The utility model discloses a chemistry technical field's a multilayer separates oxygen protection pyroreaction sample device, including the one -level crucible, the inner chamber of one -level crucible is equipped with the second grade crucible, lay tertiary crucible in the second grade crucible, it has the active carbon bisque all to fill between one -level crucible and the second grade crucibleand in the cavity that forms between second grade crucible and the tertiary crucible, the one -level crucible is fixed with the apron that is located its top through the external bolt of fixed orifices, and this device adopts three group's crucibles to be used for depositing the sample, and just three group's crucibles all adopt the stainless steel shaping, utilize its high temperature resistanceperformance, do benefit to high temperature and separate the oxygen protection to packing the active carbon bisque in the cavity that forms between adjacent two sets of crucibles, doing benefit to the isolated oxygen of the sample in the crucible, this device design is equitable, novel structure, and it is effectual to separate oxygen.