In general, no more than 1 g of metal sulfide can be completely digested in 20 mL of inverse aqua regia using the Carius tube technique. In this study, the sample weight increased after adding HClO4 to inverse aqua regia while the volume of acid concurrently decreased significantly. Three grams of metal sulfide were digested in 12 mL of acid (3 mL of HClO4 and 9 mL of inverse aqua regia) via the HClO4-inverse aqua regia method. The results using molybdenite reference materials JDC and HLP mixed with 3 g of pyrite were consistent with certified values. Compared to the traditional method, the HClO4-inverse aqua regia method could dissolve a larger sample mass (3 g) with a smaller volume of acids (12 mL). We simultaneously found that the oxidation of digestion acids greatly affected the Os signal but had no influence on the equilibrium of isotope exchange between 185Re and 190Os spikes in Re and Os samples. Remarkably, the heating temperature was the most significant factor influencing the equilibrium of isotope exchange, and the Os in a sample was not equilibrated with the spike until the heating temperature reached 190 °C
