Labconco FreeZone Plus User manual

T
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CHAPTER 1: INTRODUCTION 1
Freeze Dry Process 1
Freeze Dry Rates 2
Freeze Dry Capacity 4
Samples Containing Volatile Substances 5
About This Manual 5
Typographical Conventions 7
YourNextStep 7
CHAPTER 2: PREREQUISITES 9
ElectricalRequirements 10
Location Requirements 10
Vacuum Pump Requirements 10
Chamber or Manifold Requirements 11
Space Requirements 11
YourNextStep 11
CHAPTER 3: GETTING STARTED 13
Unpacking Your Freeze Dryer 14
Freeze Dryer Components 14
Setting Up Your Freeze Dryer 15
Component Orientation & Hose Connections 15
ElectricalConnection 16
Drying Chamber Installation 16
DryingManifoldInstallation 16
Solvent Safety Precautions 17
YourNextStep 18
CHAPTER 4: USING YOUR FREEZE DRYER 19
Freeze Dryer Controls 20
OperationChecklist 21
Operating the Freeze Dryer 22
AutomaticStart-Up 22
ManualStart-Up 23

AddingSample 23
Alarms & Informational Messages 25
ShutDown 26
Defrosting 27
CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 29
CHAPTER 6: MODIFYING YOUR FREEZE DRYER 31
RecorderJack 31
ComputerConnection 32
CHAPTER 7: TROUBLESHOOTING 35
VacuumLeakDetection 36
Refrigeration Module Operation 37
APPENDIX A: FREEZE DRYER COMPONENTS 39
APPENDIX B: FREEZE DRYER DIMENSIONS 43
APPENDIX C: FREEZE DRYER SPECIFICATIONS 45
Wiring Diagram (115V) 47
Wiring Diagram (230V) 48
APPENDIX D: FREEZE DRYER ACCESSORIES 49
DECLARATION OF CONFORMITY 57

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Congratulations on your purchase of a Labconco Freeze
Dry System. Models are available for operation on
115V or 230V.
The Labconco FreeZone® Plus 2.5 Liter Freeze Dry
System is designed for laboratory lyophilization
procedures. It is CFC 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.
Freeze Dry Process
Dehydration is an important process 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
microorganisms). The nondestructive nature of this
process has been demonstrated by the retention of
viability in freeze dried viruses and microorganisms.

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Chapter 1: Introduction
Freeze drying is a process whereby water is removed
from frozen materials by converting the frozen water
directly into its 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 water; the use
of a vacuum pump to enhance the removal of water
vapor from the surface of the sample; the transfer and
deposit of water vapor onto a collector; and the removal
of heat due to ice formation from the collector by
means of a refrigeration system. In essence, the freeze
dry process is a balance between the heat absorbed by
the sample to vaporize the water and the heat removed
from the collector to convert the water vapor into ice.
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 three 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.
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
*Total sample quantities are contingent on various freeze dryer capacities.
Table 1

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Chapter 1: Introduction
Up to the point of overloading the system, the greater
the surface area of the sample, the greater 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 10 to 15°C
colder than the eutectic temperature (melting
temperature) of the sample, traps vapor as ice. Since
the vapor pressure at the collector is less 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 efficient rate.
In most applications, the maintenance of a vacuum of
133 x 10-3 mBar or less is required for freeze drying to
occur.
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 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 at 0°C. Although the
eutectic temperature is not dependent upon the

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Chapter 1: Introduction
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
there is a simple sugar such as a 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 to less than 133 x 10-3 mBar
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 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

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Chapter 1: Introduction
cascade type refrigeration so that the collector
temperature can be cooled to below –75°C, or a dry
ice/solvent trap can be used between the collector and
the vacuum pump.
Samples Containing Volatile
Substances
In certain cases the solvent in a sample to be freeze
dried may contain volatile components such as acetic
acid, formic acid or pyridine. In addition to these
substances having an effect on the eutectic temperature,
they may enhance 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, freeze drying 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.

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Chapter 1: Introduction
Chapter 3: Getting Started contains the information
you need to properly unpack, inspect and install your
Freeze Dryer.
Chapter 4: 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 5: Maintaining Your Freeze Dryer explains
how to perform routine maintenance on your Freeze
Dryer.
Chapter 6: Modifying Your Freeze Dryer describes how
to attach a recorder or computer for monitoring the
operation.
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
comprehensive diagrams showing the dimensions for
the Freeze Dryer.
Appendix C: Freeze Dryer Specifications contains
product specifications. Wiring diagrams for both the
115V and 230V Freeze Dryer are also included.
Appendix D: Freeze Dryer Accessories lists the part
numbers and descriptions of all of the accessories
available for your Freeze Dryer.

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Chapter 1: Introduction
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.
Your Next Step
If your Freeze Dryer needs to be installed, proceed to
Chapter 2: Prerequisites to ensure your installation site
meets all of the requirements. Then, go to Chapter 3:
Getting Started for instructions on how to install your
Freeze Dryer and make all of the necessary
connections.
For information on the operational characteristics of
your Freeze Dryer, go to Chapter 4: Using Your Freeze
Dryer.
If your Freeze Dryer is installed and you need to
perform routine maintenance on the Freeze Dryer,
proceed to Chapter 5: Maintaining Your Freeze Dryer.
!
☞

8 Product Service: Domestic 1-800-522-7658, International 816-333-8811
Chapter 1: Introduction
For information on making modifications to the
configuration of your Freeze Dryer go to Chapter 6:
Modifying Your Freeze Dryer.
Refer to Chapter 7: Troubleshooting if you are
experiencing problems with your Freeze Dryer.

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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.
Carefully read this chapter to learn:
• the electrical supply requirements.
• the vacuum pump requirements.
• chamber or manifold requirements.
Refer to Appendix C: Freeze Dryer Specifications for
complete Freeze Dryer electrical and environmental
conditions, specifications and requirements.

