X-ray absorption spectroscopy (XAS) has been revealed to be a potential tool for determining the electronic and geometrical structure of transition metal compounds. The position and shape of X-ray absorption discontinuities have been used to deduce structural and chemical bonding information on the compounds. This book, therefore, provides X-ray K absorption spectroscopic study which is a very strong informative experimental approach to study the coordination geometry and bonding relation in metal compounds. The X-ray absorption measurements were performed at the BL-8 DEXAFS beamline at INDUS-2 Synchrotron Source at RRCAT, India at copper and cobalt K-edge for measuring the absorption spectra of copper (II) and cobalt (II) compounds respectively. A simple and innovative procedure for analysis of EXAFS data has been presented employing computer software Mathcad. This book gives details regarding experiment and analysis of the XAFS data, so that any one who wants to do research work in the field of XAFS, may get necessary information at one place. Also a simplified method using Mathcad software has been presented as a learning tool for the new researchers. Enjoy reading!