Determination of saturated and a-unsaturated aliphatic aldehydes in environmental water samples by GC

• Published in: Bunseki kagaku Vol. 37; no. 10; pp. 519 - 523
• Main Authors: BABA, Kenzo, ISHIKAWA, Seiichi, HANADA, Yosifumi, UCHIMURA, Yutaka, SUETA, Shintaro, KIDO, Kozo
• Format: Journal Article
• Language: English
• Published: Tokyo Japan Science and Technology Agency 1988
• ISSN: 0525-1931
• DOI: 10.2116/bunsekikagaku.37.10_519

A method for the separation and determination of trace amounts of saturated and unsaturated aliphatic aldehydes, in environmental waters is described, in which aldehydes were converted to their O-(pentafluorobenzyl) oximes with O-(pentafluorobenzyl) hydroxylamine (PFBOA). Then the PFBOA derivatives were measured with a gas chromatograph equipped with a flame thermionic detector (GC-FTD). The water sample (500 ml) was purified and concentrated to 40 ml by distillation. The distillate was added to 5 ml PFBOA solution (2 mg/ml) and reacted at 20°C for over 4 h. Then 1 ml of sulfuric acid was added to the reacted solution, and PFBOA derivatives were extracted with 10 ml of hexane. The heaxne layer was washed with 40 ml of water, dried over anhydrous sodium sulfate and concentrated to about 2 ml in a Kuderna-Danish concentrator. As the internal standard, m-nitrotoluene was added. Each PFBOA derivative was measured by GC-FTD using a 5% phenylmethylsilicone fused silica capillary column. Butyraldehyde, isobutyraldehyde, crotonaldehyde and methacrolein could be separated from each other and determined with high sensitivity. Recoveries of the aldehydes from pure water in the range of 14μg/l were 77110% with a relative standard deviation of 2.69.7%. The detection limits were 0.60.9μg/l. Recoveries from river and seawater were 9096% and 8694%, respectively. Each PFBOA derivative was identified by GC/MS.