R. Vichot et Kg. Furton, VARIABLES INFLUENCING THE DIRECT DETERMINATION OF HALOACETIC ACIDS INWATER BY REVERSED-PHASE ION-PAIR CHROMATOGRAPHY WITH INDIRECT UV DETECTION, Journal of liquid chromatography, 17(20), 1994, pp. 4405-4429
A reversed-phase ion-pair chromatographic system for the direct determ
ination of haloacetic acids in water has been optimized utilizing indi
rect photometric detection. Acetic, chloroacetic, bromoacetic, iodoace
tic, dichloroacetic and dibromoacetic acids were used to characterize
the chromatographic system. The effect of temperature on retention tim
e shows a non linear van't Hoff behavior indicating a change in the me
chanism of retention at about 30 degrees C. Above 30 degrees C, retent
ion times decreased proportionally to increases in the temperature of
the column. Separations are achieved in the pH range of 3.5 to 6.3 wit
h an optimum at ca. pH 5.4. Increases in the concentrations of KH2PO4,
1-hexanesulfonate (competing ion) and acetonitrile result in proporti
onal decreases in capacity factors with some selectivity variations de
pending on the analyte. Increases in the concentration of benzyltribut
ylammonium ion (ion interaction reagent) resulted in increases in capa
city factors with a usable range from 8 to 12 mM. Of the reversed phas
es studied, Spherisorb C-18 yielded the optimal results for the acids
studied. Linear calibration curves for these acids were obtained utili
zing indirect UV detection with detection limits as low as 2 parts per
million.