Analysis of semi-volatile organics in aqueous process streams using solid-phase microextraction and gas chromatography

Analysis of aqueous streams contaminated with complex organic mixtures commonly used in industrial processes can be problematic. In this study, we describe the development of the solid-phase microextraction (SPME) headspace extraction technique in combination with gas chromatography (GC) to measure the leakage of n-decanol and Exxsol(R) D-110 (commercial solvent containing primarily napthenes and paraffins) into aqueous streams. These streams were derived from a continuous liquid membrane separator for the removal and recovery of Cr(VI) from industrial effluents. In one stream that was dilute in Cr(VI) at pH 2-3, a method giving good results for n-decanol analysis involved the addition of n-octanol as an internal standard to GC calibration standards and test samples prior to SPME extraction with the appropriate adjustment of pH. The addition of 20 w/w% NaCl as an additional solute to all standards and test samples with pH adjustment was found to be successful for quantitative determination of Exxsol(R) D-110. In a second stream that was strongly alkaline and more concentrated in Cr(VI), GC calibration using standards containing NaOH and 300-500 ppm Cr(VI) gave satisfactory results for quantitative determination of both species. (C) 2001 Elsevier Science Ltd. All rights reserved.