Jul 17, 2024
BAF_S04_LABCONCO freeze dryer
- 1University of Virginia Biomolecular Analysis Facility Core
Protocol Citation: Nicholas Sherman 2024. BAF_S04_LABCONCO freeze dryer . protocols.io https://dx.doi.org/10.17504/protocols.io.261ge5r87g47/v1
License: This is an open access protocol distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited
Protocol status: Working
We use this protocol and it's working
Created: June 13, 2024
Last Modified: July 17, 2024
Protocol Integer ID: 101754
Keywords: Lyophilizer, drying, samples
Abstract
General operation of the Lyophilizer unit.
Guidelines
All samples must be frozen PRIOR to putting in the freeze dryer for the sample to dry correctly
Safety warnings
Alerts: A number of events may occur during a lyophilization procedure that will cause an
alert to be displayed on the Freeze Dryer touch screen. An audible alarm (beeper)
will also be sounded that will automatically be muted after one minute.
The specific alert type can be identified by observing the message box on the
display. The alert message box and audible alarm can be dismissed by pressing the
“Back” button on the alert message box. The following conditions will initiate an
alert.
Power Fail
If a power failure occurs during a Freeze Dry process, the vacuum control valve
will allow air to bleed into the Freeze Dryer System. If the failure is of a short
duration and the collector does not warm up above -30°C, when power is restored
the Freeze Dryer will restart and resume operation of the refrigeration and vacuum
systems. If the power failure lasts for a longer duration and the collector warms
above safe limits, when the power is restored, the Freeze Dryer will not
automatically restart. This prevents melted sample from being drawn into the
collector and prevents liquid from being drawn into the vacuum pump.
When power is restored, the POWER FAIL alert message will be displayed on the
touch screen and the audible alarm will sound.
Line Voltage Range
If the voltage supplied to the Freeze Dryer varies beyond allowable limits, the
LINE VOLTAGE RANGE alert will be activated. The high and low alarm points
are preset at the factory to correspond to the normal allowable voltage variations
based on the nominal voltage specified for the freeze dryer. Some models may be operated outside the normal voltage limits (see Appendix C). If necessary, the high
and low LINE VOLTAGE OFFSETS may be adjusted from the Settings /
Maintenance screen.
Collector Temp
After the collector temperature has cooled to below -40°C, an alert will be
activated if the collector temperature rises above –40°C for more than 5 minutes.
Collector Moisture
If there is liquid in the collector chamber and either the COLLECTOR or
VACUUM start button is pressed, neither function will start and an alert will be
activated. This feature prevents the inadvertent start of the vacuum pump when
liquid is in the collector and thereby can extend the life of the vacuum pump.
A few drops of liquid may remain in the drain hose after draining. When the
vacuum pump is started these drops may be sucked into the collector chamber.
This is normal.
Service Vacuum Pump
The vacuum pump normally plugs into the vacuum pump electrical receptacle on
the back of the Freeze Dryer. When the Freeze Dryer has accumulated a total of
1000 operating hours, an alert will be activated. It may be necessary to service the
vacuum pump more frequently than every 1000 hours depending on the operation
of the Freeze Dryer. The pump oil should be regularly monitored to verify that
it is clean. The “Set hours between oil change” can be reprogrammed from the
Settings / Maintenance screen for any value from 0 to 9999 hours.
Vacuum Leak
If the vacuum level in the freeze dryer has not reached at least 5 mbar within 30
minutes of starting the vacuum, an alert will be activated and the vacuum pump
will be turned off (if it is plugged into the Freeze Dryer vacuum pump outlet).
Vacuum Set Point
If the system is unable to achieve the vacuum set point (during Manual or Program
mode), an alert will be activated. This alert will be activated if the vacuum level is
not within 0.500 mbar of the vacuum set point in 20 minutes.
Before start
THIS CHECKLIST SHOULD BE FOLLOWED PRIOR TO EACH USE:
1. remove the accessory drying chamber or manifold from the collector chamber lid and using a soft, lint free paper towel, wipe the port gasket(s) and sealing surfaces of the drying chamber/manifold and collector chamber lid to remove any dirt or contaminants that could cause a vacuum leak.
2. Ensure that the collector chamber and drain line are free of water. Place the drain hose in a suitable container to collect the condensate from the collector chamber. Insert the quick connect drain fitting into the quick connect drain coupling located on the left hand side of the Freeze Dryer. Note: Freeze Dryer (Collector or Vacuum) will not start if moisture is detected in the drain line.
3. after completely draining the system, disconnect the quick connect drain fitting from the quick connect drain coupling.
4. wipe the interior of the collector chamber with a paper towel to remove any remaining moisture.
5. reinstall the drying chamber or manifold on the collector chamber lid.
6. check that each sample valve is closed or in the VENT position.
7. start COLLECTOR and allow the refrigeration system to reach its specified operating temperature.
