Multicomponent analysis of volatile organic compounds in water by automated purge and trap coupled to gas chromatography–mass spectrometry

Abstract

The performance of an automated purge and trap concentrator coupled to gas chromatography–mass spectrometric detection was evaluated by analyzing 40 volatile organic compounds of different chemical families. Compounds chosen defined as toxic for the environment and for human health were selected according to Directive 76/464/CEE. The present work includes: (i) the optimization of the purge and trap conditions, (ii) the establishment of quality parameters and in last instance (iii) the analysis of surface waters. The analytical method consisted of a modification of the EPA Method 524.2 in which water was pumped, via an automated AquaTek 70 Liquid Autosampler to a 25-ml purging device, where samples were purged and trapped in a Tenax or Tenax-Silica and Charcoal column. Afterwards, helium was used to desorb the trapped analytes that flow directly into the GC column. Mass spectrometric analysis was carried out in selected ion monitoring and scan modes to ensure quantification and confirmation of the results. Parameters optimized were the sample volume analyzed, bubbling flow-rate and time and temperature of desorption. Optimal conditions lead to mean recoveries of 80%, limits of detection between 0.002 and 0.1 μg/l, linearity from 0.01 to 2.5 μg/l and maximum standard deviation of 10%, using a Tenax trap. This protocol permitted a high precision and sample throughput and was used to determine volatile organic compounds in surface river, effluents and coastal waters of Portugal, on a routine basis.