Chapter 5: Using Your Freeze Dryer
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THE VACUUM SHOULD ALWAYS BE TURNED OFF WHILE
USING THE SHELVES TO FREEZE SAMPLES
The sample container volume should be at least two to three times greater than the
sample volume. The temperature required for pre-freezing is dependent on the
characteristics of the sample. Pre-freezing temperature is typically at least 10° to
20°C below the eutectic or collapse temperature of the sample. Pre-freezing on the
Triad shelf can be done in Manual or Program modes as long as the shelf set point
temperature is adequate to fully freeze the sample.
In MANUAL mode, simply set the Shelf temperature to the desired value for
freezing the sample, and allow an appropriate amount of time for the sample to be
fully frozen before starting the vacuum and the freeze drying process.
In PROGAM mode, the vacuum set point can be programmed to OFF for the
initial pre-freezing step. If multiple steps are desired for more complex pre-
freezing/annealing processes, then program the vacuum set point to OFF for each
of the pre-freezing / annealing steps.
If desired, place the sample probe in a sample vial to monitor the sample
temperature throughout the pre-freezing & freeze dry process.
Shelf Loading
The stoppering mechanism is capable of generating a very strong force, which
could damage the shelf or mechanism. Therefore, it is important to distribute the
serum bottles to be stoppered evenly across the entire surface of the shelf. When
stoppering vials, always place a vial on each corner of the shelf.
Setting the Operating Vacuum Level
To change the Vacuum Set Point
1. Go to Home screen
2. Press VACUUM,
enter new Vacuum Set Point value
press APPLY (or START if vacuum pump is not already running)
The vacuum level may be set by the user to optimize the freeze dry process.
Normally, the sublimation rate will increase as the pressure increases 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. The reference
table below shows the relationship between ice temperature and vapor pressure.
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