Coconut Charcoal Solid Phase Extraction - Large Volume Splitless Injection - GC-MS for Analysis of Dioxane, Tetrahydrofuran, Nitrosamines, Ethylene Dibromide, Trichloropropane, Dibromochloropropane, Chlorinated Solvents, and Disinfection Byproducts in Drinking Water: The Possibility for a Single Comprehensive Method

Oral Presentation

Prepared by C. Rattray, M. Misselwitz, J. Kowalski, C. English, J. Cochran
Restek Corporation, 110 Benner Circle, Bellefonte, PA, 16823

Contact Information: chris.rattray@restek.com; 814-353-1300


ABSTRACT

Currently there are multiple EPA methods for the analysis of 1,4-dioxane, tetrahydrofuran, nitrosamines, ethylene dibromide (1,2-dibromoethane), 1,2,3-trichloropropane, 1,2-dibromo-3-chloropropane, chlorinated solvents, and disinfection byproducts in drinking water (e.g. 504.1, 521, 522, 524.3, 551.1), all requiring different sample preparation methods including solid phase extraction (SPE), liquid-liquid extraction, and purge-and-trap. We looked at combining these methods into one by extracting drinking waters with coconut charcoal SPE, eluting with an appropriate organic solvent, followed by concurrent solvent recondensation – large volume splitless injection (CSR-LVSI) – gas chromatography – mass spectrometry (GC-MS).

The benefits of a combination method include fewer samples for collecting and shipping and extracting, and less instrumental time. Because the final SPE extract cannot be concentrated via evaporation due to volatile compound loss, we employed CSR-LVSI, which uses a standard splitless injector to deliver as much as 50µL extract to a retention gap connected to a typical GC column for separation and then MS analysis. This large volume injection allows the low detection limits needed for drinking water analysis, especially for selected ion monitoring, but also even for full scan MS, which provides a better qualitative confirmation of the compounds of interest.

Data will be shown for spiked and unspiked drinking water samples analyzed by the proposed method and for more conventional 500 series methods.