FreeZone Benchtop Freeze Dryers (7343000 Rev E)
FreeZone Benchtop Freeze Dryers (7343000 Rev E)
FreeZone Benchtop Freeze Dryers (7343000 Rev E)
Models
70020**** 2.5L -50°C Series
71020**** 2.5L -84°C Series
70040**** 4.5L -50°C Series
71040**** 4.5L -84°C Series
72040**** 4.5L -105°C Series
70080**** 8L -50°C Series
Original instructions
Copyright © 2018 Labconco Corporation. The information contained in this manual and the accompanying
products are copyrighted and all rights reserved by Labconco Corporation. Labconco Corporation reserves
the right to make periodic design changes without obligation to notify any person or entity of such change.
Warranty
Labconco Corporation provides a warranty to the original buyer for the repair or replacement of parts and
reasonable labor as a result of normal and proper use of the equipment with compatible chemicals. Broken
glassware and maintenance items, such as filters, gaskets, light bulbs, finishes and lubrication are not
warranted. Excluded from warranty are products with improper installation, erratic electrical or utility supply,
unauthorized repair and products used with incompatible chemicals.
The warranty for FreeZone® Freeze Dry Systems will expire one year from date of installation or two years
from date of shipment from Labconco, whichever is sooner. Warranty is non-transferable and only applies to
the owner (organization) of record.
Buyer is exclusively responsible for the set-up, installation, verification, decontamination or calibration of
equipment. This limited warranty covers parts and labor, but not transportation and insurance charges. If the
failure is determined to be covered under this warranty, the dealer or Labconco Corporation will authorize
repair or replacement of all defective parts to restore the unit to operation. Repairs may be completed by 3 rd
party service agents approved by Labconco Corporation. Labconco Corporation reserves the rights to limit this
warranty based on a service agent’s travel, working hours, the site’s entry restrictions and unobstructed access
to serviceable components of the product.
Under no circumstances shall Labconco Corporation be liable for indirect, consequential, or special damages
of any kind. This warranty is exclusive and in lieu of all other warranties whether oral, or implied.
TABLE OF CONTENTS
CHAPTER 1: INTRODUCTION 1
Intended Use 1
Freeze Dry Process 1
Freeze Dry Rates 2
Freeze Dry Capacity 3
Samples Containing Volatile Substances 4
About This Manual 4
Typographical Conventions 5
CHAPTER 2: PREREQUISITES 6
Electrical Requirements 6
Location Requirements 7
Vacuum Pump Requirements 7
Chamber or Manifold Requirements 7
Settings Screen 24
Language 24
Time & Date 25
Units 25
Security 25
Alerts 25
Configure Email Settings 26
Maintenance 28
Vacuum Pump Settings 28
Refrigeration System Settings 28
Freeze Dryer Line Voltage Offset 28
Vacuum Pump Protection 28
Calibration 29
Display 30
Network 30
Sensors Screen 31
Drying Accessory Screen 32
End Point Detection Screen 33
Help Screen 34
Diagnostics 34
User’s Manual 34
About 34
Program Complete 42
Copy (export) a Data Log File 42
Download a Data Log File via Ethernet 42
Copy a Program 43
CHAPTER 7: TROUBLESHOOTING 46
Vacuum Pump 46
Gaskets, Tubing, Connections, Sample Valves 47
System Components & Collector Chamber Isolation 49
Refrigeration Module Operation 51
CHAPTER 1
INTRODUCTION
Congratulations on your purchase of a Labconco FreeZone® Freeze Dry System,
which is designed for laboratory lyophilization procedures. The refrigerant used in
the refrigeration system is HCFC-free so it will not endanger the environment.
The unit is easy to install and maintain. Proper care and maintenance of this
product will result in many years of dependable service.
Intended Use
The Labconco Freeze Dryers described in this manual are intended for laboratory
use to facilitate the lyophilization process.
Freeze drying is a process whereby water or other solvent is removed from frozen
material by converting the frozen water directly into vapor without the
intermediate formation of liquid water. The basis for this sublimation process
involves the absorption of heat by the frozen sample in order to vaporize the ice;
the use of a vacuum pump to enhance the removal of water vapor from the surface
of the sample; the transfer of water vapor to a collector; and the removal of heat by
the collector in order to condense the water vapor. In essence, the freeze dry
process is a balance between the heat absorbed by the sample to vaporize the
ice and the heat removed from the collector to convert the water vapor into ice.
