2.2. Sequential extraction
Sequential extraction involves the treatment of a solid material with a series of chemical reagents with increasing dissolution and displacement power, in order to extract metals according to the chemical activity and property of their binding to the solid. Depending upon the reagents chosen, the method can assess the level of water-soluble and exchangeable metals, as well as metals contained in easily reducible or oxidizable compounds. Thus, a sequential extraction scheme will operationally distinguish between reversibly and irreversibly (or slowly reversibly) associated metal fractions in the sediments.
In this experiment, sequential extraction was performed broadly as described by Oughton et al. [10], but modified according to the work done by Gómez Ariza et al. [12]. The leachate sediments had a relatively high iron content (4.1–24%), and Gómez Ariza et al. reported that it was necessary to perform several repetitions (up to seven) of extraction step 4 (0.4 M NH2OH·HCl in 25% (v/v) acetic acid) in order to achieve complete extraction of reducible compounds from iron-rich sediments. The extraction procedure was thus modified by increasing the concentration of NH2OH·HCl from 0.04 to 0.4 M in step 4, and by performing this step seven times instead of once. It is known that concentrations of NH2OH·HCl even as high as 1 M will not dissolve metal bound to organic matter or silicates [13]. The entire procedure is shown schematically in Fig. 2.