Development of a Solid-Phase Microextraction GC-NPD Procedure for the Determination of Free Volatile Amines in Wastewater and Sewage-Polluted Waters

• Published in: Analytical chemistry (Washington) Vol. 71; no. 16; pp. 3531 - 3537
• Main Authors: Ábalos, Manuela, Bayona, Josep M, Ventura, Francesc
• Format: Journal Article
• Language: English
• Published: Washington, DC American Chemical Society 15.08.1999
• Subjects: Amines - analysis; Analytical chemistry; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, Gas - methods; Effluents; Exact sciences and technology; Gas chromatographic methods; Gas Chromatography-Mass Spectrometry; Kinetics; Microchemistry - methods; Other wastewaters; Pollution; Rivers; Sewage - chemistry; Waste materials; Wastewaters; Water; Water pollution; Water Pollution, Chemical - analysis; Water treatment and pollution; Solid phase extraction; Chemical analysis; Alkylamine; Volatile organic compound; Environmental control; Waste water; Chemical enrichment; Gas chromatography; Multicomponent analysis; Preconcentration; Thermoionic detector; Water pollution; Waste water purification; Quantitative analysis
• ISSN: 0003-2700; 1520-6882
• DOI: 10.1021/ac990197h

An analytical procedure for the determination of free volatile C1−C6 amines in aqueous matrixes has been developed and applied to their determination in wastewater, primary and secondary effluents, and sewage-polluted river samples. The developed analytical procedure involves headspace sampling using solid-phase microextraction with a poly(dimethylpolysiloxane) coating (100 μm) followed by GC-NPD determination and GC/MS confirmation using a tailor-made PoraPLOT amines capillary GC column for volatile amines. Procedural detection limits were compound dependent but ranged from 3 to 56 μg L-1, being close to or lower than the odor threshold concentration, and the reproducibility was ca. 15% (N = 5) in real water samples. The developed analytical procedure is solvent free, cost-effective (no cryogenic trap needed), and faster than existing methods because no derivatization step is involved in the determination. Linearity was compound dependent but ranged at least from 50 to 600 μg L-1.