The demand of the modern times for minimalization has actualized the advance of new materials with extremely fine microstructures. Accordingly, the FINEMETs, NANOPERMs, HITPERMs and some aluminium based heat-treated ribbons symbolize the particular category of the nanocrystalline alloys in which the development of the three-dimensional nanostructure can be controlled by a special thermal treatment of rapidly quenched precursors. In this work, we developed an optimized procedure for rapid digestion of NANOPERM samples by acid attack in an oven under microwave irradiation. Experimental design was used as a multivariate strategy for variable effects evaluation using metal ion concentrations as response variable