A series of FePt nanoparticles was synthesized by the thermal decomposition of iron pentacarbonyl and reduction in platinum acetylacetonate in phenyl ether solvent. A range of precursor molar ratios of 2, 1.5, and 1 between iron pentacarbonyl and platinum acetylacetonate was studied. After 30 min of reflux, the synthesis method produced a wide distribution in composition and size for the nanoparticles. Given 200 min of reflux, it was observed that the particle-to-particle composition and size narrowed, and the atomic ratio of Fe to Pt, for the majority of nanoparticles, approached the initial precursor molar ratios except for the molar ratio of 1. It is speculated that the compositional variability may be a result of the slow kinetics of iron pentacarbonyl’s decomposition in the reaction.