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X-ray diffraction and absorption spectroscopy measurements have been performed in metastable solid materials obtained by mechanical attrition or codeposition process of immiscible systems in view to investigate the short and long range order obtained inside these solutions. Firstly, experiments show that CuBoFeloColo milled powders are in quasi perfect solid solution ; this result arouses interest because giant magnetoresistance is more readily controlled by decomposition of a supersatured solid solution. Secondly, codeposition of CuSOMoSO presents a long range order typical of a well-defined cristalline structure whereas the short range order appears very disordered.