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Chapter 2: Prerequisites
Electrical Requirements
The Freeze Dryer requires a dedicated electrical outlet.
This outlet requires a 20 Amp circuit breaker or fuse for
models rated at 115V (60 Hz). A 10 Amp circuit
breaker or fuse is required for models rated at 230V
(50 Hz). 115V models are equipped with a 20 Amp
NEMA 5-20P plug. 230V models are not equipped
with a plug. It will be necessary to install a plug to
match the available receptacle.
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 grill on the
front panel and exhausts it out through the back and
sides of the cabinet. A minimum of 3" must be allowed
between the back and sides of the Freeze Dryer and
adjacent wall surfaces. Restriction of airflow during
operation could adversely affect performance.
Vacuum Pump
Requirements
A vacuum pump must be provided by the user. A
vacuum pump with a displacement of 113 liters per
minute and 0.2 x 10-3 mBar blank off pressure is
adequate for most samples. The inlet fitting on the
vacuum pump must be suitable for 0.75 ID hose which
is provided.

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Chapter 2: Prerequisites
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 320 plug. This will
allow the vacuum pump to be plugged into the
receptacle on the back of the Freeze Dryer. See
Appendix D: Freeze Dryer Accessories for vacuum
pumps available from Labconco.
Chamber or Manifold
Requirements
A freeze drying chamber or manifold must be
purchased separately. These allow samples to be
attached to the Freeze Dryer. See Appendix D: Freeze
Dryer Accessories for available chambers and
manifolds.
Space Requirements
Refer to Appendix C: Freeze Dryer Specifications for
dimensional drawings of the Freeze Dryer.
Your Next Step
After you have determined that the location for your
Freeze Dryer accommodates the installation and
operational requirements, you are ready to unpack and
install your Freeze Dryer. Proceed to Chapter 3:
Getting Started.

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Chapter 2: Prerequisites

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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 Freeze Dryer weighs over 135 lbs.
(61 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 (2)
persons and follow safe lifting
guidelines.
!
!!
!

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Chapter 3: Getting Started
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.
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
As previously mentioned, the Freeze Dryer System is
available in 115V or 230V. Locate the model of Freeze
Dryer you received in the following table. Verify that
the components listed are present and undamaged.
The United States
I
nterstate Commerce
Commission rules
require that claims be
f
iled with the delivery
carrier within fifteen (15)
days of delivery.
☞
☞

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Chapter 3: Getting Starte
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Catalog # Product Description
76700-00 Freeze Dryer – 115V, 60 Hz
76700-01 Freeze Dryer – 230V, 50 Hz
Plus the Following:
Part # Component Description
74776-00 User’s Manual
13364-00
13373-00
Power Cord – 115V
or
Power Cord – 230V
76460-00 Tubing
19676-00 Clamp (2)
If you do 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.
Component Orientation & Hose
Connections
The refrigeration system in the Freeze Dryer exhausts
air through the rear of the cabinet. A minimum of 3"
should be allowed between the back of the Freeze
Dryer and the adjacent wall surface and between the
sides of the Freeze Dryer and the adjacent wall
surfaces. Restriction of the airflow through the cabinet
during operation could adversely affect performance.
Position the vacuum pump near the vacuum exhaust
port on the rear of the cabinet. Attach the supplied hose
to the exhaust port using the clamp provided. Attach
the other end of the hose to the inlet fitting on the
vacuum pump. Secure with the clamp provided. The
hose may be cut to proper length to allow for gentle
bends without kinks.

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Chapter 3: Getting Started
Electrical Connection
Plug the power cord into the receptacle on the back of
the Freeze Dryer and plug the other end into a suitable
power receptacle. Plug the power cord from the
vacuum pump into the receptacle on the back of the
Freeze Dryer. If the vacuum pump has an off/on
switch, turn the switch on. The vacuum pump will be
controlled by the Freeze Dryer.
Drying Chamber Installation
The drying chamber, purchased separately, may be
positioned directly above and centered over the
collection chamber. When vacuum is applied to the
system, the chamber will be held securely in place.
Drying Manifold Installation
If a drying manifold is to be installed, first place the
accessory acrylic attachment port lid 74774-00 over the
collection chamber. Then the manifold can be inserted
into the hole on the lid making sure that the rubber
gasket is between the lid and the flange on the
manifold.
Solvent Safety
Precautions
Solvents used in the Freeze Dryer may
be flammable or hazardous. Use
extreme caution and keep sources of
ignition away from the solvents.
When using flammable or hazardous
solvents, the vacuum pump should 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
!
!!
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Chapter 3: Getting Starte
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spilled. If a sample is spilled in the
collector chamber it must immediately
be cleaned up.
Several components of the Freeze
Dryer, which are located inside the
chamber, are made of stainless steel
which can be attacked by acids. Use
of acids can result in degradation of
the product and the vacuum pump.
Use care when using aggressive liquids
which can damage the Freeze Dryer
and thoroughly clean the Freeze
Dryer after each use. Instructions for
cleaning are in Chapter 5: Maintaining
Your Freeze Dryer.
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.
Your Next Step
The installation and setup of your Freeze Dryer is now
complete. To learn how to load and operate your
Freeze Dryer, proceed to Chapter 4: Using Your Freeze
Dryer. To make a modification to the configuration of
your Freeze Dryer, proceed to Chapter 6: Modifying
your Freeze Dryer. To perform additional diagnostics
on your Freeze Dryer, proceed to Chapter
7:Troubleshooting. To learn about the maintenance
requirements for your Freeze Dryer, proceed to Chapter
5: Maintaining Your Freeze Dryer.

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Chapter 3: Getting Started