Up to the point of overloading the system, the greater the surface area of the
sample, the faster the rate of freeze drying. By contrast, for a given surface area,
the thicker the sample the slower the rate of freeze drying. This is based on the
fact that the heat of sublimation is usually absorbed on one side of the frozen
sample and must travel through the frozen layer to vaporize water at the other
surface. In addition, as the sample is freeze dried, the water vapor must travel
through the layer of dried material. The thicker the sample, the greater the chance
that the dried layer may collapse which would cause an additional decrease in the
rate of freeze drying.
The surface area and thickness of the sample can usually be ignored when each
sample contains only a few milliliters. However, for larger volumes, the samples
should be shell frozen to maximize the surface area and minimize the thickness of
the sample. The volume of the freeze dry flask should be two to three times the
volume of the sample.
In order for lyophilization to occur, ice must be removed from the frozen sample
via sublimation. This is accomplished by the collector and the vacuum pump. The
collector, which should be at least 15 to 20°C colder than the eutectic temperature
(melting temperature) of the sample, traps vapor as ice. Since the vapor pressure
at the collector is lower than that of the sample, the flow of water vapor is from the
sample to the collector. Since this vapor diffusion process occurs very slowly
under normal atmospheric conditions, a good vacuum is essential to maintain an
The rate of freeze drying is directly proportional to the vapor pressure and the
vapor pressure is dependent upon both eutectic temperature and solute
concentration of the sample. For example, a solution of sodium chloride and water
would freeze dry at a slower rate than pure water. The eutectic temperature of a
sodium chloride solution is about –21°C and at this temperature the vapor pressure
is about 1/16 that of water at 0°C. Although the eutectic temperature is not
dependent upon the concentration of sodium chloride, the vapor pressure of the
water would decrease as the concentration of sodium chloride increased. This is
due to the fact that as the solute concentration increases, less of the surface area of
the frozen sample is occupied by water. In general, most solutions or biological
samples will have a eutectic temperature of –10 to –25°C. However, if the sample
contains a simple sugar such as glucose or if the sample is animal or plant tissue,
the eutectic temperature may be as low as –30° to –50°C.
If there is a problem with a particular type of sample melting when placed on the
freeze dry system, dilution of the sample with more water or providing some
insulation around the flask to decrease the rate of heat absorption by the sample
may help. If the eutectic temperature of the sample is –40 to –60°C, the freeze dry
system selected for use must be equipped with cascade type refrigeration so that
the collector temperature can be cooled to below –75°C, or a dry ice/solvent trap
may be used between the collector and the vacuum pump.
Chapter 2: Prerequisites explains what you need to do to prepare your site before
you install your Freeze Dryer. Electrical requirements are discussed.
Chapter 3: Getting Started contains the information you need to properly unpack,
inspect and install your Freeze Dryer.
Chapter 4: Lyo-Works Operating System describes the display screens and user
interface software that controls the Freeze Dryer.
Chapter 5: Using Your Freeze Dryer discusses the basic operation of your Freeze
Dryer. Information on how to attach samples and run the Freeze Dryer is included.
Typographical Conventions
Recognizing the following typographical conventions will help you understand and
use this manual:
Book, chapter, and section titles are shown in italic type (e.g., Chapter 3:
Getting Started).
Steps required to perform a task are presented in a numbered format.
Comments located in the margins provide suggestions, reminders, and
references.
Critical information is presented in boldface type in paragraphs that are
! preceded by the exclamation icon. Failure to comply with the information
following an exclamation icon may result in injury to the user or permanent
damage to your Freeze Dryer.
Important information is presented in capitalized type in paragraphs that are
preceded by the pointer icon. It is imperative that the information contained in
these paragraphs be thoroughly read and understood by the user.
CHAPTER 2
PREREQUISITES
Before you install your Freeze Dryer, you need to prepare your site for installation.
Carefully examine the location where you intend to install your Freeze Dryer. You
must be certain that the area is level and of solid construction. An electrical source
must be located near the installation site.
Electrical Requirements
115V models
o 20 Amp dedicated single phase circuit.
US
o Properly grounded receptacle for NEMA 5-20P
NEMA 5-20P plug.
230V models
o 15 Amp dedicated single phase circuit.
o Properly grounded receptacle that matches the plug supplied with
the unit, (230V models are supplied with one of the following
plugs):
US EU China UK India
(NEMA 6-15P)
o If the plug does not match the available receptacle, remove the plug
and replace it with an approved plug of the suitable style.
!
