Ultrasensitive direct determination of BTEX in polluted soils using a simple and novel pressure-controlled solid-phase microextraction setup

A pressure-controlled headspace solid-phase microextraction (PC-HS-SPME) setup was developed, by reconsidering the strengths and weaknesses points of the similar reported systems. The new setup was coupled with gas chromatography-flame ionization detection (GC-FID) for direct analysis of benzene, toluene, ethylbenzene and xylene (BTEX) in contaminated soils, without any sample preparation step. The important experimental factors, affecting the performance of the method, including volumes of extraction and vacuum vials, type of SPME fiber, extraction time and temperature, moisture content of the sample, and sonication time were studied and optimized. Under the optimal conditions, good linearity of the calibration curves (R-2 > 0.997) was obtained in the concentration range of 0.1-20,000 ng g(-1). The limits of detections were found to be 0.001-0.08 ng g(-1). The relative standard deviations, for six repetitive analyses of 100 ng g(-1) BTEX, were obtained to be 5.7-12.3%. The PC-HS-SPME-GC-FID procedure was successfully applied for the extraction and determination of BTEX in the polluted soil samples.