Electrothermal atomic absorption spectrometric determination of lead, cadmium, copper and zinc in high-salt content samples after simultaneous separation on polyethylene powder impregnated with 1-(2-pyridylazo)-2-naphthol: application to the analysis of hemodialysis fluids

Abstract

A simultaneous separation and preconcentration of lead, cadmium, zinc and copper from high-salt content matrices for subsequent electrothermal atomic absorption spectrometric determination was developed. The metals were preconcentrated on a micro-column filled with polyethylene powder impregnated with the complexing agent 1-(2-pyridylazo)-2-naphthol. The determinations, without the interference of the saline matrix, were carried out after metals elution with a small volume of an ethanolic solution of nitric acid. The saline matrices were sodium, potassium, magnesium and calcium chlorides, sodium acetate and bicarbonate, which constitute concentrates for hemodialysis. The immobilisation capacity of the complexing agent is about 2.5 µmol per gram of polyethylene and the column capacity with respect to each metal is about 0.75 µmol per gram resin for copper, cadmium and zinc and 0.25 µmol per gram for lead. For the optimisation of the procedure, effects of sample flow rate and pH, eluent composition and concentration, and the influence of salts on the complexation of the metals were investigated. The proposed method was characterised by a precision of about 95% (n = 3) and recoveries from spiked samples of the salts were 81–112%. All results were in agreement with those obtained by anodic stripping voltammetry, the technique used for comparison. The method was applied to the analysis of saline concentrates for hemodialysis, where the investigated metals were found in concentrations between 3.1 µg l^–1 for cadmium and 90.5 µg l^–1 for zinc.