Experimental and statistical validation of SPME-GC–MS analysis of phenol and chlorophenols in raw and treated water Original Research Article

A procedure based on solid-phase microextraction (SPME) and gas chromatography coupled with mass spectrometry (GC–MS) was developed and validated in order to analyse 10 phenols in water samples. The optimised conditions were obtained using polyacrylate fibre (PA), 20 ml of sample volume, 10% NaCl, pH 4.0 and direct extraction at 35 °C and 1000 rpm, for 40 min. The linear range and quantification limits for these compounds by SPME-GC–MS were defined. An evaluation of the main uncertainty sources of this method is included, which allows expanded uncertainties in the 9.4–35% range for the majority of the compounds. The main source of uncertainty is associated with matrix effects. The validated method is suitable for monitoring the production and distribution of potable water and was used, in field trials, for the analysis of samples from main intakes of water (surface or underground) and from water supply system of a large area (Lisbon and neighbour municipalities).