Ultrasound-assisted pseudodigestion for toxic metals determination in fish muscles followed by electrothermal atomic absorption spectrophotometry: multivariate strategy.

A simple and efficient procedure for the determination of arsenic (As), cadmium (Cd), and lead (Pb) in the edible parts of freshwater fish by ultrasonic-assisted acid pseudodigestion (USD) was developed. A Plackett-Burman experimental design was used as a multivariate strategy for the evaluation of the effects of several variables at once. Five variables--sonication time, sample mass of muscle tissue, temperature of the ultrasonic bath, mL of nitric acid, and mL of a mixture of acid and oxidant--were regarded as factors. From these studies, certain variables showed up as significant, and they were optimized by a 23+star central composite design, which involved 16 experiments. Optimum values of the variables were selected for the development of USD to determine the contents of As, Cd, and Pb in fish muscles used as pollution bioindicators from Lake Manchar (Sindh, Pakistan). The determination of the 3 toxic metals under study was performed by electrothermal atomic absorption spectrometry. The accuracy of the optimized procedure was evaluated by analysis of certified reference materials BCR 185R bovine liver and by comparison with conventional wet acid digestion methodology. The result obtained by the optimized method showed good agreement with the certified values and sufficiently high recovery. No significant differences were observed for P = 0.05. Relative standard deviation values (average of 10 separate determinations) were 1.21, 5.52, and 5.32% for As, Cd, and Pb, respectively.

Speciation of heavy metals in untreated domestic wastewater sludge by time saving BCR sequential extraction method.

In this work the modified three-stage sequential extraction procedure developed within the Standards, Measurement and Testing Programme (formally the Community Bureau of Reference BCR) of the European Commission, was applied for the fractionation of Cd, Cr, Cu, Ni, Pb and Zn in the untreated domestic wastewater sludge (DWS) collected from the Hyderabad city of Pakistan. The aim of our study was to evaluate the impact of different time intervals for shaking, and sample mass of sewage sludge on optimal recovery of all metals under study. Analyses of the extracts were performed by flame atomic absorption spectrometry (FAAS) and electrothermal atomic absorption spectrometry (ETAAS). The precision and accuracy of the proposed procedure was evaluated by using a certified reference material of soil amended with sewage sludge BCR 483. The maximum recoveries for Cd and Zn were observed for all three steps of BCR protocol at 26 hours (h) total shaking period, while Cr, Cu, Ni and Pb were achieved at 32 hours instead of previously reported 51 hours, with (p < 0.05). The maximum level of all heavy metals was achieved in samples mass 0.2-0.4 g, where as the extractant-sample mass ratio was kept according to the optimized BCR method. The results of the sequential extraction study of untreated DWS indicates that more easily mobilized forms (acid exchangeable) were found to be 31.0, 3.1, 2.5, 7.6, 2.6 and 8.4% of total contents of Cd, Cr, Cu, Ni, Pb and Zn, respectively. The oxidizable fraction is dominant for all the heavy metals, except Cd. The lixiviation tests (DIN 38414-S4) were used to evaluate the leaching of heavy metals from sewage sludge used for agricultural purposes.