Labconco FreeZone 6 User manual

FreeZone® 6, 12 and 18 Liter
Freeze Dry Systems
Models
7753000 7753500 7754000 7754500 7755000 7755500
7753001 7753501 7754001 7754501 7755001 7755501
7753003 7753503 7754003 7754503 7755003 7755503
7753010 7753510 7754010 7754510 7755010 7755510
7753011 7753511 7754011 7754511 7755011 7755511
7753013 7753513 7754013 7754513 7755013 7755513
User’s Manual
LABCONCO CORPORATION
8811 PROSPECT AVENUE
KANSAS CITY, MO 64132-2696
800-821-5525, 816-333-8811
FAX [phone]
E-MAIL [email protected]
HOME PAGE www.labconco.com
Labconco’s Mascot,
Labby the LABster
Register your product online at
www.labconco.com/productreg.html
or return the attached card and
receive FREE LabbyWear™!

Product designs are subject to change without notice
© 2002 Labconco Corporation
Printed in U.S.A.

Copyright Information
Copyright © 2002 Labconco Corporation. All rights reserved.
Labconco Corporation
8811 Prospect Avenue
Kansas City, Missouri 64132
The information contained in this manual and the accompanying product are copyrighted and all rights are
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.
FreeZone® is a registered trademark of Labconco Corporation.
Warranty
Labconco provides a warranty on all parts and factory workmanship. The warranty includes areas of
defective material and workmanship, provided such defect results from normal and proper use of the
equipment.
The warranty for all Labconco products will expire one year from date of installation or two years from
date of shipment from Labconco, whichever is sooner, except the following:
• Purifier® Delta® Series Biological Safety Cabinets carry a three-year warranty from date of
installation or four years from date of shipment from Labconco, whichever is sooner.
• Carts carry a lifetime warranty.
• Glassware is not warranted from breakage when dropped or mishandled.
This limited warranty covers parts and labor, but not transportation and insurance charges. In the event of a
warranty claim, contact Labconco Corporation or the dealer who sold you the product. If the cause is
determined to be a manufacturing fault, the dealer or Labconco Corporation will repair or replace all
defective parts to restore the unit to operation. Under no circumstances shall Labconco Corporation be
liable for indirect, consequential, or special damages of any kind. This statement may be altered by a
specific published amendment. No individual has authorization to alter the provisions of this warranty
policy or its amendments. Lamps and filters are not covered by this warranty. Damage due to corrosion or
accidental breakage is also not covered.
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 7:00
a.m. and 6:00 p.m., Central Standard Time.
Visit Labconco’s web site at: http://www.labconco.com or email Labconco at: [e-mail].
Part #7517300
REV C/ECO B184
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CHAPTER 1: INTRODUCTION 1
FreezeDryProcess 1
FreezeDryRates 2
FreezeDryCapacity 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
UnpackingYourFreezeDryer 14
Freeze Dryer Components 14
Setting Up Your Freeze Dryer 16
Component Orientation 16
Vacuum Pump Connection 16
ElectricalConnection 17
Drying Chamber or Drying Manifold Installation 17
Solvent Safety Precautions 17
YourNextStep 18
CHAPTER 4: USING YOUR FREEZE DRYER 19
FreezeDryerControls 20
OperationChecklist 22
Vacuum Pump Ballast Setting 22
PurgeValve 23
Operating the Freeze Dryer 24
AutomaticStart-Up 24
ManualStart-Up 25

AddingSample 26
Alarms&InformationalMessages 28
ShutDown 29
Defrosting 30
ShellFreezer 31
CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 33
CHAPTER 6: USING THE RECORDER JACK 35
Recorder Jack Pin Configuration 35
Computer Connection 36
CHAPTER 7: TROUBLESHOOTING 41
VacuumPump 41
Gaskets, Tubing, Connections, Sample Valves 42
System Components & Collection Chamber Isolation 44
Refrigeration Module Operation 48
APPENDIX A: FREEZE DRYER COMPONENTS 49
APPENDIX B: FREEZE DRYER DIMENSIONS 53
APPENDIX C: FREEZE DRYER SPECIFICATIONS 55
Electrical Specifications 55
Environmental Conditions 56
Wiring Diagram (115V) 57
Wiring Diagram (230V) 58
APPENDIX D: FREEZE DRYER ACCESSORIES 59
DECLARATION OF CONFORMITY 69

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Congratulations on your purchase of a Labconco
FreeZone® Console Freeze Dry System. Console
models are available in 6, 12, and 18 liter system
capacity. PTFE coated collector chamber, purge
valve, and shell freezer are optional on all models.
The Labconco Console 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 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.
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 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 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 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
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
the sample contains 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 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, 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: Using the Recorder Jackr 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. A wiring diagram for the Freeze
Dryer is 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.
!
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Chapter 1: Introduction
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.
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). An outlet equipped with
a 15 Amp circuit breaker or fuse is required for models
rated at 230V (50/60 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 through the back. A
minimum of 3" must be allowed between the back 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 150 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 3/4” ID vacuum
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 250V, 15 Amp NEMA 6-15P plug (a
250V, 15 Amp NEMA 6-15P plug is included with
230V models). This will allow the vacuum pump to be
plugged into the receptacle on the junction box inside
the console cabinet. See Appendix D: Freeze Dryer
Accessories for vacuum pumps available from
Labconco.
Chamber or Manifold
Requirements
A freeze drying chamber or manifold is not included
and 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 300 lbs.
(136 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
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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