Abstract
There is a current trend in automation of leaching tests for trace elements in solid matrixes by use of flow injection based column approaches. However, as a result of the downscaled dimensions of the analytical manifold and execution of a single extraction at a time, miniaturized flow-through column approaches have merely found applications for periodic investigations of trace element mobility in highly homogeneous environmental solids. A novel flow-based configuration capitalized on stirred-flow cell extraction is proposed in this work for simultaneous fractionation of trace elements in three solid wastes with no limitation of sample amount up to 1.0 g. A two-step sequential extraction scheme involving water and acetic acid (or acetic acid/acetate buffer) is utilized for accurate assessment of readily mobilizable fractions of trace elements in fly ash samples. The fully automated extraction system features high tolerance to flow rates (< or = 6 mL min(-1)) and, as opposed to operationally defined batchwise methods, the solid to liquid ratio is not a critical parameter for determination of overall readily leachable trace elements provided that exhaustive extraction is ensured. Analytical performance of the dynamic extractor is evaluated for fractionation analysis of a real coal fly ash and BCR-176R fly ash certified reference material. No significant differences were found at the 0.05 significance level between summation of leached concentrations in each fraction plus residue and concentration values of BCR-176R, thus revealing the accuracy of the automated method. Overall extractable pools of trace metals in three samples are separated in less than 115 min, even for highly contaminated ashes, versus 18-24 h per fraction in equilibrium leaching tests. The multiple stirred-flow cell assembly is thus suitable for routine risk assessment studies of industrial solid byproduct.
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