Abstract
The study proposes a simple and fast extraction-based procedure for the determination of trace elements in estuarine sediment samples by inductively coupled plasma mass spectrometry (ICP-MS). The extraction conditions were optimized using a central composite design. Optimum results were obtained when 100mg of sediment sample was used followed by ultrasound-assisted extraction for 15min with 7.50molL−1 HF (1mL HF) and 3.50molL−1 HNO3 (1mL HNO3 65%m/m). Calibration against aqueous standards was carried out with rhodium as an internal standard. The method was successfully applied for the quantitative extraction of As, Cd, Co, Cr, Cu, Ni, Pb, Sn, V and Zn. Detection limits ranging from 0.02 to 0.1μgg−1 and relative standard deviation lower than 8% were obtained. The method accuracy was assessed by using three certified reference materials and comparing the results from the extraction procedure with those obtained following microwave-assisted digestion of the samples; no statistical differences, based on t-test at a confidence level of 95%, were detected. The proposed method showed to be simple and fast and can be applied for sediment samples with the elimination of the sample digestion step prior to analysis.
•An extraction-based procedure for the determination of trace elements is proposed.•A central composite design was employed to optimize the extraction conditions.•As, Cd, Co, Cr, Cu, Ni, Pb, Sn, V and Zn were determined in sediment samples.•Reduced amounts of sample and acid were used, along with a short extraction time.•The procedure is an alternative to the traditional acid-based digestion protocols.