Simultaneous determination of cyanogen chloride and cyanogen bromide in treated water at sub-μg/L levels by a new solid-phase microextraction–gas chromatographic–electron-capture detection method

A headspace solid-phase microextraction (HS-SPME) procedure has been developed and applied for the determination of cyanogen halides in treated water samples at μg/L concentrations. Several SPME coatings were tested, the divinylbenzene–Carboxen–polydimethylsiloxane fiber being the most appropriate coating. GC–electron-capture detection was used for separation and quantitation. Experimental parameters such as sample volume, addition of a salt, extraction time and desorption conditions were studied. The optimized method has an acceptable linearity, good precision, with RSD values <10% for both compounds, and it is sufficiently sensitive to detect ng/L levels. HS-SPME was compared with liquid–liquid microextraction (US Environmental Protection Agency Method 551.1) for the analysis of spiked ultrapure and granular activated carbon filtered water samples. There was good agreement between the results from both methods. Finally, the optimized procedure was applied to determine both compounds at the Barcelona water treatment plant (N.E. Spain). Cyanogen chloride in treated water was <1.0 μg/L and cyanogen bromide ranged from 3.2 to 6.4 μg/L.