Do not use any detachable power cord that is not adequately
rated for the unit.
!
Frequency must agree with the serial tag rating.
Improper frequency will damage the compressor.
ADDITIONAL APPLIANCES ON THE SAME CIRCUIT MAY
CAUSE THE CURRENT TO EXCEED THE RATING OF THE
CIRCUIT BREAKER OR FUSE.
Location Requirements
The Freeze Dryer should be located in an area that provides an unobstructed flow
of air around the cabinet. This air cools the refrigeration system. The refrigeration
system draws air through the rear panel and exhausts it through the sides. A
minimum of 3" must be allowed between the back and both sides of the Freeze
Dryer and adjacent wall surfaces. Restriction of airflow during operation could
adversely affect performance.
Vacuum pumps used with 115V models should be equipped with a 115V, 15 Amp
NEMA 5-15P plug. Vacuum pumps used with 230V models should be equipped
with a reverse IEC plug (included with 230V pumps purchased from Labconco).
This will allow the vacuum pump to be plugged into the receptacle on the back
panel of the freeze dryer.
CHAPTER 3
GETTING STARTED
Now that the site for your Freeze Dryer is properly prepared, you are ready to
unpack, inspect, install and test your Freeze Dryer. Read this chapter to learn how
to:
DO NOT RETURN GOODS WITHOUT THE PRIOR
filed with the
AUTHORIZATION OF LABCONCO. UNAUTHORIZED delivery carrier
RETURNS WILL NOT BE ACCEPTED. within fifteen
(15) days of
delivery.
DO NOT DISCARD THE CARTON OR PACKING MATERIAL
FOR YOUR FREEZE DRYER UNTIL YOU HAVE CHECKED
ALL OF THE COMPONENTS AND INSTALLED AND TESTED
THE FREEZE DRYER.
If you did not receive one or more of the components listed for your Freeze Dryer,
or if any of the components are damaged, contact Labconco Corporation
immediately for further instructions.
Component Identification
USB Port
Touch Screen Display
Quick-Connect
drain coupling
Quick-Connect
drain fitting
Vacuum Connection
Ethernet Port
Drying Accessory
Serial Tag
(& Electrical Rating)
End Point Detection
Vacuum Pump
Outlet
Power Inlet
Circuit Breaker
Reset
! Make certain that the oil in the vacuum pump is at the proper
level.
Electrical Connection
Make sure that the outlet that you intend to use meets the voltage and amperage
requirements listed on the serial tag of the Freeze Dryer. Plug the power cord into
the receptacle on the back of the Freeze Dryer and plug the other end into a
suitable power outlet. It will take approximately 90 seconds for the operating
system to fully load.
Baffle Installation
A cylindrical plastic baffle is shipped with -84C & -105C Freeze Dryers (Models
71020xxxx, 71040xxxx & 72040xxxx). The baffle is designed to evenly distribute
collected ice over the entire collector coil. Proper positioning of the baffle is
required to achieve maximum ice loading capabilities.
The baffle installs into the collector chamber with the flat flange upward. The
arrow should point toward the front of the Freeze Dryer (as shown below).
LATCH
SPACER(SSTL)
DRYING CHAMBER
GASKET
GASKET SPACER(PLASTIC)
ACRYLIC
LID ASSEMBLY COLLAR STAINLESS STEEL
LID ASSEMBLY
GASKET LIP
FACING DOWN
MANIFOLD
ACRYLIC LID GASKET
ASSEMBLY
SPACER(PLASTIC)
SPACER(SSTL)
LATCH
GASKET LIP
FACING DOWN
Clear Drying chambers come with their own bottom adapter plate that will be used
in place of the collector chamber lid supplied with the Freeze Dryer.
CLEAR CHAMBER
major components of the FreeZone Freeze Dry System that are susceptible to
degradation are as follows:
Carbon Tetrochloride
Sodium Phosphate
Calcium Chloride
Acetic Acid 20%
Cyclohexane
Acetonittirle
Formic Acid
Pyridine
Dioxane
Acetone
Component Material
Valve Stem Acetal C D D D D
Collector Acrylic D D D D
Lid
Hoses, Neoprene C D D C C D D D C D
Gaskets &
Valve
Bodies
Flask Top Silicon C D D D D D C D
Rubber
Chamber & Stainless C
Fittings Steel
When using compounds in the Freeze Dryer that are hostile to the materials of
construction, it is imperative the equipment is thoroughly cleaned after use.
