Determination of halonitromethanes in treated water

As halonitromethanes (HNMs) have begun to play an increasingly important role as disinfection by-products, the development of a highly sensitive method for their analysis has become a priority. The mass spectrometric behavior of the 9 HNMs revealed that trihalonitromethanes are more unstable than di- or monohalonitromethanes under common chromatographic conditions. The absence of a comprehensive method for HNMs has given rise to the development of the first method for the whole array of these species, involving the selection of a solventless technique. Single drop microextraction in the headspace mode (HS-SDME) was selected as it is inexpensive and easy to operate. Comparative measurements through EPA liquid-liquid extraction (LLE) method for halogenated volatile compounds, show this approach to be superior to the manual LLE procedure (the average limits of detection (LODs) for the 9 HNMs were 0.5 and 1 μg/L for the HS-SDME and EPA methods, respectively), adequate precision (8.2 and 7.0% for HS-SDME and EPA methods, respectively) and does not consume excessive solvent since the total extract (∼2 μL) was injected completely into the GC-MS instrument. The method was used to measure HNMs in treated water and the results were compared to the EPA method in parallel.