Fe-Ni nano-alloy which was prepared by chemical reduction with KBH4 as reductant and polyethylene glycol (PEG) its dispersant had high surface energy after being deoxiclized in H-2 atmosphere at 400 degrees C. It could cause breakage of C-Cl bond of organic chloride in the presence of a small amount of oxygen. The result of elemental analysis indicated that the reaction products were FeCl2, NiCl2 and Cl-2, the production of Cl-2 was because of the combination of Cl atom or Cl free radical that came from the breakage of C-Cl bond. High-performance liquid chromatography (HPLC) result showed that the existence of new organic compound such as biphenyl and so on. The results of X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) showed that carbon free radical or carbonaceous free radical enchased on the surface of nano-alloy and produced Fe3C, Fe2C after being baked in N-2 atmosphere at 600 degrees C. (C) 2007 Elsevier Ltd. All rights reserved.