Another way to extend the life of the vacuum pump is to install an optional
secondary trap in the line between the Freeze Dryer and the vacuum pump.
Contact Labconco for ordering information.
With prudent maintenance the FreeZone Freeze Dry System will provide years of
service. Warranty on the affected parts will be voided if maintenance has been
obviously neglected. If you have questions about using specific compounds in the
Freeze Dryer, contact Labconco Technical Service at 1-800-821-5525 or 816-333-
8811 or e-mail: [email protected].
CHAPTER 4
LYO-WORKS™ OPERATING SYSTEM
After your Freeze Dryer has been installed as detailed in Chapter 3: Getting
Started, read this chapter to learn how to:
Control Panel
The control panel for the Freeze Dryer is shown below with a description of its
functions.
Initial Power Up
When the Freeze Dryer is initially plugged into a power source, the On / Standby
LED will begin flashing (1 flash per second). The display will remain OFF for the
first 10 to 15 seconds, then the FreeZone animated graphics will appear. It will
take approximately 90 seconds for the operating system to fully load.
Menu
Indicator Bar
Line 1
Line 2 Operation
Line 3 Buttons
Line 4
Line 5 Time / Date
1. Home
2. Programs
3. Data Logging
4. Settings
5. Sensors
6. Drying Accessory
7. End Point Detection
8. Help
The Following system parameters are displayed in the center portion of the screen:
Line 1
COLLECTOR & VACUUM HEADING – Describes the measurement
that is displayed directly below the text.
Line 2
COLLECTOR MEASUREMENT - Displays the temperature of the
collector coil in °C or °F (as selected in Settings). The value displayed
will be RED if the temperature is:
> -40° C (for -50C models)
> -60° C (for -84C models)
> -75° C (for -105C models)
The value displayed will be GREEN if the temperature is:
≤ -40° C (for -50C models)
≤ -60° C (for -84C models)
≤ -75° C (for -105C models)
Line 3
Vacuum Set Point – Displays the current vacuum set point in mbar, Pa, or
Torr (as selected in Settings) on the right hand side of Line 3.
Line 4
Operation Mode – Indicates the current status of the Freeze Dryer. One of
the following will always be displayed on this line:
Line 5
Data Logging Status – On or Off
Operation Buttons
Operation buttons are displayed across the bottom of the Home screen.
Programs Screen
There are two accessories (Tray Dryer & Heated Product Shelves) that will run
programs when connected to a Benchtop Freeze Dryer. The Programs screen will
allow you to create and store up to 30 programs with up to 16 segments per
program. When no program has been selected the “New” button will be the only
active button along the bottom of the screen. A program can be selected from the
program list by pressing the program name. When a program has been selected,
the program row will be highlighted (blue). With a program selected, the rest of
the buttons along the bottom of the screen will become active (Start, Edit/View,
Copy & Delete).
New – Use this button to add a new program to the program list. The new
program name will be defaulted to a two digit sequential number (starting
with “Program 01”) that will be incremented as new programs are added to
the list (i.e. Program 02, Program 03…). The default name can be edited as
desired in the New or Edit/View screen. Up to 30 programs can be saved.
Start/Stop – Use this button to start or stop a program. The wording on
this button will change from “Start” to “Stop” depending on whether or not
a program is currently running.
When a program is currently in progress, a “running man” icon will appear to the
left side of the program name. If the running program is selected (highlighted), the
“Stop” button will be active, and the “Delete” button will be inactive.
“New” program
When the “New” button is selected, the following screen will be displayed.
Pressing the program name field will allow you to edit the program name.
The Step numbers are listed in numerical order. Shelf Temp., Time, and Vacuum
can be edited by pressing any of these cells. The “Add” button will add a new
Step to the program. Pressing the “remove” button will delete the selected step
from the program. Changes will not be saved until the “Save” button is pressed.
Pressing the “Back” button will return to the Programs screen without saving
changes.
If no data log file has been selected the “New” button will be the only active
button along the bottom of the screen. A data log file can be selected from the list
by pressing the data log file name. When a data log file has been selected, the row
will be highlighted (blue). With a data log file selected, the rest of the buttons
along the bottom of the screen will become active (Data View, Chart, Copy &
Delete). If a data log file is currently running (collecting data), the “running man”
icon will appear to the left of data log file name. If the currently running data log
file is selected (highlighted), the Copy & Delete buttons will be inactive.
New/Stop – Use this button to start a new data log file or to stop a running
data log file. The wording on this button will change from “New” to
“Stop” depending on whether or not a data log file is currently running.
