The large quantity of wash water used in the electroplating and etching process in the manufacturing of printed circuit boards (PCBs) contains a high level of heavy metal ions (Cu ++, Zn ++, Ni ++, Cr +++, Pb ++). These potentially toxic ions are removed from the wash water effluent through a polyelectrolyte flocculation and hydroxide precipitation process during which a hydroxide sediment sludge rich in metal ions and polymers is generated. This sediment sludge possesses some unique characteristics and properties in terms of composition, fine particle size distribution, high specific surface area, and a tendency to agglomerate after drying. Direct disposal of this classified “special waste” (Department of Environment of Northern Ireland, The Special Waste Regulations, Northern Ireland, 1998) at landfill sites may cause serious soil and underground water pollution through a gradual ionic leaching process. This paper describes an experimental investigation, exploratory in nature, which employs microwave radiation for detoxification of the sediment sludge through microwave heating, drying and metal ion immobilization within the sediment solids. The effectiveness of microwave assisted binding and immobilization of the metal ions within the sediment solids was studied in conjunction with an evaluation of microwave energy efficiency in comparison to the more conventional convective heating and drying processes. Given a sufficient amount of microwave radiation, leaching of Cu 2+ and Pb 2+ was reduced by 2700% and 1080%, respectively, over a period of 12 weeks, and further leaching was not detectable within six months at simulated local landfill aqueous conditions. This paper also attempts, through experimental observation, to add to the very limited understanding of the complex interactions and binding of free metal ions with the polymeric materials and metal hydroxides under the influence of an electromagnetic field. The high specific surface of the sediment solids and their adsorption properties were further explored and characterized in a study of adsorption of reactive dyes by the microwave processed solids.