Poly(tetrafluoroethylene) (PTFE) latex particles have been analyzed and sorted according to size using asymmetric flow field flow fractionation (AF4) coupled with multiple-angle light scattering (MALS). Characterization of fractions by regular and depolarized dynamic light scattering confirmed that smaller particles elute prior to larger ones, as expected for field flow fractionation. The measured radii of the optically and geometrically anisotropic particles are consistent with those determined from transmission electron microscopy (TEM). A certain amount of heterogeneity remains in the fractions, but their uniformity for use as diffusion probes is improved. Full characterization of PTFE colloids will require a difficult assessment of the distribution, even within fractions, of the optical anisotropy. A general method to obtain number versus size distributions is presented. This approach is valid even when an online concentration detector is not available or ineffective. The procedure is adaptable to particles of almost any regular shape.