Jag. Neto et al., DETERMINATION OF CADMIUM IN FOODSTUFFS AND PLANT MATERIALS BY FLOW INJECTION-SPECTROPHOTOMETRY INCLUDING ION-EXCHANGE, Analytica chimica acta, 306(2-3), 1995, pp. 343-349
A flow-injection system with a minicolumn packed with a strongly basic
anion exchanger (AG1-X8 resin, 200-400 mesh) is proposed for the spec
trophotometric determination of cadmium in foodstuffs, plants and simi
lar based on the formation of a cadmium iodide-Malachite Green (MG) as
sociate. Improved sensitivity and selectivity are attained since cadmi
um is in-line concentrated as chlorocomplexes whereas lead, copper and
other potential interferents are discarded. Reagent compositions, flo
w rates, commutation times, mean available time for chlorocomplexes fo
rmation, and conditions for concentration and elution were investigate
d. A 2.0 M NaCl-0.1 M HCl solution was elected for chlorocomplexes for
mation, and a 90-s concentration time was set. The eluant, also sample
carrier stream, was a 2.0 M NaNO3 plus 0.1 M HNO3 solution. The propo
sed system handles about 25 samples per hour (2.50-25.0 mu g Cd l(-1))
, consuming ca. 8 ml of sample, 0.25 mg MG and 0.41 g KI per determina
tion. The detection limit is 0.11 mu g Cd l(-1). Results are precise (
R.S.D. 2.72 and 2.26% for 5.12 and 19.7 mu g Cd l(-1)) and in agreemen
t with certified values of standard reference materials. Recoveries wi
thin 99.1 and 111.2% were found. With two resin minicolumns, the appli
cability of the system is expanded, and samples solubilized with nitri
c and perchloric acids can also be run. The first minicolumn stands fo
r in-line perchlorate removal before chlorocomplex formation, and the
second one for cadmium concentration. Although more complex, similar s
ystem performance and results quality relatively to the system with a
single minicolumn are attained.