Ultra-small-angle X-ray scattering (USAXS) is employed to quantify the average size, interparticle spacing, and volume fraction of the primary B2 precipitates in Fe-based superalloys with varying Al concentration. The results are analyzed with a model incorporating polydispersity and interference effects and verified by transmission electron microscopy (TEM) characterizations. As the Al amount increases from 4 to 10 mass pct, there is an approximately 40 pct decrease in the average interparticle spacing and ~30 pct reduction in the average particle diameter.