Characterization of organic pollutants in industrial effluents using liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry

Abstract

Contaminated industrial effluents often contain a variety of organic pollutants which are difficult to analyse by standard GC–MS methods since this technique often misses the more polar or non-volatile fraction of these organic compounds. In the present work a method for the characterization of complex mixtures of organic contaminants present in various industrial effluents is proposed. The protocol consists of setting-up a methodology based on solid phase extraction (SPE) using an Automated Sample Preparation with Extraction Columns system (ASPEC XL) and Lichrolut EN sorbent material for preconcentrating 300–500 ml of water volumes spiked with a variety of pollutants: phenolic compounds, benzophenone, isothiocyanate-cyclohexane, ethylbenzoate, 1-methyl-2-pyrrolidinone, 2-methylbenzenesulphonamide, benzidines, acridine, 1,1,3,3-tetramethyl-2-thiourea, 2,2-dimethyl-1,3-propanediol, phosphates, phthalates and non-ionic detergents characterized by LC–MS using atmospheric pressure chemical ionization in the positive and negative ion modes. The developed protocol permitted unequivocal identification of target analytes such as pentachlorophenol, tributyl phosphate, 4-nonylphenol, dibutylphthalate, dimethylphthalate, bis(2-ethylhexyl)phthalate, isothiocyanate-cyclohexane, ethylbenzoate, 2-methylbenzene-sulphonamide, tetramethyl-thiourea, 2,2-dimethyl-1,3-propanediol and 1-methyl-2-pyrrolidinone at concentration levels varying from 0.16 to 54.4 μg l-1. © 1997 John Wiley & Sons, Ltd.