© 2016 Informa UK Limited, trading as Taylor & Francis Group. A simple and efficient method has been developed for the extraction and determination of 16 common volatile halogenated disinfection by-products (DBPs) (four trihalomethanes, six haloacetonitriles, and six halonitromethanes) in blending desalinated waters, using headspace solid-phase microextraction and gas chromatography with flame ionization detector (HS-SPME/GC-FID). After the optimization using factorial designs of the HS-SPME parameters (optimum: carboxen/polydimethylsiloxane such as fiber, extraction time of 60 min at 30°C, pH 7, addition of 40% (w/v) of sodium chloride, and desorption time of 2 min at 250°C), quantification limits ranged from 3.03 to 40.8 µg L −1 , and relative standard deviation (inter-day) were lower than 9.7% for all the target DBPs. Adequate relative recoveries (with the exception of chloronitromethane) were obtained even when spiking waters at low levels (25 µg L −1 ), with values between 83.1% and 119% for ultrapure water, and between 87.4% and 115% for blending desalinated waters, supporting in this way the applicability of the method. The influence of various dechlorinating agents on the stability of 16 DBPs in water was evaluated, with ammonium chloride being the most suitable inhibitor of residual chlorine and carrying out the analytical determination of DBPs within 48 h after sampling. Different blending desalinated water samples collected in the South of Tenerife Island (Spain) were successfully analyzed.
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