- if using auto start up: go to home screen and press AUTO --> START. collector starts immediately, vacuum starts once collector reaches -40°C
- if using manual star up: go to home screen, press COLLECTOR --> START. when collector reaches -40°C, manually press VACUUM --> START
9. attach a pre-frozen sample to sample valve on drying chamber or manifold.
Checklist before starting - from User Manual
Checklist before starting - from User Manual
Remove the accessory drying chamber or manifold from the collector chamber
lid and using a soft, lint-free cloth or paper towel, wipe the port gasket(s) and
sealing surfaces of the drying chamber/manifold and collector chamber lid to
remove any dirt or contaminants that could cause a vacuum leak.
Ensure that the collector chamber and drain line are free of water. Place the
drain hose in a suitable container to collect the condensate from the collector
chamber. Insert the quick connect drain fitting into the quick connect drain
coupling located on the left side of the Freeze Dryer. Note: Freeze
Dryer (Collector or Vacuum) will not start if moisture is detected in the
drain line.
After completely draining the system, disconnect the quick connect drain
fitting from the quick connect drain coupling.
Wipe the interior of the collector chamber with a soft cloth or paper towel to
remove any remaining moisture. Reinstall the drying chamber or manifold on the collector chamber lid. Note: Vacuum grease is NOT required on the drying or collector chamber lid gasket to obtain a proper vacuum seal.
Check that each sample valve is closed or in the “vent” position.
Turn on the lyophilizer
Turn on the lyophilizer
Go to the Home screen, for the auto-start procedure click on AUTO and then press START.
The collector starts cooling down, and once temperature reaches -40 C, the VACCUM pump will start.
Wait until temperature reaches -80 C temperature, and pressure reaches 0.001 mbar.
Depending on sample type these parameters should be adjusted, refer to User Manual.
Add samples
Add samples
MAKE SURE ALL SAMPLES ARE PRE-FROZEN
Connect a pre-frozen sample to a sample valve on the drying chamber or manifold using an adapter. Turn the plastic valve knob to the “VACUUM” position to open the valve, which connects the attached sample to system vacuum. The bevel on the knob should be positioned toward the sample port to apply vacuum to the sample.
Before adding another sample, allow system vacuum to return to 0.133 mbar or
lower. Any combination of valves and sample sizes may be utilized at one
time provided that the system vacuum and collector temperature remain
sufficiently low to prevent melting of the frozen sample.
When all the frost has disappeared from the outer surface of the sample
container and no cold spots can be detected by handling the container, the
sample is nearly dry. To be certain of low final moisture content, dry the
sample for several hours past this point.
To remove a container after drying is complete, turn the plastic knob on the
valve to the “VENT” position, which closes the valve and vents the container.
Should back-filling with an inert gas be required, connect the gas supply line to
the vent port on the valve before turning the plastic knob on the valve to vent
position. The sample container may now be removed. In the vent position the
bevel on the valve knob should point away from the sample port
Ampules may be flame sealed while connected to a valve by using a sealing
torch. Care must be taken not to burn the valve. An insulation material placed
between the valve and the torch is recommended.
Shut down
Shut down
At the end of a run or when a sufficient amount of condensate accumulates on the
collector coil to obstruct the flow of vapor to the collector chamber, the Freeze
Dryer should be defrosted.
Go to Home screen, press VACUUM, then STOP to
turn the vacuum pump OFF. Then release system vacuum by turning the plastic
knob on a valve (that has no sample attached) to the open position or opening the
vent valve on Tray Dryer or Clear Chamber. Press COLLECTOR, then STOP to
turn the refrigeration system OFF.
Defrost the collector coil
Defrost the collector coil
The hot gas defrost function can be used to speed up the defrosting process.
Defrost can be activated as follows: Go to Home screen, press COLLECTOR
button, press Defrost Options, then press START.
To turn off Defrost: Go to Home screen, press DEFROST button, press STOP.
The defrost function will turn off automatically if the collector temperature
reaches +60°C or if defrost has been running for 2 hours.
If rapid defrost is desired, pour warm water over the collector coil. Do not
allow the liquid to enter the vacuum port on the upper rear wall of the chamber.
Place the drain hose in a suitable container to collect the condensate from the
collector chamber. Insert the quick connect drain fitting into the quick connect
drain coupling located on the left hand side of the unit.
Flush the collector chamber with water and wipe chamber dry
Disconnect the quick connect drain fitting from the quick connect drain coupling
Export data log file
Export data log file
Data Log Files can be copied (exported) to a USB flash drive via the USB port on
the left side of the Freeze Dryer. The file will be exported as a “comma separated
values” file (.csv file extension), which can be easily opened with a spreadsheet
application program for data analysis and graphing. To export a file:
Insert USB flash drive into the Freeze Dryer USB port --> Go to Data Logging screen --> Select the file that you want to export by pressing the Data Log File name --> Press the Export button
Protocol references
FreeZone Benchtop Freeze Dryers (7343000 Rev K) - LABCONCO User Manual.