Determination of naphthalenesulfonic acid isomers by large-volume on-line derivatization and gas chromatography–mass spectrometry

This work presents a modified method to analyze polar and water-soluble naphthalene monosulfonic acid (NS) isomers in industrial effluents and river water samples. The method involves extraction of samples by a styrene–divinylbenzene copolymer solid-phase extraction cartridge, and on-line derivatization in the GC injection port using a large-volume (10 μl) sample injection with tetrabutylammonium salts. The analytes were then identified and quantitatively determined by GC–MS. The large-volume injection-port derivatization technique provides sensitivity, fast and reproducible results for NS isomers, to quantitation at 0.05 μg/l in 200 ml of water sample. Enhanced extracted mass chromatograms of molecular ion and [M−56]+ ion of butylated NS isomers by electron impact ionization MS allows us to determine residues at trace levels in environmental samples. Recoveries of the NS isomers in spiked water samples ranged from 70 to 82% with RSDs around 10%. Naphthalene-2-sulfonic acid was found as a major pollutant and propagated in surface water and industrial effluents.