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For plasmonic alloy nanoparticles, theoretical modeling and experimental characterization are both central to our capabilities involving predictable synthesis and targeted applications. This article uses composition-tunable colloidal Au−Cu nanoparticles as a model system for exploring the issue of reliable experimental determination of composition in plasmonic alloy nanoparticles and correlation of this experimental data with theoretical predictions. Highly uniform spherical Au1-xCux alloy nanoparticles were synthesized with compositions ranging from x = 0 to 0.5. The particle compositions were analyzed independently using both powder X-ray diffraction (XRD) and energy dispersive X-ray spectroscopy (EDS), which represent two of the most common nanoparticle composition analysis techniques. The plasmon resonance frequencies, determined experimentally for each sample using UV−vis spectroscopy, red shift with increasing copper content as expected. These experimentally determined plasmon resonance frequencies ...