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  • Determination of aldehydes in drinking water using pentafluorobenzylhydroxylamine derivatization and solid-phase microextraction.

Determination of aldehydes in drinking water using pentafluorobenzylhydroxylamine derivatization and solid-phase microextraction.

Journal of chromatography. A (2002-02-01)
Beatriz Cancho, Francesc Ventura, M Teresa Galceran
ABSTRACT

A headspace solid-phase microextraction (HS-SPME) procedure followed by gas chromatography and electron capture detection (GC-ECD) has been developed for the determination of aldehydes in drinking water samples at microg/l concentrations. A previous derivatization with o-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) was performed due to the high polarity and instability of these ozonation by-products. Several SPME coatings were tested and the divinylbenzene-polydimethylsiloxane (DVB-PDMS) coating in being the most suitable for the determination of these analytes. Experimental SPME parameters such as selection of coating, sample volume, addition of salt, extraction time and temperature of desorption were studied. Analytical parameters such as precision, linearity and detection limits were also determined. HS-SPME was compared to liquid-liquid microextraction (proposed in US Environmental Protection Agency Method 556) by analyzing spiked water samples; a good agreement between results obtained with both techniques was observed. Finally, aldehydes formed at the Barcelona water treatment plant (N.E. Spain) were determined at levels of 0.1-0.5 microg/l. As a conclusion, HS-SPME is a powerful tool for determining ozonation by-products in treated water.

MATERIALS
Product Number
Brand
Product Description

Supelco
SS-174 PTFE-Faced Septa, diam. 12.5 mm ( 1/2 in.)
Supelco
SS-174 PTFE-Faced Septa, diam. 9.5 mm ( 3/8 in.), pkg of 100 ea
Supelco
O-(2,3,4,5,6-Pentafluorobenzyl)hydroxylamine hydrochloride, for GC derivatization, LiChropur, ≥99.0% (AT)
Sigma-Aldrich
O-(2,3,4,5,6-Pentafluorobenzyl)hydroxylamine hydrochloride, ≥98%