DETERMINATION OF CHLORIDE, NITRATE, SULFATE, NITRITE, FLUORIDE, AND PHOSPHATE BY ON LINE COUPLED CAPILLARY ISOTACHOPHORESIS-CAPILLARY ZONE ELECTROPHORESIS WITH CONDUCTIVITY DETECTION
D. Kaniansky et al., DETERMINATION OF CHLORIDE, NITRATE, SULFATE, NITRITE, FLUORIDE, AND PHOSPHATE BY ON LINE COUPLED CAPILLARY ISOTACHOPHORESIS-CAPILLARY ZONE ELECTROPHORESIS WITH CONDUCTIVITY DETECTION, Analytical chemistry, 66(23), 1994, pp. 4258-4264
Capillary zone electrophoresis (CZE) on-line coupled with capillary is
otachophoresis (ITP) in the column-coupling configuration of the separ
ation unit was studied for determination of nitrite, fluoride, and pho
sphate persent in a large excess of chloride, nitrate, and sulfate. Su
ch distributions of these anions are typical for many environmental ma
trices, and it is shown that the ITP-CZE tandem enables the ITP determ
ination of the macroconstituents, while ITP-preconcentrated microconst
ituents cleaned up from the macroconstituents can be determined by CZE
with a conductivity detector. This approach was effective when the co
ncentration ratio of macro-microconstituents was less than (2-3) x 10(
4). The limits of detection achieved for the microconstituents (200, 3
00, and 600 pptr for nitrite, fluoride, and phosphate, respectively) e
nabled their determinations at low parts per billion concentrations in
instances when the concentrations of sulfate or chloride in the sampl
es were higher than 1000 ppm. Although in such situations the load cap
acity of the ITP column was not sufficient to provide the quantitation
s of the macroconstituents, the ITP sample cleanup enabled the CZE det
erminations of the microconstituents present in the samples at 10(5)-1
0(6)-fold lower concentrations. Experiments with samples of such extre
me compositions showed that anionic impurities from the ITP electrolyt
e solutions transferred together with the analytes into the CZE column
are probably the main hindrances in extending this dynamic concentrat
ion range by decreasing the limits of the detection to a level associa
ted with the noise characteristics of the conductivity detector.