:Toluene; D001554:Benzene; C004912:ethylbenzene