Magnetization measurements, transmission electron microscopy (TEM), and high-resolution micro-x-ray fluorescence (μ-XRF) using a synchrotron radiation source (Advanced Photon Source) were used to examine Fe3O4 particle agglomerates of nominally 10-nm particles at low concentrations (down to 0.03%) in thick epoxy resin samples. The magnetization measurements showed that at low concentrations (<0.5%) the magnetite particles, although closely packed in the agglomerates, did not interact magnetically. Predicated on a 2-μm sample step scan, the μ-XRF results were compatible with the presence of spherical agglomerates due to magnetostatic attraction, and these ranged in size from 100 to several thousand nanometers, as observed in TEM measurements. At smaller step scans the resolution could be significantly improved. Thus, the synchroton μ-XRF method was very useful in detecting very small concentrations of particles in thick samples and could probably be used to detect particles in amounts as low as 10−16 g.