Abstract : Chemically and magnetically homogenous samples of amorphous iron-boron alloys over a wide concentration range have been fabricated and examined for their atomic and magnetic structures. The knowledge of homogeneity is important in obtaining controllable materials for defice applications, and the determination of atomic structure, distribution of magnetic oments and isomer shift is essential to the knowledge of chemical short-range order and the direction and amount of charge transfer. The details of these measurements along with their interpretation and formulation of theoretical models are described.