The structure of amorphous alloys has been studied by using various techniques, such as x-ray, neutron, and electron diffraction experiments. X-ray diffraction is the most conventional of all the techniques and is based on EXAFS (extended x-ray absorption fine structure) [1-3] and AXS (anomalous x-ray scattering) [4-5] experiments, which are used for the investigation of the local environment around a species of atom. Recently, x-ray diffraction has been applied to the structural analysis of some quasicrystals [5,7]. It is, of course, hard to determine the local structure of a noncrystalline material only from ordinary x-ray diffraction experiments. However, the role of x-ray diffraction in structural analysis is still important from the viewpoint that this supplies a relatively convenient method, and the appropriate selection of a Sample makes it possible to extract the dominant atomic correlation in the material. In the present study, a conventional -2 diffractometer was used with a monochrometor in the diffracted beam. First, the theoretical background is discussed, the data analysis procedure is given in detail, and error estimation in the data analysis is presented last.