Authors: Inmaculada de la Calle, Noelia Cabaleiro, Isela Lavilla, Carlos Bendicho
Journal: International Journal of Environmental Analytical Chemistry, 91: 1401-1411, 09/2011
A simple, fast and reliable method is described for the quantitative extraction of Sb and Co from inorganic environmental matrices containing variable amounts of silicates prior to their determination by electrothermal-atomic absorption spectrometry. The method is based on the ultrasound-assisted extraction of both elements using the mixture 20% v/v HF + 20% v/v HNO3 as extractant. The extraction procedure was carried out in closed Eppendorf vials immersed in a cup-horn sonoreactor for 20 min. Once extraction has been accomplished, the supernatant liquid is separated from the solid phase and subsequently transferred into the autosampler of the instrument. A two-level full factorial design (24) was applied for screening optimisation of the variables influencing the ultrasonic extraction. These variables were: sonication time; amplitude of the ultrasound energy; nitric and hydrofluoric acid concentrations. MLDs were 0.20 and 0.06 µg · g−1 for Sb and Co, respectively. Between-batch precision values, expressed as relative standard deviations (n = 3), were less than 5.5 and 9.6% for Sb and Co, respectively. The method was evaluated using a wide variety of inorganic certified reference materials, such as SRM 2702 (Marine Sediment), SRM 2782 (Industrial Sludge), BCR 176R (Fly Ash), SRM 1633b (Coal Fly Ash) SRM 2710 (Montana Soil) and SRM 2711 (Montana Soil).