How Much Can a 15m X 0.25mm X 0.10µm GC Column Be Trimmed for Maintenance Before the BDE 49 and 71 Resolution Requirements Are No Longer Met for EPA Method 1614

Poster Presentation

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

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


ABSTRACT

Polybrominated diphenyl ethers (PBDEs) have been found to be persistent and bioaccumulative in the environment. The technical mixtures containing penta and octa congeners were voluntarily withdrawn in the United States in 2005 and the last remaining PBDE mixture, decaBDE, should be completely phased out by the end of 2013. While these mixtures have been phased out of production and use, the concentrations in the environment have not been declining and are currently still widely monitored.

The analysis of PBDEs is challenging due to structural isomers that need to be chromatographically separated and thermally label compounds of interest that may breakdown during gas chromatography. PBDEs included in EPA Method 1614 are well resolved on a 15m x 0.25mm x 0.10µm Rtx-1614 GC column, a 5% diphenyl, 95% dimethyl polysiloxane type phase that was specifically designed to meet method resolution requirements. Using a short, thin film column also allows the elution of decabromodiphenyl ether (BDE-209) without on-column thermal degradation.

Monitoring efforts of the levels of PBDEs include a wide array of biota and environmental matrices. Non-volatile material may still persist even in cleaned-up final extracts, requiring GC column and inlet maintenance to be performed. Using a 15m x 0.25mm x 0.10µm column, how many loops of the GC column can one clip for maintenance before the Method 1614 resolution requirements of BDE 49 and BDE 71 can no longer be met? The resolution between BDE 49 and 71 must be less than 40% valley height to meet method criteria.