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The introduction of microwave (MW) heating devices inthe “chemical laboratory” represents one of the most important andrelevant application that contributes to speed up the “samplepreparation” step and, therefore, dramatically reduces the timeneeded for the analytical response. On the other hand, few andgeneric are the criteria developed to compare analytical dataobtained with conventional sample preparation approach withrespect to the MW one. In fact, when reference materials, RMs, arenot available, or not sufficiently representative of the real matrixunder investigation, it is often difficult to know when the sampledisgregation has come to completeness or if it is still possible tosave more time on the MW heating process. This contribute willdeal with the use of the more innovative Design of Experimentstools to the MW assisted digestion of organic rich matrices focusing on the potentialities of these experimental approaches when developing new disgregation analytical methods. The experimental approach concerns in finding the “optimum process conditions” in terms of solvent reaction mixture and recovery metal content.