Study of matrix effects and spectral interferences in the determination of lead in sediments, sludges and soils by SR-ETAAS using slurry sampling

Abstract

An interference-free, fast, and simple method is proposed for Pb determination in environmental solid samples combining slurry sampling and electrothermal atomic absorption spectrometry. Samples were ground to an adequate particle size and slurries were prepared by weighing from 0.05 g to 0.20 g of dry sediment, adding nitric acid, and a solution containing 0.1% Triton X-100. Ultrasonic agitation was employed for slurries homogenization. Analytical variables including acid pre-treatment conditions, particle size, slurry stability, temperature program of the graphite furnace, and type and concentration of the chemical modifier were studied. The undesirable effects of potential non-specific and spectral interferences on Pb signal were also taken into account. Continuum source and self-reversal methods for background correction were evaluated and compared. For calibration, synthetic acid solutions of Pb were employed. Calibration was linear within the range 1–30 μg L−1 and 5–30 μg L−1 when the 217.0 nm and 283.3 nm analytical lines were used. Correlation coefficients of 0.9992 and 0.9997 were obtained. Using optimized conditions, limits of detection (3σ) of 0.025 μg g−1 and 0.1 μg g−1 were achieved for the 217.0 nm and 283.3 nm analytical lines, respectively. The method was successfully applied to the determination of lead in soil, contaminated soil, municipal sludge, and sediment samples. The accuracy was assessed by the analysis of two certified reference materials: municipal sludge (QC MUNICIPAL SLUDGE A) and lake sediment (TRAP-LRM from IJS).