Table 2.
Stage | Modes |
---|---|
1 | Pre-cooling, pre-freeze temperature: 5°C |
2 |
Freeze mode Temperature: − 50°C, ramp duration: 120 min, soak duration: 420 min |
3 |
Condenser mode/vacuum mode Condenser cooling: − 55°C, vacuum start value: 75 mTorr |
4 |
Heating mode (primary dry) Step 1. Temperature: − 10°C, ramp duration: 120 min, soak duration: 1120 min, vacuum: 75 mTorr Step 2. Temperature: 10°C, ramp duration: 180 min, soak duration: 1200 min, vacuum: 75 mTorr |
5 |
Secondary dry Temperature: 25°C, ramp duration: 120 min, soak duration: 600 min, vacuum: 15 mTorr |
6 |
Stoppering Injection N2 gas (> 99.999%) at vacuum break time, stoppering on − 0.4 Bar |