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http://dx.doi.org/10.5806/AST.2011.24.5.352

Solvent-free determination of BTEX in water using repetitive membrane extraction followed by GC-MS  

Kim, He-Kap (Department of Environmental Science, College of Natural Sciences, Kangwon National University)
Kim, Se-Young (Department of Environmental Science, College of Natural Sciences, Kangwon National University)
Lee, Soo-Hyung (Department of Environmental Science, College of Natural Sciences, Kangwon National University)
Publication Information
Analytical Science and Technology / v.24, no.5, 2011 , pp. 352-359 More about this Journal
Abstract
An analytical method for solvent-free determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using repetitive membrane extractions coupled to cryofocusing and GC-MS was derived. BTEX compounds that permeated through a nonporous silicone membrane from the aqueous phase and evaporated into the acceptor phase were purged into a cryofocusing trap ($-100^{\circ}C$) with helium gas. The BTEX compounds, thus enriched in the trap, were thermally desorbed into a capillary column GC and detected using an MS. The flow rate of the donor phase (30 mL water) was set at 10 mL/min, and membrane extractions, accomplished by returning the water drained from the extraction module to the sample container, were repeated three times at $20{\pm}2^{\circ}C$. Although recoveries (%) were variable, from the highest for benzene (approximately 80%) to the lowest for ethylbenzene and xylenes (3.5-10%), the method showed satisfactory precision (RSD 2.2-10%) with good-linearity calibration curves ($r^2$ 0.9976-0.9997 in 1-100 ${\mu}g$/L range) for all of the compounds. The method detection limits (MDLs) ranged from 0.16 to 1.8 ${\mu}g$/L. The results showed the method's advantages such as short analysis time and overall simplicity without solvent compared to the conventional techniques.
Keywords
BTEX; cryofocusing; GC-MS; repetitive membrane extractions; nonporous silicone membrane;
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