Sorbent-packed needle microextraction trap for benzene, toluene, ethylbenzene, and xylenes determination in aqueous samples

J Sep Sci. 2010 Sep;33(17-18):2833-40. doi: 10.1002/jssc.201000213.

Abstract

A needle trap (NT) device filled with Carbopack X as a sorbent material is evaluated for the static headspace analysis of benzene, toluene, ethylbenzene, and xylene (BTEX) compounds in aqueous samples. Injection parameters used with the NT device (e.g. volume of carrier gas and time to open the split valve) are evaluated to determine the mechanism involved during the desorption and transferring of the target compounds into the GC column. Furthermore, different parameters affecting the adsorption capacity of the sorbent are studied (e.g. sampling time and temperature, headspace/sample volume ratio, salting-out, and stirring). The evaluation of the method with aqueous samples shows that repeatability and recoveries with the NT device are equivalent to those obtained using solid-phase microextraction with a carboxen/PDMS (CAR/PDMS) coating. LODs obtained with flame ionization detection are in the range of 10-25 μg/L, and in the range of hundredths of μg/L with MS detection. The method developed is satisfactorily applied to the analysis of aqueous samples obtained from wastewater treatment plants.