An ultrasound method for simultaneous extraction of Cr, Cu, Zn, Cd, and Pb from sediment, and determination by flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) was proposed. The experimental results obtained using analytical curves and the method of standard additions agreed at a confidence level of 95% for all the analytes, as determined by FAAS and GFAAS, indicating no significant matrix effects. Recoveries ranged from 80.1 to 93.7% (certified reference material) and from 89 to 107% (spike tests). The LOD and LOQ results from the method were consistent with the techniques used (FAAS and GFAAS), with high analytical throughput. The proposed method was then used to determine Cr, Cu, Zn, Cd, and Pb in river sediment samples from Rio Doce, Minas Gerais, Brazil. The results indicated levels below those permitted by Brazilian legislation for all the analytes, with the exception of Cr.
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