Jh. Watkinson et Mj. Kear, HIGH-PERFORMANCE ION CHROMATOGRAPHY MEASUREMENT OF SULFATE IN 20 MM PHOSPHATE EXTRACTS OF SOIL, Communications in soil science and plant analysis, 25(7-8), 1994, pp. 1015-1033
High Performance Ion Chromatography (HPIC) methods for measuring sulfa
te in 20 mM phosphate extracts of soil need to cope with low sulfate (
down to 0.1 ppm S) in up to 5000 times the molar concentration of phos
phate and potassium or calcium, a diversity of solutes including organ
ic compounds, and colloidal particles. Anions were detected by electri
cal conductivity rather than indirect photometry, because interference
from the high phosphate concentration on sulfate measurements was muc
h less, particularly under acid conditions. Orthophosphate has a much
lower limiting equivalent conductivity than sulfate, and H2PO4- has on
ly half the conductivity of HPO42-. Also, H2PO4- is retained less, and
in acid gives a wide peak separation from sulfate. Under the acid con
ditions proposed the phosphate peak is negative, and elutes just after
the solvent front, thus eliminating interference on sulfate. By makin
g the acid pH of the eluent that of the extractant, pH 4, baseline cha
nges were also minimized. Eluents of trimesic acid (TMA) and o-phthali
c acid (PA), were investigated. PA required a higher eluent concentrat
ion than TMA to elute sulfate rapidly but, with the instrumentation us
ed, the stability of the higher baseline conductance was no problem an
d PA, unlike TMA, produced no interfering system peaks. The method usi
ng PA has been used commercially by the New Zealand AgResearch Soil Fe
rtility Service for over three years on a variety of soils involving o
ver 75,000 samples.