Electroplating is a key technology in the LIGA process (German acronym for Lithographie (Lithography), Galvano (Electroplating) and Abformung (Moulding)). The electroplating process determines the physical, chemical, and mechanical properties of a device. In the macro environment, the process is empirically understood arid electroplating results are fairly well predictable. For use in the micro environment, in particular in microfabrication of LIGA components with high-aspect-ratios, effects like delamination from the substrate, inhomogeneous material distribution, pores in the material and large grain sizes have to be avoided. It is, therefore, important to investigate the structure and composition of such materials. Various electroplated Permalloy foils have been prepared, which are of interest because of their soft magnetic behaviour and use as materials for microsensors and microactuators. X-ray absorption fine structure (XAFS) and x-ray absorption near edge structure (XANES) have been recorded at the Nickel and Iron K-edges (8333 and 7112 eV respectively) for electroplated Permalloy.