The contamination of sediments with polychlorinated organics such as polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (Dioxins) and polychlorinated naphthalenes (PCNs) remains a significant problem in many rivers, harbors, and estuarine areas in the US and around the world. In this work, rapid dechlorination of PCBs, PCNs, and Dioxins by palladium - coated magnesium (0.01% by weight Pd) has been demonstrated in pure solvent systems (10% methanol in distilled water). This reaction was investigated with the goal of developing it as a future sediment treatment method. More than 90% of the initial single PCB congeners BZ 3 and 170 were removed in 1 to 10 minutes and about 58% of the total initial Arochlor 1260 was removed in 4 minutes. The removal of single Dioxin and PCN congeners also occurred rapidly resulting in a 69 to 95% reduction in 30 minutes. Rapid removal of biphenyl, the expected degradation end product for PCBs, was also observed (80% removal in 5 minutes). Experiments conducted with Arochlor 1260 and biphenyl did not identify significant volatile fractions. A significant amount of PCBs were extracted from the filtered Mg/Pd material suggesting that PCBs first adsorb to the surface of the bimetal and then dechlorination occurs; lesser chlorinated congeners and biphenyl were also found adsorbed to the Mg/Pd material. Experiments conducted with single PCB congeners BZ 194 and 204 demonstrated the formation of lower - chlorinated PCB congeners, indicating that dechlorination was occurring. A stepwise dechlorination process was suggested in which chlorines in the ortho position were removed last.