Work was undertaken to develop an analytical technique for the determination of several classes of disinfection byproducts (DBPs), which was amenable to a wide range of compounds with high sensitivity. A solid-phase microextraction (SPME)-gas chromatography/electron capture detector (GC/ECD) technique was developed and used in conjunction with several other analytical methods (i.e., solid-phase extraction [SPE]-GC/mass spectrometry [MS], purge-and-trap [P&T]-GC/MS, and liquid-liquid extraction [LLE]-GC/ECD). These methods were used to investigate the occurrence of DBPs at 12 water treatment plants in the U.S. The SPME-GC/ECD technique is simple and eliminates the need for solvents and the complicated steps necessary for analyzing for semivolatile DBP. This technique has been automated and has reduced sample preparation time. Development of this method included investigating various types of SPME fibers, adsorption and desorption times, injector/desorption temperatures, headspace versus direct extraction techniques, and the use of an internal standard. The method developed here samples the headspace of a 5-mL sample, which has the addition of sodium chloride (25 percent by weight), with a Carboxen/divinylbenzene/polydimethylsiloxane (CAR/DVB/PDMS) fiber. A 30-min adsorption time and a 5-min desorption in a 200C injector gave the best results for analyzing for the target DBPs. Most, if not all, of the analytes can be detected below 1.0 ug/L. Includes 9 references, tables, figures.
