Abstract: Different sample digestion systems for Re-Os dating of black shale were studied. The sample digestion effect of aqua regia Carius tube digestion system and CrO3-H2SO4Carius tube digestion system at different digestion temperature were compared. The results from the study show that the CrO3-H2SO4. Carius tube digestion system provides the lower total procedure blank value for rhenium (less than 10 pg) than aqua regia system. Combined with high sensitive inductively coupled plasma-mass spectrometric (ICP-MS) analytical technique, a new CrO3-H2SO4Carius tube digestion-ICPMS determination system for Re-Os dating of black shale has been established.