Desenvolvimento de metodologias para determinação de Cd e Pb em amostras de lodo de esgoto e sedimentos com o emprego da espectrometria de absorção atômica com forno tubular na chama e aerossol térmico

Abstract

In this work, Thermospray Flame Furnace Atomic Absorption Spectrometry (TS-FF-AAS) and Flame Atomic Absorption Spectrometry (FAAS) were employed in order to propose methods for determination of total and bioavailability concentration of Cd and Pb in environmental samples. The sediments were collected in the basin of the Jundiaí river and the sewage sludge (industrial and home) in the Jundiaí sewage treatment station. The metals bioavailability contents were determined by extraction using 1.0 g of sample and 25.0 mL HCl 0.1 mol/L for 2 hours in horizontal stirrer 600 rpm. The total concentrations were determined using pre-digestion step for 12h followed by a microwave digestion of 0.1 g sample with 2.0 mL mixture concentrated HNO3 HCl (1:3 v/v) and 1.0 mL of H2O2 using heating program for 34 minutes. In determinations by TS-FF-AAS, 200 μL of sample was carried out into a nickel atomization tube with a flow rate of 0.5 mL/min. During Cd and Pb determinations in extracts HNO3 0.014 mol/L solution was used as carrier. In the case of the digested samples, EDTA 0.5% (m/v) and Triton X-100 0.1% (v/v) solution was used as carrier. The method accuracy was checked by Cd and Pb determination in in three certified samples: NIST 2782 and NIST 146R (industrials sludge) and NIST 8704 (Buffalo river sediment). The bioavailability and total concentrations range in sediments were 0.08-1.7 and 0.44- 2.47 mg/kg for Cd; 2.91- 13.6 and 8.9-24.7 mg/kg for Pb, respectively. Limits of detection (LOD) and quantification (LOQ) for TS-FF-AAS were 1.13 and 3.75 μg/L for Cd, 16.5 and 55.1 μg/L for Pb, respectively (n=3). In FAAS, limits of detection and quantification were 63.0 and 210 μg/L for Cd, 119 and 395 μg/L for Pb, respectively (n=3). The repeatability and reproducibility obtained were 1.0-8.0% and 7.0-24% for Cd, 2.4- 14% and 5.4-32% for Pb, presented as relative standard deviation (RSD, %).