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 3rd
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.
Do not return goods without the prior authorization from Labconco. Unauthorized returns will not be
accepted. If your shipment was damaged in transit, you must file a claim directly with the freight carrier.
Labconco Corporation and its dealers are not responsible for shipping damages.
The United States Interstate Commerce Commission rules require that claims be filed with the delivery
carrier within fifteen (15) days of delivery.
Limitation of Liability
The disposal and/or emission of substances used in connection with this equipment may be governed by
various federal, state, or local regulations. All users of this equipment are required to become familiar with
any regulations that apply in the user’s area concerning the dumping of waste materials in or upon water,
land, or air and to comply with such regulations. Labconco Corporation is held harmless with respect to
user’s compliance with such regulations.
Contacting Labconco Corporation
If you have questions that are not addressed in this manual, or if you need technical assistance, contact
Labconco’s Customer Service Department or Labconco’s Product Service Department at 1-800-821-5525
or 1-816-333-8811, between the hours of 7:30 a.m. and 5:30 p.m., Central Standard Time.
Part #7343300, Rev. A
ECO L423
Original instructions
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
Congratulations on your purchase of a Labconco FreeZone® Triad™ 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 Dry Process
Freeze drying is an important process in sample preparation and for the preservation
and storage of biologicals, pharmaceuticals and foods. Of the various methods of
dehydration, freeze drying (lyophilization) is especially suited for substances that are
heat sensitive. Other than food processing (e.g., coffee, whole dinners), freeze drying
has been extensively used in the development of pharmaceuticals (e.g., antibiotics) and
preservation of biologicals (e.g., proteins, plasma, viruses and cell lines). The
nondestructive nature of this process has been demonstrated by the retention of
viability in freeze dried viruses and microorganisms.
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.
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Chapter 1: Introduction
2
Original instructions
SAFE TEMPERATURE AND DRYING TIMES
FOR SELECTED MATERIALS
Material
10mm Thick
Safe
Temperature
°C
Collector
Temperature
°C
Hours
(Approx.)
Milk
-5
-40
10
Urea
-7
-40
10
Blood Plasma
-10 to -25
-40
16
Serum
-25
-40
18
Vaccinia
-30 to -40
-50
22
Influenza Vaccine
-30
-50
24
Human Tissue
-30 to -40
-50
48
Vegetable Tissue
-50
-80
60
Table 1
Freeze Dry Rates
The efficiency of the Freeze Drying process is dependent upon the surface area and
the thickness of the sample, the collector temperature and vacuum obtained, the
eutectic point and solute concentration of the sample. It is important to remember
these factors when trying to obtain efficient utilization of your Freeze Dry system.
A listing of selected materials and their approximate drying times are shown in
Table 1 for your reference.
*Total sample quantities are contingent on various freeze dryer capacities.
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
Product Service 816-333-8811 or 1-800-522-7658
Chapter 1: Introduction
3
Original instructions
efficient rate. In many applications, the maintenance of a vacuum of 0.133 mbar
or less is recommended.
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.
Freeze Dry Capacity
The volume of a sample that can be freeze dried at one time is related to factors
discussed previously and the size and design of the freeze dry system. With any
given instrument, the capacity is based on the surface area of the sample; the
eutectic temperature and concentration of the sample; and the rate and amount of
heat transferred to the frozen sample. Of these factors, the eutectic temperature is
the most important factor in determining the amount of sample that can be freeze
dried at one time, particularly when flasks are used. This is because as the eutectic
temperature decreases, the vapor pressure decreases but the rate of heat absorption
by the sample does not change. This tends to promote melting of the sample,
which leads to a marked increase in vapor pressure and ultimately overloads the
collector and vacuum pump. Samples that have eutectic temperatures of –20°C or
lower should be placed on the freeze dry system one flask at a time so that the
vacuum in the system may recover before adding another sample to the system. If
the vacuum does not recover, the capacity of the freeze dry system has been
exceeded and the sample should be removed.
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 (when utilizing In-Flask mode) to decrease the rate of
heat absorption by the sample may help.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 1: Introduction
4
Original instructions
Samples Containing Volatile Substances
In certain cases the solvent in a sample to be freeze dried may contain volatile
components such as acetonitrile, methanol, acetic acid, formic acid or pyridine. In
addition to these substances having an effect on the eutectic temperature, they may
increase the vapor pressure at the surface of the sample. Also, compared to water,
they will require the absorption of less heat for sublimation to occur. Hence,
samples that contain volatile substances will have a greater tendency to melt,
particularly when placed in flasks or exposed to room temperature. If a sample
containing a volatile substance tends to melt when placed on a freeze dry system,
dilution of the sample with more water will help keep the sample frozen. For
example, a 0.2M solution of acetic acid is much easier to freeze dry than a 0.5M
solution.