The new data log file name will be defaulted to a three digit sequential
number (starting with “Batch 001”) that will be incremented as new data
log files are added to the list (i.e. Batch 002, Batch 003…). The default
name can be edited as desired in the New or Data View screen.
Data View – Use this button to view the data from a saved data log file in
table format.
Chart – Use this button to view data from a saved data log file in chart
format (1 temperature sensor & 1 vacuum sensor can be graphed at a time).
Temperature and vacuum sensors can be selected from pop-up menus.
Copy – Use this button to copy a selected data log file to a USB flash drive
or computer via the USB port on the left side of the Freeze Dryer.
Delete – Use this button to delete a saved data log file from the list.
Settings Screen
Many of the user preferences may be configured from the Settings menu.
Before operating the freeze dryer you may want to configure some of the available
preferences. There are nine categories in the Settings menu.
Time Zone – Enter the Greenwich Mean Time (GMT) offset value for
your location (integer value between -12 & +12).
NTP server – Enter the “web address” (URL) of the NTP server (of
your choice) that will provide clock synchronization data to the Freeze
Dryer via the Ethernet connection.
Daylight Savings (ON/OFF) – This feature can be used to adjust the
time for areas observing Daylight Savings Time (DST).
3. Units – Select your desired unit of measure for Temperature (°C , °F) and
Vacuum (mbar, Pa, Torr)
4. Security – A four digit security code can be set that will require users to enter
the code to gain access to selected screens. A security code will always be
required to enter the “Security” screen.
THE FACTORY DEFAULT SECURITY CODE IS “1234”
5. Alerts – If a valid network connection has been established (via the Settings /
Network screen) and Email Settings have been properly configured, alerts can
be emailed to selected users, by entering the appropriate email address(es) and
selecting the type of alerts that will be sent to each email address.
The Edit & Delete buttons will be inactive until an email address is selected
from the list. When an email address has been selected, it will be
highlighted (blue).
Add – Use this button to add a new email address to the list.
Edit – Use this button to edit an existing email address.
Delete – Use this button to delete an existing email address.
Device Name – The default name for this field will be “Labconco
Freeze Dryer”. The name can be edited by pressing the name field.
Configure Email Settings – Pressing this button will bring up the
following screen, where the appropriate email settings can be
entered.
If you do not know the proper information to enter into each of the SMTP
fields, consult your IT personnel or email service provider.
After entering the appropriate information in all of the SMTP fields, press
the Save button. The system will check the information entered into each
field to make sure each entry is valid. If one or more invalid entries are
found the following message will appear: EMAIL SETTINGS ERROR –
Error connecting to email server, check your settings.
If all the SMTP fields entered are valid, but the network connection is not
working (or Ethernet cable is not connected) the following message will
appear after pressing the Save button: EMAIL SETTINGS ERROR –
Network connection is not active
Test Email – After the Email Settings and Network Settings have
been correctly entered, pressing this button will send a test email to
the selected email address.
CALIBRATION
Offset: ________
Cancel Calibrate
Calibrate - Pressing this button will save the entered offset value.
Temperature sensor offset values can range from -5 to +5° C.
Vacuum Sensor offset values can range from -0.020 to +0.020
mbar.
8. Display – This screen contains settings for controlling various functions of the
touch screen display.
Brightness Slider – Moving the slider to the right will increase the
brightness level, moving to the left will decrease the brightness level
of the display.
Touch Sounds – With Touch Sounds turned ON, there will be an
audible sound each time the display is touched. Pressing the Touch
Sounds button will toggle between ON & OFF.
Screen Timeout Function – If this function is turned ON, the screen
will go into low power mode (sleep) when no screen touches have
been detected for the allotted set time (Screen Timeout). Pressing the
Screen Timeout Function button will toggle between ON & OFF.
Screen Timeout – This value can be set to 5, 10, 15, 30 min, 1, 2, or 3
hours.
9. Network – If the DHCP Enabled button is turned ON, and an Ethernet cable is
connecting the Freeze Dryer to an active network, then the IP Address, Subnet
Mask, and Default Gateway fields will be populated automatically. If the
DHCP Enabled button is turned OFF, the IP Address, Subnet Mask, and
Sensors Screen
This screen contains a list of all sensors currently installed on the Freeze Dryer and
any attached accessory. The screen can be scrolled up and down if the list is too
long to be viewed on a single page. The Sensors screen is for viewing only (there
are no selectable fields on this screen).
