Abstract
A method for the simultaneous determination of metals (Fe 3+, Fe 2+, Cu, Ni, Zn, Co, Cd, Mn and Pb) at μg/l levels in environmental matrices is demonstrated. The metals are separated by ion chromatography on a mixed-bead ion-exchange column (IonPac CS5A) and detected by post-column reaction and spectrophotometric detection. The use of a gradient program (based on oxalic acid–hydrochloric acid–sodium chloride and sodium nitrate eluents) allows the separation of nine metals in a single run. The direct injection of a large volume of samples lowers the detection limits to below and/or few μg/l. The chromatographic conditions and colour-development reaction were optimised. Two post-column reagents, 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) and 4-(2-pyridylazo) resorcinol, were tested and detection limits were compared. The use of 5-Br-PADAP increased the sensibility for Cu, Cd, Zn and Mn. For the proposed method, linearity, reproducibility, detection limits and interference due to alkaline-earth metals (noticeably Mg and Ca) were discussed. Under the suggested chromatographic conditions Mg 2+ and Ca 2+ up to 0.2 g/l do not interfere with separation and quantitative analysis of the metals. The calibration graphs were linear ( r 2>0.986) in the range 5–5000 μg/l. The application of the method to the determination of metals in coastal marine sediments is shown.
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