About This Manual
This manual is designed to help you learn how to install, use, and maintain your
Freeze Dryer. Instructions for performing routine maintenance and making minor
modifications to your Freeze Dryer are also included.
Chapter 1: Introduction provides a brief overview of the Freeze Dryer, explains
the organization of the manual, and defines the typographical conventions used in
the manual.
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.
Chapter 6: Maintaining Your Freeze Dryer explains how to perform routine
maintenance on your Freeze Dryer.
Chapter 7: Troubleshooting contains a table of problems you may encounter while
using your Freeze Dryer, including the probable causes of the problems, and
suggested corrective actions.
Appendix A: Freeze Dryer Components contains labeled diagrams of the
components of the Freeze Dryer.
Appendix B: Freeze Dryer Dimensions contains diagrams showing the dimensions
for the Freeze Dryer.
Appendix D: Freeze Dryer Accessories seewww.labconco.com for a complete list
of Freeze Dry accessories.
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.
Product Service 816-333-8811 or 1-800-522-7658
6
Original instructions
CHAPTER2
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.
Refer to Appendix C: Freeze Dryer Specifications for complete Freeze Dryer
electrical and environmental conditions, specifications and requirements.
Electrical Requirements
230V models
o 20 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.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 2: Prerequisites
7
Original instructions
!
!
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. The Triad Freeze Dryer must be placed on a work
surface or table that will support over 400 lbs.
Refer to Appendix B: Freeze Dryer Dimensions for dimensional drawings.
Vacuum Pump Requirements
A vacuum pump must be provided by the user. A vacuum pump with a
displacement of 98 liters per minute and 0.007 mbar ultimate pressure is adequate
for most samples. The inlet fitting on the vacuum pump must be suitable for 3/4"
ID vacuum hose, which is provided. It is recommended that the vacuum pump is
equipped with an exhaust filter to minimize oil mist exhausting from the vacuum
pump. The operating vacuum level may be set on the Freeze Dryer. The higher
the vacuum set point, the more likely it is that oil mist will be exhausted.
Vacuum pumps 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.
Product Service 816-333-8811 or 1-800-522-7658
8
Original instructions
!
The United
States
Interstate
Commerce
Commission
rules require
that claims be
filed with the
delivery carrier
within fifteen
(15) days of
delivery.
CHAPTER3
GETTINGSTARTED
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:
Unpack and move your Freeze Dryer.
Set up your Freeze Dryer.
Connect the electrical supply source to your Freeze Dryer.
Properly exhaust your Freeze Dryer.
Safely use solvents with your Freeze Dryer.
The Triad Freeze Dryers weigh over 400 lbs (181 Kg). The
carton allows for lifting with a mechanical lift truck or hand
truck. If you must lift the Freeze Dryer manually, use at least
two (4) persons and follow safe lifting guidelines.
Unpacking Your Freeze Dryer
Carefully unpack your Freeze Dryer and inspect it for damage that may have
occurred in transit. If your Freeze Dryer is damaged, notify the delivery carrier
immediately and retain the entire shipment intact for inspection by the carrier.
DO NOT RETURN GOODS WITHOUT THE PRIOR
AUTHORIZATION OF LABCONCO. UNAUTHORIZED
RETURNS WILL NOT BE ACCEPTED.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
9
Original instructions
Qty.
Part #
Description
Comments
1
1089005
User’s Manual
USB Flash Drive
1
Various
Power Cord
See parts list (Appendix A)
1
7373450
Vacuum Hose
2
1488800
Hose Clamp
IF YOUR FREEZE DRYER WAS DAMAGED IN TRANSIT,
YOU MUST FILE A CLAIM DIRECTLY WITH THE FREIGHT
CARRIER. LABCONCO CORPORATION AND ITS DEALERS
ARE NOT RESPONSIBLE FOR SHIPPING DAMAGE.
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.
Freeze Dryer Components
Verify that the components listed below are present and undamaged.
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.
Setting Up Your Freeze Dryer
After you verify receipt of the proper components, move your Freeze Dryer to the
location where you want to install it. Then, follow the steps listed below.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
10
Original instructions
Sample Valves
USB Port
Touch Screen
Stoppering Control
Vacuum Release
Backfill Port
On/Standby Button
LED Indicator
Ethernet Port
End Point Detection
Vacuum Pump Outlet
Power Inlet
Vacuum Connection
Circuit Breaker Reset
Component Identification
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
11
Original instructions
HOSE
CLAMP
VACUUM HOSE
3/4" ID
VACUUM
PUMP
!
