The speciation of Ga, Ge, Ni, V, S and Fe in fly ash from IGCC power plant were investigated for possible further extraction process by combining conventional mineral and chemical analysis, leaching tests, wet sequential traction, Mosshauer and XAFS spectroscopies. The results shown that Ge occurs mainly as water-soluble species, GeS and/or GeS2 and hexagonal GeO2 Ga is present as an oxide. Ni occurs mainly as nickeline (NiAs), with minor proportions of Ni arsenates and vanadium as V(III) with minor amounts of V(IV) in the aluminosilicate glass matrix. Pyrrhotite and wurtzite-sphalerite are Sulfide species containing Fe and Zn. but an important fraction of iron is also present in the aluminosilicate glass. These clear differences between the speciation of the above element,, in this material and those reported for fly ash from conventional PC combustion. (c) 2004 Elsevier Ltd. All rights reserved.