Table 3.
Step | Reactants | Time | Temp. |
---|---|---|---|
Step 1 | 50 mL 30% CH3COOH + 50 mL H2O | 1 day | 20 °C |
Step 2 | 25 mL 16 M HNO3 + 50 mL H2O | 5 days | 20°C |
Step 3 | 30 mL 12 M HCl + 35 mL H2O | 1 day | 75°C |
Step 4 | 30 mL 30 M HF + 15 mL 12 M HCl + 15 mL H2O | 1 day | 75°C |
Step 5 | 10 mL 30 M HF + 10 mL 12 M HCl | 3 days | 150°C |
Step 6 | 2 mL 16 M HNO3 + 2 mL 30 M HF | 15 hours | 120°C |
Step 6 is applied to a fraction of Step 5 residue)