Diffraction anomalous fine structure (DAFS) is the fine structure in the intensity of an X-ray diffraction peak in the vicinity of an absorption edge. DAFS is measured by monitoring the intensity of a diffraction peak as a function of the incident X-ray energy as it is scanned through an absorption edge. It combines the short range structural sensitivity of X-ray absorption spectroscopy with the long range periodicity of X-ray diffraction and can provide structural information which is not available from these techniques alone or in combination. We demonstrate the technique for several different dilute, polycrystalline samples, and present an iterative data analysis method which allows the extraction of a specific X-ray absorbance spectrum from the DAFS spectrum