Qualitative and quantitative analysis of water and sediment samples for semivolatile brominated fire retardants was conducted. Four brominated fire retardants were identified and quantitated. Sample analysis included solvent extraction followed by gas-liquid chromatography/mass spectrometry (GLC-MS) and thin-layer chromatography/scanning spectrodensitometry (TLC-SD).

The fire retardants decabromobiphenyl ether (DBBE) and tris(2,3-dibromopropyl) phosphate (tris) presented special analytical problems related to their very low volatility and thermal instability, respectively. More than one analytical method was developed for some of the fire retardants under investigation. For most brominated compounds gas-liquid chromatography/electron capture detector (GLC-ECD) was the most sensitive method. Tris required a very short [0.2 cm inside diameter by 42 cm long, 2 percent OV-101 on Chromosorb W(HP) ] column to avoid extensive thermal degradation, and decabromobiphenyl ether could not be readily analyzed by GLC-ECD due to the very high temperature at which it must be chromatographed and GLC-MS or TLC was used for its quantitation with GLC-MS confirmation of identity. The very low volatility of DBBE required the use of a short [0.2 cm inside diameter by 42 cm long, 2 percent OV-101 on Chromosorb W(HP)] column. The GLC-MS methods for DBBE are also applicable to 2,2-bis(dibromo-4-hydroxy- phenyl)propane (Tetrabromobisphenol A, TBBA) and 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE, Firemaster 680).

Samples from the vicinity of manufacturing sites were examined. The analytical procedures employed and representative samples of qualitative and quantitative data from these samples will be presented.