Capillary gas chromatographic analysis of highly brominated fire retardant compounds

We report the development of a capillary gas chromatographic method, superior to existing packed column methods, for the analysis of highly brominated additive fire-retardants, including decabromodiphenyl ether (1) and decabromodiphenoxyethane (II). Neither compound has been analyzed previously by capillary GC, and there are no published methods for (II). For (I), the new method is 5–10 times faster than an analogous packed column method, and it has 100 times lower detection limits and twice the precision of a gas chromatographic/mass spectrometric method. For (II), the capillary method is 30–50% faster than an unpublished liquid chromatographic method. The greater efficiency of the capillary method makes possible the complete resolution (R ≥ 1.25) of structurally very similar compounds (e.g. compound (II) and its Br₉Cl₁ and Br₈Cl₂ analogues). With the new method, commercial preparations of (I) and (II) can be rapidly analyzed, and samples from combustion and pyrolysis experiments can be evaluated for compositional changes.