Lyophilizer — Standard Operating Procedure

1. Pre-Operation Checks

• [ ] Verify condenser temperature reaches −80 °C
• [ ] Check vacuum pump oil level and condition
• [ ] Confirm shelf cleanliness
• [ ] Verify temperature probe calibration
• [ ] Check drain valve is closed
• [ ] Review cycle parameters in batch record

2. Loading Procedure

1. Pre-cool shelves to 4 °C or specified loading temperature
2. Load trays or vials containing peptide solution
3. Insert temperature probes in representative samples
4. Close chamber door and verify seal integrity

3. Freeze-Drying Cycle

Stage	Temperature	Ramp Rate	Hold Time	Vacuum
Freezing	−40 °C	1.0 °C/min	2 – 4 h	Atmospheric
Primary Drying	−10 °C	0.5 °C/min	12 – 36 h	0.05 – 0.1 mbar
Secondary Drying	+25 °C	0.3 °C/min	4 – 8 h	<0.02 mbar

4. Termination Criteria

• Product temperature within 2 °C of shelf temperature
• Vacuum level stable for ≥1 h
• Pressure rise test (<0.01 mbar/min)
• Residual moisture target: ≤1.0% (by Karl Fischer)

5. Unloading Procedure

1. Backfill chamber with dry N₂ to atmospheric pressure
2. Open vent valve slowly
3. Remove product trays
4. Immediately transfer to sealed containers with desiccant
5. Document batch yield and appearance

6. Cleaning and Maintenance

Frequency	Activity
After each cycle	Wipe shelves with 70% IPA
Weekly	Condenser drain and defrost
Monthly	Vacuum pump oil check and filter inspection
Quarterly	Temperature probe calibration
Annually	Full PM including seal replacement and pump overhaul