The invention provides a black shale Carius
pipe complete sample dissolving method which comprises the following steps: weighing a black shale sample, adding the black shale sample into a sample dissolving tank, adding HF into the sample dissolving tank, and standing to dissolve the sample to obtain a pre-dissolved solution; the pre-dissolved solution is heated, HCl is added for acid removal when the pre-dissolved solution is heated to be nearly dry, and acid removal is repeated for multiple times so that HF can be removed; adding HCl into the pre-dissolved solution after acid removal, completely transferring the pre-dissolved solution into a Carius tube, adding a mixed
diluent and a sample dissolving
reagent into the Carius tube, and carrying out Carius tube sealing and complete sample dissolving to obtain a sample dissolving solution; separating Re and Os in the sample dissolving solution by adopting a direct
distillation method; and enriching and purifying Re in the
distillation residual solution and Os in the
distillation absorption liquid to respectively obtain a to-be-measured Re sample and an Os sample. According to the method, it is guaranteed that Re and Os are almost not lost, and meanwhile complete sample dissolving of
organic matter-rich
sedimentary rock samples such as black shale is effectively achieved.