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We have developed a method to determine the Pore Size Distribution (PSD) of porous low-k dielectric materials. The method is based on a modified version of Small Angle X-ray Scattering (SAXS). We fix the incident Xray angle such that it is a larger angle than the total reflection critical angle for the low-k dielectric material, and a smaller angle than the critical angle for the substrate material. The scattered X-rays are then collected using a two dimensional position sensitive X-ray detector. Measurements were collected on a set of porous SiLK ™ , organic, low-k dielectric, films. The results are compared with Transmission SAXS (T-SAXS) measurements collected using Synchrotron Radiation (SR) as the X-ray source.