Electron Capture Gas Chromatography of Tertiary Amines After a Demethylation Reaction to Secondary Amines

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Abstract
A gas chromatographic method for the determination of tertiary amines in micro- and nanogram amounts is presented. The tertiary amine is reacted with ethyl chloroformate to form a urethan, which is cleaved to a secondary amine. This is transformed to heptafluoro-butyramide, which makes quantitative determination with electron capture detection possible. The yields of the secondary amines for two tertiary amines were 60 and 75%. By use of internal standard technique in the entire reaction recoveries of 97.6 ± 2.2% at the 100 μg level and 100 ± 4% at the 200 ng level were obtained.