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Gas chromatographic and mass spectrometric determination of some resin and fatty acids in pulpmill effluents as their pentafluorobenzyl ester derivatives

✍ Scribed by Lee Hing-Biu; Thomas E. Peart; John M. Carron


Publisher
Elsevier Science
Year
1990
Tongue
English
Weight
823 KB
Volume
498
Category
Article
ISSN
1873-3778

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✦ Synopsis


A sensitive gas chromatographic method for the determination of resin and fatty acids commonly found in pulpmill effluents is presented. The acids are extracted from effluent samples at pH 8 by methyl tert.-butyl ether and converted into their respective pentafluorobenzyl ester derivatives. After silica gel column cleanup, sample extracts are analyzed by gas chromatography with an electron-capture detector using a 30-m DB-17 column. Mass spectral data of these esters obtained under electron impact and electron capture negative ion chemical ionization conditions are also described. The abundant and characteristic (M ~ 181)-ions are used for the identification and quantitation of resin and fatty acids using a selected ion monitoring technique. Using an effluent with a low blank, spiked recovery of a mixture of 15 acids at lOOO-, lOO-and lo-pg/l levels is quantitative.

Based on a 25-ml sample and a concentration factor of 10, the method detection limit is 1 pg/l for all acids. Application of this procedure to some Canadian pulpmill samples is also presented.