Overview of Performed Drying Cycles (Shelf Temperature, Ts; Chamber Pressure, Pc)
| Cycle | Loading | Freezing | Primary Drying | Secondary Drying | |||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Ts (°C)* | hold (min) | Ts (°C)* | ramp (°C/min) | hold (min) | Ts (°C)* | ramp (°C/min) | hold (min) | Pc (Pa)** | Ts (°C)* | ramp (°C/min) | hold (min) | Pc (Pa)** | |
| A | 5 | 60 | –40 | 0.3 | 240 | 0 | 0.2 | 4500 | 10 | 20 | 0.2 | 360 | 10 |
| B | 5 | 60 | –40 | 0.5 | 240 | 0 | 0.2 | 4500 | 10 | 20 | 0.2 | 360 | 10 |
| C | 5 | 60 | –40 | 1.5 | 240 | 0 | 0.2 | 4500 | 10 | 20 | 0.2 | 360 | 10 |
| D*** | 5 | 60 | –40 | 1.5 | 120 | 0 | 0.2 | 4500 | 10 | 20 | 0.2 | 360 | 10 |
| Aggressive | 5 | 60 | –40 | 0.5 | 240 | 10 | 0.2 | 4500 | 5 | 20 | 0.2 | 360 | 5 |
| Gentle | 5 | 60 | –40 | 0.5 | 240 | −20 | 0.2 | 4500 | 5 | 20 | 0.2 | 360 | 5 |
| VIAL (M) | 5 | 60 | –40 | 0.5 | 240 | 10 | 0.2 | 4500 | 20 | 20 | 0.2 | 360 | 20 |
| DCS (E) | 5 | 60 | –40 | 0.5 | 240 | −10 | 0.2 | 4500 | 10 | 20 | 0.2 | 360 | 10 |
| LPC (K) | 5 | 60 | –40 | 0.5 | 240 | −10 | 0.2 | 4500 | 5 | 20 | 0.2 | 360 | 5 |
↵* Shelf temperature
↵** Chamber pressure
↵*** Plus annealing step (after freezing the product down to T= –40 °C, the shelf temperature was ramped to T= –10 °C at a rate of 1 °C/min and held at that temperature for 120 min before ramping back to T= –40 °C at a rate of 1 °C/min and holding for additional 120 min)