The synthesis of high surface area carbide and nitride materials from binary and ternary oxides of vanadium, niobium, tantalum, molybdenum, and tungsten, suitable for use as catalysts for a wide range of reactions, has been investigated via the temperature-programmed reaction (TPRe) method, in various gas mixtures. TPRe of oxides in CH4/H-2, C2H6/H-2, or NH3 yield materials with surface areas >40 m(2) g(-1). For the reaction with ethane or ammonia the reaction appears to proceed topotactically while that with methane does not; however, the conversion of nitrides to-carbides in CH4/H-2 does appear to proceed topotactically.