Labconco Freeze Dryer Standard Operating Procedure Model FreeZone 4.5 Plus version 1.1

Labconco Freeze Dryer Standard Operating Procedure

Model FreeZone 4.5 Plus verson 1.1 

*Approved by Laboratory Manager on 11-30-2019

*Additional information on website: https://www.labconco.com/product/freezone-45-liter-105c-benchtop-freeze-dryer-13/6175

*Obtain training prior to operation from the laboratory manager. 

*Schedule use of the freeze dryer on the laboratory website http://www.uwyo.edu/ecologybgc .

1. Pre-Freezing Samples.

   1. Smaller samples in ampules and serum bottles may be frozen in a freezer. The sample container size should always be at least two to three times the sample size (i.e., 40 ml samples should be prepared in 80 ml containers or larger). The temperature required for pre-freezing is dependent on the characteristics of the sample. Pre-freezing temperatures are typically at least 10 to 20 degrees C below the eutectic or collapse temperature of the sample.

2. Closing the system

   1. Before starting the freeze dryer make sure the plug is tightly inserted into the hose to seal the entire system.  Place lab tape, parafilm, etc. over the plug and hose.

3. Check the vacuum pump oil

   1. Make sure the level is in the indicated range on the front site glass.

4. Automatic Start-Up. (Use this always unless instructed otherwise by Laboratory Manager)

   1. To run the Auto Mode, press the panel switch labeled REFRIGERATION AUTO. The green LED above the switch will illuminate. This will start the refrigeration system. When the collector reaches -40 degrees C, the vacuum pump will start. The Temperature and Vacuum Graphs will indicate collector temperature and system vacuum. The LCD display will show the actual temperature of the collector.  When the vacuum in the system is above 5 mBar the vacuum display will indicate "HI." At 5 mBar and below, the display will show the actual vacuum. When the system vacuum is between 0.450 and 0.133 mBar, the lower green vacuum graph LED will flash. When the system vacuum level is <0.133 mBar, the green LED will be lit steadily indicating that most samples may be added.

   2. Check the system after 15 minutes and if the green lights aren’t moving you have a leak in the system.  Turn the freeze dryer off and start steps 2-4 again.

   3. Make sure to check the system every day to make sure the coil isn’t covered in frost.

5. Manual Start-Up

   1. To manually run the freeze-dry process, press the REFRIGERATION MAN switch. This will start the refrigeration system. The green LED above the switch will illuminate. When the collector temperature reaches -40 C, the vacuum pump may be started by pressing the VACUUM switch. The Temperature and Vacuum Graphs will display the collector temperature and system vacuum. The LCD display will show the actual temperature of the collector. When the vacuum in the system is above 5mBar the vacuum display will indicate ''HI." At 5 mBar and below, the display will show the actual vacuum. When the system vacuum is between 0.450 and 0.133 mBar, the lower green vacuum graph LED will flash. When the system vacuum level is <0.133 mBar, the green LED will be lit steadily indicating that samples may be added.

6. Shutdown

   1. Turn the freeze dryer off and pull the plug out carefully. 

   2. Place a the drain bucket under the hose, this is where the condensation from the coil drains.

7. Setting the Operating Vacuum Level

   1. The vacuum level may be set by the user to optimize the freeze dry process. Normally, the sublimation rate will increase if there is less vacuum (a higher pressure) in the Freeze Dryer. A good starting place is to set the vacuum so its level is equivalent to about 10°C colder than the eutectic or collapse temperature of the sample. Adjustments to the vacuum level must be made for various freeze-drying conditions.

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