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A series of experiments with surrogate materials was performed at bench scale to demonstrate a halogenation technique applicable to the treatment of used aluminum matrix test reactor fuel. The technique involves the dissolution and separation of aluminum from used aluminum matrix test reactor fuel in molten-halide salt systems, as a head-end step to the subsequent treatment and disposition of the fuel's uranium and fission products. The demonstration of the halogenation technique was performed with neodymium metal as a nonradiological surrogate for uranium metal. The experiments involved blending and heating forms of aluminum and neodymium metal with ammonium and lithium chloride or ammonium and lithium bromide. The sublimation and decomposition of ammonium chloride or bromide yielded ammonia gas along with the respective hydrogen chloride or bromide gas, the latter of which reacted and formed the respective aluminum and neodymium halides. At elevated temperatures, aluminum halides gasified and separated from the respective neodymium halides, which fused with their respective lithium halides. Samples of the fused and distillate salts were collected during the series of experiments and analyzed, yielding the extents of aluminum removal that ranged from 94.5-98.2% for chlorination runs and 91.4-97.8% for bromination runs. No neodymium was detected in any of the distillation fractions. Some experiments were repeated to verify the effectiveness, and a portion of aluminum chloride distillate was processed into a consolidated waste form.