A. Krug et R. Kellner, DETERMINATION OF CITRIC-ACID BY MEANS OF COMPETITIVE COMPLEX-FORMATION IN A FLOW-INJECTION SYSTEM, Mikrochimica acta, 113(3-6), 1994, pp. 203-210
A photometric method for the determination of citrate and other organi
c acids based on their ability to complex Fe3+-ions is presented. The
red colored complex of [Fe(SCN)2]+, used as reagent, is destroyed upon
contact with the sample because the organic acid complexes the Fe3+-i
on. The decrease in absorption is monitored at 460 nm. The reaction is
carried out in a simple flow injection system either in single or pre
ferably double channel configuration. The influence of pH was investig
ated. Best results were obtained by adjusting the carrier stream to pH
2.0-2.5 with a KCl/HCl-buffer. With an increasing concentration of re
agent the linear range is shifted to higher citrate concentrations. Th
e slope of the calibration graph and the linear range are influenced b
y the sample volume. Other variations of parameters include flow rate,
reactor volume and diameter of tubing. Generally speaking, optimum co
nditions for the flow system are not specified because they vary with
the application. The typical conditions for a calibration graph from 1
to 8 mmol/l citrate were a reagent concentration of 2.6 mmol/l [Fe(SC
N)2]+, a flow rate of 2.4 ml/min, a reactor length of 50 cm with tubin
g of 0.97 mm inner diameter and a sample volume of 100 mul. At these s
ystem settings the coefficients of variation were 2.5% and 1.6% for ei
ght replicate measurements of samples containing 4 mmol/l and 8 mmol/l
citrate, respectively. Up to 180 samples can be analyzed per hour. Na
turally the method is disturbed by all other ions that form complexes
or precipitates with Fe3+ -ions. Therefore its application is limited
to samples with a known matrix, which was given in the analysis of cit
rate in lemon flavored soft drinks, where the citric acid usually acco
unts for 95 to 99% of the total acidity and other interfering ions are
absent.