Porous carbons have received much attention recently for potential applications in energy generation and storage, molecular sieving, and environmental remediation. Property optimization for specific applications rests largely on controlling the volume, size, and shape of the pores at the synthetic level. Direct atom-scale experiments which might accurately and reliably measure these quantities are problematic, so indirect methods such as gas sorption are generally employed. Here we apply a second indirect method, small-angle X-ray scattering (SAXS), to study porosity in carbide-derived carbons (CDC). The results qualitatively confirm and reinforce model-dependent conclusions drawn from gas sorption isotherms. In particular, both techniques indicate the onset of broad polydispersity under the same processing conditions for particular porous carbon materials.