Evaluation of a sequential extraction process used for determining mercury binding mechanisms to coal combustion byproducts.

Leaching of mercury from coal combustion byproducts is a concern because of the toxicity of mercury. Leachability of mercury can be assessed by using sequential extraction procedures. Sequential extraction procedures are commonly used to determine the speciation and mobility of trace metals in solid samples and are designed to differentiate among metals bound by different mechanisms and to different solid phases. This study evaluated the selectivity and effectiveness of a sequential extraction process used to determine mercury binding mechanisms to various materials. A six-step sequential extraction process was applied to laboratory-synthesized materials with known mercury concentrations and binding mechanisms. These materials were calcite, hematite, goethite, and titanium dioxide. Fly ash from a full-scale power plant was also investigated. The concentrations of mercury were measured using inductively coupled plasma (ICP) mass spectrometry, whereas the major elements were measured by ICP atomic emission spectrometry. The materials were characterized by X-ray powder diffraction and scanning electron microscopy with energy dispersive spectroscopy. The sequential extraction procedure provided information about the solid phases with which mercury was associated in the solid sample. The procedure effectively extracted mercury from the target phases. The procedure was generally selective in extracting mercury. However, some steps in the procedure extracted mercury from nontarget phases, and others resulted in mercury redistribution. Iron from hematite and goethite was only leached in the reducible and residual extraction steps. Some mercury associated with goethite was extracted in the ion exchangeable step, whereas mercury associated with hematite was extracted almost entirely in the residual step. Calcium in calcite and mercury associated with calcite were primarily removed in the acid-soluble extraction step. Titanium in titanium dioxide and mercury adsorbed onto titanium dioxide were extracted almost entirely in the residual step.