Drying Accessory Sensor Table – The middle section of the screen displays a
list of all the sensors that are available for the connected Drying Accessory.
Sensors that are disconnected will have three dashes (---) for their value.
Drying Accessory Status Box – The status box is located directly below the
sensor table. The text on the left side will indicate the current operation mode
of the Drying Accessory (OFF, Manual, or Program). When in Manual mode,
the word “Manual” and the current Shelf Temp Set Point value will be
displayed in this location. If a program is running the program name, Step #,
and Time Remaining (TR) in the current Step will be displayed in this location.
The right side of the status box will indicate if Data Logging is currently ON or
OFF.
End Point Detection status – Shows the current status for each flask.
The status will be one of the following: ON, OFF or COMPLETE.
Touching the end point detection cell for any given flask will allow you
to turn the end point detection ON/OFF. The End Point Detection
status will display COMPLETE automatically when an End Point
Detection alert is achieved for any given flask.
Offset from Ref. Vacuum – This allows the user to determine the level
of dryness at which the system will declare that the primary drying end
point has been reached. The offset from Ref. Vacuum represents the
difference between the Reference vacuum sensor and the individual
flask sensor. This value can be set from 0.010 to 0.050 mbar (0.010
being the most dry & 0.050 being the least dry).
Help Screen
Diagnostics – This screen will give information about the power supply
to the Freeze Dryer (Voltage, Current & Frequency) and allow the user
to run Manual or Auto Diagnostics on the unit.
About – Displays the catalog number of the Freeze Dryer and the
software versions currently installed.
CHAPTER 5
USING YOUR FREEZE DRYER
Operation Checklist
The following checklist should be followed prior to each use of your Freeze Dryer:
1. 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.
2. Remove baffle (if equipped) and wipe with a soft cloth or paper towel to
remove any remaining moisture.
3. 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.
4. After completely draining the system, disconnect the quick connect drain
fitting from the quick connect drain coupling.
DISCONNECT THE QUICK CONNECT DRAIN FITTING BEFORE
STARTING THE VACUUM PUMP. FAILURE TO REMOVE THE
FITTING WILL RESULT IN A LARGE VACUUM LEAK.
5. Wipe the interior of the collector chamber with a soft cloth or paper towel to
remove any remaining moisture.
6. Reinstall baffle (if equipped) in collector chamber.
7. 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.
8. Check that each sample valve is closed or in the “vent” position.
9. Start COLLECTOR and allow the refrigeration system to reach its specified
operating temperature (-50°C, -84°C, or -105°C depending on model)
10. Start VACUUM when collector temperature is -40°C or colder.
Manual start-up
1. Go to Home screen
2. Press COLLECTOR, then press START
3. When COLLECTOR temperature reaches -40°C (or colder)
Press VACUUM, then press START
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.
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.
Solidification/Eutectic Pre-Freeze
Material Vacuum Set Point
Temperature Temperatures
Bacteria, Virus ≤ -40°C ≤ -50°C ≤ 0.04 mbar
Milk -5 to -13 -15 to -23 1.65 to 0.77
Fungi ≤ -40 ≤ -50 ≤ 0.04
Vegetable Tissue -25 to -50 -35 to -60 0.22 to 0.01
Human Tissue -30 to -40 -40 to -50 0.12 to 0.04
Blood Plasma -10 to -25 -20 to -35 1.03 to 0.22
Vaccine -30 to -40 -40 to -50 0.12 to 0.04
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-
freezing temperature is typically at least 10° to 20°C below the eutectic or collapse
temperature of the sample.
Adding Sample
The following procedure should be followed when using chambers or manifolds
with sample valves in the freeze dry process:
Vent/Backfill Port
Bevel in “vacuum”
position
Adapter
2. 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.
3. 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.
4. 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 backfilling 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.
BEFORE STARTING A PROGRAM YOU SHOULD ALWAYS ENSURE
THAT THE COLLECTOR IS “ON” AND HAS COOLED TO -40°C OR
BELOW.
1. Go to the Programs screen. You can access the Programs screen in two
different ways, both lead to the same location.
a. Directly access the Programs screen by selecting the Programs icon
from the main menu bar at the top of the display.
b. Go to the Drying Accessory screen, then select the PROGRAM
button at the bottom of the screen.
2. Select a program from the saved programs list, or create a new program.
3. With the desired program selected from the list, press the START button.
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.
Defrosting
The following procedure should be followed when defrosting the collector coil:
1. 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.
2. 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.
