Evaluation of a dedicated gas chromatography–mass spectrometry method for the analysis of phenols in water

The increasing need to routinely analyse phenolic hydrocarbons in aqueous samples was addressed by the development and implementation of a state-of-the-art, though relatively straightforward, analytical procedure. The proposed method is based on acetic anhydride derivatisation of the native phenols, liquid–liquid extraction of the corresponding phenyl acetate esters and subsequent analysis by GC–MS. The key feature and main strength of the method is located at the injection step which applies ‘at-once’ large volume injection with a programmable temperature vaporizer (PTV)-type injector. In the proposed method, the sensitivity gain inherent to the higher injection volume was used entirely to proportionally miniaturize, considerably accelerate and effectively simplify the otherwise tedious and time-consuming derivatisation/extraction step. Method performance, as expressed in terms of repeatability, reproducibility, linearity and accuracy, was found to be excellent. R.S.D. values, determined in the framework of an extensive reproducibility study, ranged between 1.47 and 9.02%. Detection limits were in the low ng/L range for all compounds with linear ranges extending up to two orders of magnitude. Method accuracy was determined by analyzing a certified reference material (PH-1JM), spiked water samples and participating in a series of round robin tests and did not reveal any significant bias for the different compounds under investigation.