US EPA

7757603 

Journal Article 

A CONTINUOUS 2-PHASE REACTION SYSTEM COUPLED ONLINE WITH CAPILLARY CHROMATOGRAPHY FOR THE DETERMINATION OF POLAR SOLUTES IN WATER 

Goosens, EC; Broekman, MH; Wolters, MH; Strijker, RE; Dejong, D; Dejong, GJ; Brinkman, UAT 

1992 

1 

Journal of High Resolution Chromatography (HRC)
ISSN: 0935-6304
EISSN: 1521-4168 

15 

4 

242-248 

English 

10.1002/jhrc.1240150408 

WOS:A1992JB05900007 

Gas chromatographic procedures are described for the determination of carboxylic acids and chlorinated anilines in water samples. Propionic acid and 2,6‐difluorobenzoic acid in aqueous solution have been simultaneously alkylated and extracted by means of a continuous two‐phase reaction system, and then quantitated by on‐line coupled capillary gas chromatography; tetrahexyl‐ammonium hydrogen sulfate was used as phase transfer catalyst and pentafluorobenzyl bromide as reagent. A factorial design approach was used to optimize on‐line derivatization of aqueous propionic acid with regard to pH and concentration of phase transfer catalyst. Alkylation and extraction, under optimized conditions, followed by quantitation of the pentafluorobenzyl ester by flame ionization detection furnished a linear calibration for concentrations between 0.1 and 10 μg/ml. The relative standard deviation was 9–15 %. The continuous two‐phase reaction system was also used to determine (chlorinated) anilines present in water at concentrations of 0.1–1 μg/ml; pentafluorobenzoyl chloride was used as reagent and analysis was performed by capillary gas chromatography with flame ionization or electron capture detection. The on‐line acylation of p‐chloroaniline was optimized with regard to pH, reagent concentration, and reaction time. The on‐line reaction system worked satisfactorily for both applications, although excess reagent caused some problems with the chromatography. Copyright © 1992 Dr. Alfred Huethig Publishers 

CAPILLARY GC; ONLINE EXTRACTIVE ALKYLATION; ONLINE ACYLATION; CARBOXYLIC ACIDS; AMINES