3. 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.
4. 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.
5. Flush the collector chamber with water and wipe chamber dry.
6. Disconnect the quick connect drain fitting from the quick connect drain
coupling.
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.
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.
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).
1. Insert USB flash drive into the Freeze Dryer USB port
2. Go to Data Logging screen
3. Select the file that you want to copy by pressing the Data Log File name
4. Press the Copy button
3. Write down the “IP Address” shown on the Settings>Network screen of the
Freeze Dryer (this number will be used in Step 5)
4. Open an internet browser of your choice from a computer that is connected
to your LAN.
5. Type the following into the address bar at the top of the browser screen:
http://“IP Address”:8080 where “IP Address” represents the number
written down from the Settings>Network screen in Step 3 (example =
http://10.10.9.117:8080).
6. The following webpage will appear with a list of all the Data Log files that
are stored on the Freeze Dryer.
7. Single click on a file name from the list to download the file.
8. Single click on the downloaded file to open the file in Excel.
Copy a Program
If you wish to duplicate a program or quickly create a program that is similar to an
existing program, you can use the copy program function. The new program file
created by the copy function will be stored on the Freeze Dryer (programs cannot
be copied to a USB flash drive or computer). To copy a program:
1. Go to Programs screen
2. Select a program from the list by pressing the program name
3. Press the COPY button
4. Edit program name if desired (the default program name will be “copy of
program name”)
CHAPTER 6
MAINTAINING YOUR FREEZE
DRYER
Service Safety Precautions
Always ensure that only authorized technicians service the refrigeration,
vacuum and electrical systems.
If performing any electrical maintenance, always disconnect the power at
!
the main disconnect.
If the refrigeration system must be operated with access panels removed
(for diagnostic purposes only), stay clear of moving fan blade.
Always practice team lifting when moving heavy equipment.
After servicing, verify that all access panels or covers are in place before
resuming normal operation of the equipment.
As needed:
6. Check the collector chamber for condensed or frozen solvents and dispose of
appropriately. Completely empty the collector chamber before the next run or
before attempting to start the vacuum pump.
7. If sample valves leak or stems become difficult to turn, pull the stem out of the
rubber valve body and apply a thin coat of vacuum grease to the stem.
Reinsert the stem into the valve body.
Monthly:
1. The rubber components on the Freeze Dryer may eventually deteriorate and
require replacement. The effective life of rubber parts depends upon both their
usage and the surrounding environment. Check all rubber hoses and gaskets
and replace any that show signs of hardening, permanent set or deterioration.
2. Using a soft cloth, sponge or chamois and a mild, non-abrasive soap or
detergent, clean the acrylic chamber lid.
3. Using a soft cloth, sponge, or chamois and a mild, non-abrasive soap or
detergent, clean the exterior surfaces of the Freeze Dryer. Liquid spray
cleaners and polishes may be used on the exterior surfaces. Do not use
solvents to remove stains from the exterior surfaces as they may damage the
finish.
Annually:
CHAPTER 7
TROUBLESHOOTING
Refer to the following if your Freeze Dryer fails to operate properly. If the
suggested corrective actions do not solve your problem, contact Labconco for
additional assistance.
Labconco Freeze Dry Systems that are clean, dry and without samples attached
should reach a vacuum of 0.133 mbar within 10 minutes and should achieve an
ultimate vacuum of 0.040 mbar within 18 hours when the refrigeration is
operating. If the Freeze Dryer does not obtain a satisfactory vacuum, perform the
following maintenance tests.
I. Vacuum Pump
First make sure that the vacuum pump operates. If it fails to operate, check the
electrical connections of the Freeze Dryer to the power source and then check the
electrical connection of the vacuum pump to the Freeze Dryer. If the vacuum
pump has a power switch, make sure that it is turned on. Note: If the vacuum
pump is plugged directly into a wall outlet for troubleshooting purposes, the
vacuum START button must be initiated on the display screen. If the vacuum
START button is not initiated the vacuum vent valve will remain open and
the vacuum reading will remain on HIGH. If the vacuum is not adequate when
the vacuum pump is operating, proceed with the following steps:
1. Check the oil and ensure it is clear and clean. If the oil looks cloudy or has
any particulates, replace the pump oil. Sometimes it may be necessary to
flush the pump with clean oil several times. To flush the pump, run the
pump 5 to 10 minutes to allow the oil to warm up. Drain the oil and refill
with clean oil. Repeat as necessary.
