Abstract

The present paper describes the development of a method for the determination of copper in airborne particulate matter using slurry sampling and chemical vapor generation atomic absorption spectrometry (CVG AAS). Chemometric tools were employed to characterize the influence of several factors on the generation of volatile copper species. First, a two-level full factorial design was performed that included the following chemical variables: hydrochloric acid concentration, tetrahydroborate concentration, sulfanilamide concentration and tetrahydroborate volume, using absorbance as the response. Under the established experimental conditions, the hydrochloric acid concentration had the greatest influence on the generation of volatile copper species. Subsequently, a Box–Behnken design was performed to determine the optimum conditions for these parameters. A second chemometric study employing a two-level full factorial design was performed to evaluate the following physical factors: tetrahydroborate flow rate, flame composition, alcohol volume and sample volume. The results of this study demonstrated that the tetrahydroborate flow rate was critical for the process. The chemometric experiments determined the following experimental conditions for the method: hydrochloric acid concentration, 0.208M; tetrahydroborate concentration, 4.59%; sulfanilamide concentration, 0.79%; tetrahydroborate volume, 2.50mL; tetrahydroborate flow rate, 6.50mLmin−1; alcohol volume, 200µL; and sample volume, 7.0mL. Thus, this method, using a slurry volume of 500µL and a final dilution of 7mL, allowed for the determination of copper with limits of detection and quantification of 0.30 and 0.99µgL−1, respectively. Precisions, expressed as RSD%, of 4.6 and 2.8% were obtained using copper solutions at concentrations of 5.0 and 50.0µgL−1, respectively. The accuracy was evaluated by the analysis of a certified reference material of urban particulate matter. The copper concentration obtained was 570±63mgkg−1, and the certified value was 610±70mgkg−1. This method was applied for the determination of copper in airborne particulate matter samples collected in two Brazilian regions of Bahia State, Brazil. The copper contents found varied from 14.46 to 164.31ngm−3.

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