Hose Barb
Clamp
Inlet
Vacuum Pump Connection
A vacuum pump (as described in Chapter 2: Prerequisites) is required to operate
your Freeze Dryer properly. The Freeze Dryer is equipped with a 3/4" ID vacuum
hose for connecting the collector chamber to the vacuum pump.
Make certain that the oil in the vacuum pump is at the proper
level.
1. Place the vacuum pump near the Triad Freeze
Dryer.
2. Remove protective caps from inlet and outlet
ports.
3. Some vacuum pumps have inlet fittings that clamp
to the pump. Place the centering ring with filter
screen on the inlet fitting.
4. Place the hose barb fitting on top of the centering
ring and secure with the clamp.
5. CHECK THE VACUUM PUMP OIL LEVEL.
Fill the pump with oil so the level is between
the lines on the sight gauge on the end of the
pump housing.
6. Attach one end of the vacuum hose to the port
on the back of the Freeze Dryer and the other
end to the inlet port of the vacuum pump with
the hose clamps provided. If necessary, cut
the hose to proper length to allow for gentle
bends without kinks.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
12
Original instructions
7. VERIFY THE VACUUM PUMP VOLTAGE SETTING AGREES WITH
THE FREEZE DRYER VOLTAGE SHOWN ON THE SERIAL
NUMBER LABEL. Reconfigure if necessary (see vacuum pump
instructions).
8. Connect the vacuum pump power cord to the receptacle labeled “vacuum
pump” on the back of the Freeze Dryer. Models rated for use on 230V
have a reverse IEC receptacle for attaching the vacuum pump power cord.
9. If the vacuum pump has an ON/OFF switch, turn the switch ON. The
vacuum pump will be controlled by the Freeze Dryer.
IT IS HIGHLY RECOMMENDED THAT AN OIL MIST
EXHAUST FILTER BE INSTALLED ON ROTORY VANE
VACUUM PUMPS TO MINIMIZE OIL MIST EXITING THE
PUMP. AN OIL RETURN KIT CAN ALSO BE USED IN
CONJUNCTION WITH THE EXHAUST FILTER TO RETURN
TRAPPED OIL BACK TO THE VACUUM PUMP.
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.
Chemical Resistance of Freeze Dryer
Components
The FreeZone Freeze Dry System is designed to be chemically resistant to most
compounds that are commonly used in freeze drying processes. However, by
necessity, the freeze dryer is comprised of a number of different materials, some of
which may be attacked and degraded by certain chemicals. The degree of
degradation is dependent on the concentration and exposure duration. Some of the
major components of the Freeze Dryer that are susceptible to degradation are as
follows:
Acetone Acetonittirle Carbon Tetrochloride Cyclohexane Dioxane Methyl t
-Butyl Ether (BTBE)
Pyridine
Valve Stem
Acetal
C D D D D
Collector
Lid
Acrylic
D D D D
Hoses,
Gaskets &
Valve
Bodies
Neoprene
C D D C C D D D C
D
Flask Top
Silicon
Rubber
C D D D D D C
D
Chamber &
Fittings
Stainless
Steel
C
C – Moderate degradation; Limited use
D – Severe degradation; infrequent use recommended; immediate thorough
cleaning required.
Most common compounds used in freeze drying processes, if allowed to enter
the vacuum pump, will degrade the oil and cause damage to the vacuum pump.
Sugars and proteins typically will have minimal negative effect on any of the
materials of construction.
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.
Rubber and plastic components that have been exposed to damaging
compounds should be removed and flushed with water.
The oil in the vacuum pump should be checked often. It must be changed if it
is cloudy, shows particles or is discolored. The useful life of vacuum pump oil
can be extended if the vacuum pump is operated for an extended period of time
after a freeze dry run. This allows contaminants to be purged from the hot oil.
This must be done with the inlet to the pump blocked off to prevent air from
free flowing through the pump. If the pump is operated at an elevated vacuum
level (> 10mbar), oil may be expelled from the pump and damage could occur.
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.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
14
Original instructions
!
With prudent maintenance the Freeze Dryer 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: labconco@labconco.com.
Solvent Safety Precautions
Solvents used in the Freeze Dryer may be flammable or
hazardous to your health. Use extreme caution and keep
sources of ignition away from the solvents. When using
flammable or hazardous solvents, the vacuum pump must be
vented to or operated inside a fume hood.
Hazardous materials such as strong acids or bases, radioactive
substances and volatile organics must be handled carefully and
promptly cleaned up if spilled. If a sample is spilled in the
collector chamber it must immediately be cleaned up.
WARNING: The disposal of substances used in connection with
this equipment may be governed by various Federal, State or
local regulations. All users of this equipment are urged to
become familiar with any regulations that apply in the user’s
area concerning the dumping of waste materials in or upon
water, land or air and to comply with such regulations.
Product Service 816-333-8811 or 1-800-522-7658
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