2. Check the oil level in the pump. Ensure it is filled to the correct level.
3. Check vacuum hose connections from the pump to the Freeze Dryer and try
running the unit.
4. Isolate the pump by disconnecting the vacuum hose from the Freeze Dryer.
Deadhead the pump by inserting the vacuum sensor from a secondary
vacuum gauge into the end of the vacuum hose and observe the vacuum
reading obtained. Confirm that the pump is capable of achieving an
ultimate vacuum less than 0.010 mbar or approximately 10 microns. If an
inadequate vacuum reading is obtained, the pump has most likely failed
and may need to be replaced or rebuilt.
The illustrations below show how the sample valve installs on a chamber and a
manifold.
Valve Body
Thrust Washer
Valve Body
1. Insert a rubber stopper in the small hole in the rear of the collector
chamber.
2. Start the Freeze Dryer and observe the vacuum indication. If the vacuum is
good, the problem is in the collector chamber. If it is bad, the problem is in
the plumbing connections from the collector chamber to the vacuum pump.
3. If the leak is in the plumbing connections, check all rubber parts, fittings
and clamps.
4. If the leak is in the chamber, check the drain hose, hose connections and
the quick connect drain coupling. The figure below shows other potential
leak areas (for 4.5L & 8L models) where bulkhead fittings are used to seal
the holes where the collector coil penetrates the bottom of the chamber.
COLLECTOR CHAMBER
AREAS FOR
POTENTIAL LEAKS
5. If a leak is observed around the bulkhead fittings, access the bottom of the
chamber and remove the insulation. Tighten the appropriate fitting by
placing a wrench on the fitting inside the chamber and use a second wrench
to turn the nut on the bottom of the chamber. Be careful not to damage the
evaporator coils or the brazed joints to the refrigeration system. Once the
fitting is tightened, perform the test again. If a leak is still present at the
bulkhead fittings, loosen the bulkhead fittings and apply vacuum grease to
the O-rings, then reassemble and test.
If any repairs are required on the refrigeration module, contact your local
laboratory supply dealer. If your laboratory supply dealer is unable to provide
assistance, please call Labconco. Repairs should only be undertaken by a
competent refrigeration technician or through an authorized Labconco service
agency.
APPENDIX A
FREEZE DRYER COMPONENTS
The following pages list components that are available for your Freeze Dryer. The
parts shown are the most common replacement parts. If other parts are required,
contact Product Service.
APPENDIX B
FREEZE DRYER DIMENSIONS
2.5L -50C Models (70020****)
APPENDIX C
FREEZE DRYER
SPECIFICATIONS
This Appendix contains technical information about the Freeze Dryer including
electrical specifications and operating conditions.
Electrical Specifications
Voltage Frequency Amps
Operating Max. with
Catalog # Description Nominal (Hz)
Range Vacuum Pump
115V 103-127 60 14
70020xxxx 2.5L -50C 230V 187-253 60 7
230V 198-253 50 7
115V 103-127 60 16
71020xxxx 2.5L -84C 230V 187-253 60 10
230V 198-253 50 10
115V 103-127 60 14
70040xxxx 4.5L -50C 230V 187-253 60 7
230V 198-253 50 7
115V 103-127 60 16
71040xxxx 4.5L -84C 230V 187-253 60 10
230V 198-253 50 10
115V 103-127 60 16
72040xxxx 4.5L -105C 230V 187-253 60 10
230V 198-253 50 10
115V 103-127 60 14
70080xxxx 8L -50C 230V 187-253 60 7
230V 198-253 50 7
Environmental Conditions
Indoor use only.
Ambient temperature range: 41° to 104°F (5° to 40°C).
Maximum relative humidity: 80% for temperatures up to 88°F (31°C),
decreasing linearly to 50% relative humidity at 104°F (40°C).
Main supply voltage fluctuations not to exceed ±10% of the nominal
voltage.
Transient overvoltages according to Installation Categories II (Overvoltage
Categories per IEC 1010). Temporary voltage spikes on the AC input line
that may be as high as 1500V for 115V models and 2500V for 230V
models are allowed.
Used in an environment of Pollution degrees 2 (i.e., where normally only
non-conductive atmospheres are present). Occasionally, however, a
temporary conductivity caused by condensation must be expected, in
accordance with IEC 664.
APPENDIX D
FREEZE DRYER ACCESSORIES
Labconco offers a full line of accessories to enhance your Freeze Dryer’s operation
and usability. For a complete list of these accessories, please consult our website
at www.labconco.com.