Abstract. Annealed iron-platinum (FePt) is ferromagnetic in a nanoscale regime which is necessary for energy and data storage, whereas the as-synthesized form of FePt-based nanoparticles exhibits superparamagnetism useful for biomedical applications. In this study, as-synthesized nanosuspensions from the reaction of Pt(acac) 2 with Fe(acac) 3 and Fe(hfac) 3 are compared. X-ray diffraction (XRD) peaks for both samples are assigned to the FePt 3 phase. As shown by transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS), nanoparticles synthesized by using Fe(acac) 3 have a smaller average diameter, but larger polydispersity index and particle agglomerations. On the other hand, the nanoparticles synthesized by using Fe(hfac) 3 can self-assemble into a longer range of patterned monolayer. Dynamic light scattering (DLS), measuring the size of cluster of nanoparticles as well as oleic acid and oleylamine at their surface, confirms that larger agglomerations in the sample were synthesized by using Fe(acac) 3 . In addition to the size distribution, magnetic properties were influenced by the composition of these nanoparticles. Another non-destructive technique to determine the size distribution is small angle X-ray scattering (SAXS) [12]. Its advantages are the accurate determination of nanoparticle size distributions and the discrimination between polydisperse single particle and polydisperse particle in aggregates. SAXS has been successfully used to complement TEM in probing the size distribution of several nanoparticles including Au [13], CoPt 3 [14] and FePt [15]. Furthermore, Fe 3 O 4 and CuO nanoparticles were comparatively characterized using X-ray diffractometry (XRD), TEM, DLS and SAXS [16].In this study, the morphology of FePt-based nanoparticles synthesized from two alternative precursors is compared by using TEM, DLS and SAXS. Iron(III) acetylacetonate (Fe(acac) 3 ) and iron(III) hexafluoroacetylacetone (Fe(hfac) 3 ) have been investigated as a replacement for highly toxic Fe(CO) 5 . The synthetic procedure, adapted from the published method [17], replaces a N 2 glove box with an Ar Schlenk line. The heating rate in the terminal process and revolution of purified centrifugation are also reduced.