Pre-Freezing Samples - Labconco FreeZone 70020 Series User Manual

Chapter 5: Using Your Freeze Dryer
Temp. Pressure Temp.
(°C) (mbar) (°C)
0 6.11 -11
-1 5.63 -12
-2 5.18 -13
-3 4.76 -14
-4 4.37 -15
-5 4.02 -16
-6 3.69 -17
-7 3.38 -18
-8 3.10 -19
-9 2.84 -20
Adjustments to the vacuum level must be made for various freeze drying
conditions. Factors that must be considered are whether the sample is freeze dried
on heated shelves or in glassware attached to manifold valves, the volatility of the
sample itself, the size of the sample and the heat energy supplied to the sample.
Some guidelines for setting the vacuum level are shown below. Exact protocols
must be determined by the user for the specific samples that are being freeze dried.
Material
Bacteria, Virus
Milk
Fungi
Vegetable Tissue
Human Tissue
Blood Plasma
Vaccine
When the vacuum control is set to operate at less vacuum (higher pressure), the ice
holding capacity of the collector may be decreased. This can be improved by
installing a baffle in the collector chamber. See Appendix A Freeze Dry
Components for the baffle part number. See Chapter 3: Baffle Installation for
proper positioning of the baffle in the collector chamber.

Pre-Freezing Samples

Appropriate containers for freeze drying include ampules, serum bottles, and wide
mouth freeze drying flasks. Shell freezing of samples is recommended for wide
mouth freeze drying flasks. Smaller samples in ampules and serum bottles may be
frozen in a freezer or in the center of the collector chamber. 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-
38
Vapor pressure above ice
Pressure Temp. Pressure
(mbar) (°C) (mbar)
2.37 -21 0.94
2.17 -22 0.85
1.98 -23 0.77
1.81 -24 0.70
1.65 -25 0.63
1.50 -26 0.57
1.37 -27 0.52
1.25 -28 0.47
1.13 -29 0.42
1.03 -30 0.38
Solidification/Eutectic
Temperature Temperatures
≤ -40°C
-5 to -13
≤ -40
-25 to -50
-30 to -40
-10 to -25
-30 to -40
Product Service 816-333-8811 or 1-800-522-7658
Temp. Pressure Temp.
(°C) (mbar)
-31 0.34
-32 0.31
-33 0.28
-34 0.25
-35 0.22
-36 0.20
-37 0.18
-38 0.16
-39 0.14
-40 0.13
Pre-Freeze
Vacuum Set Point
≤ -50°C ≤ 0.04 mbar
-15 to -23 1.65 to 0.77
≤ -50 ≤ 0.04
-35 to -60 0.22 to 0.01
-40 to -50 0.12 to 0.04
-20 to -35 1.03 to 0.22
-40 to -50 0.12 to 0.04
Original instructions
Pressure
(°C) (mbar)
-50 0.039
-60 0.011
-70 0.003
-80 0.001