Determination of cadmium in sediments and in sewage sludge by slurry sampling electrothermal atomic absorption spectrometry using iridium as permanent modifier

Abstract

A procedure for the determination of Cd in sediment and sewage sludge as slurries by electrothermal atomic absorption spectrometry is proposed. The slurry, 1 mg mL-1, was prepared by mixing sample ground to a particle size £ 50 mm with 5% v/v nitric acid in an ultrasonic bath. The homogeneity of the slurries was assured by passing a constant flow of argon into the autosampler cup, just before transferring an aliquot to the graphite furnace. Two permanent modifiers deposited on the platform were tested: Ru and Ir. Modifiers in solution were also tested: Pd plus Mg and phosphate alone or plus Mg. The Ir-treated tube was adopted due to its good performance as modifier and also for practical reasons. About 80% of Cd is extracted to the water phase of the slurry. To test the accuracy of the method, three certified materials were analyzed: a marine sediment, a river sediment and a domestic sewage sludge. The concentrations obtained, using calibration against aqueous standards prepared in the same medium as the slurries, are in agreement with the certified values, at a confidence level of 95%, according to the Student-t test. The limit of detection (3s) was 43 ng g-1 in the solid sample and the relative standard deviation for the sediment MESS-2 was 2.3% (n = 10).