Labconco FreeZone 1 User Manual
y Sy
FreeZone
Freeze Dr
Models
User’s Manual
®
1 Liter Benchtop
stems
77400 Series
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Labconco Corporation
8811 Prospect Avenue
Kansas City, MO 64132-2696
800-821-5525, 816-333-8811
FAX 816-363-0130
E-MAIL labconco@labconco.com
HOME PAGE www.labconco.com
Please read the User’s Manual before operating the equipment.
Copyright © 2004, 2007, 2012, 2013 Labconco Corporation. All rights reserved.
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 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® Logic® Biological Safety Cabinets and PuriCare® Lab Animal Research Stations
carry a three-year warranty from date of installation or four years from date of shipment from
Labconco, whichever is sooner.
• SteamScrubber® & FlaskScrubber® Glassware Washers carry a two-year warranty from date
of installation or three years from date of shipment from Labconco, whichever is sooner.
• Blood Drawing Chairs carry a ten year warranty.
• 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 not covered.
Returned or Damaged Goods
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 7:00 a.m. and 6:00 p.m., Central Standard Time.
Part #7429300, Rev. E
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CHAPTER 1: INTRODUCTION 1
Freeze Dry Process 1
Freeze Dry Rates 2
Freeze Dry Capacity 3
Samples Containing Volatile Substances 4
About This Manual 4
Typographical Conventions 6
Your Next Step 6
CHAPTER 2: PREREQUISITES 7
Electrical Requirements 7
Location Requirements 8
Vacuum Pump Requirements 8
Chamber or Manifold Requirements 8
CHAPTER 3: GETTING STARTED 9
Unpacking Your Freeze Dryer 9
Freeze Dryer Components 10
Setting Up Your Freeze Dryer 11
Vacuum Pump Connection 11
Electrical Connection 11
Drying Chamber or Drying Manifold Installation 12
Chemical Resistance of Freeze Dryer Components 12
Solvent Safety Precautions 13
CHAPTER 4: USING YOUR FREEZE DRYER 15
Freeze Dryer Controls 16
Operation Checklist 16
Vacuum Pump Ballast Setting 17
Operating the Freeze Dryer 17
Set-Up 17
Automatic Start-Up 19
Manual Start-Up 20
Pre Freezing Samples 21
Adding Sample 21
Shut Down 22
Defrosting 22
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CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 24
CHAPTER 6: TROUBLESHOOTING 26
Vacuum Pump 26
Gaskets, Tubing, Connections, Sample Valves 27
System Components & Collection Chamber Isolation 29
Refrigeration Module Operation 31
CHAPTER 7: MODIFYING YOUR FREEZE DRYER DISPLAY 32
Temperature and Vacuum Display 32
Modifying the Display 32
APPENDIX A: FREEZE DRYER COMPONENTS 34
APPENDIX B: FREEZE DRYER DIMENSIONS 37
APPENDIX C: FREEZE DRYER SPECIFICATIONS 38
Electrical Specifications 38
Environmental Conditions 38
APPENDIX D: FREEZE DRYER ACCESSORIES 39
DECLARATION OF CONFORMITY 47
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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
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.
1
1
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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1
Chapter 1: Introduction
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.
SAFE TEMPERATURE AND DRYING TIMES
FOR SELECTED MATERIALS
Material
10mm Thick
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.
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.
Safe
Temperature
°C
Collector
Temperature
°C
Table 1
Hours
(Approx.)
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Chapter 1: Introduction
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 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
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3
Chapter 1: Introduction
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 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.
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.
4
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Chapter 1: Introduction
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: 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: 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.
Chapter 7: Modifying your Freeze Dryer Display explains how to
recalibrate your Freeze Dryer display.
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.
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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5
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.
Refer to Chapter 6: Troubleshooting if you are experiencing
problems with your Freeze Dryer.
6
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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.
2
2
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). The power cord
on 115V models are equipped with a 20 Amp NEMA 5-20P plug.
Various power cord configurations are provided with 230V
models. If this does not match the available receptacle, remove
this plug and replace it with an approved plug of the suitable style.
7 Product Service: Domestic 1-800-522-7658, International 816-333-8811
Chapter 2: Prerequisites
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.
Refer to Appendix C: Freeze Dryer Specifications for dimensional
drawings of the Freeze Dryer. The space must be large enough to
accommodate the vacuum pump, which will be used with the
Freeze Dryer.
Vacuum Pump Requirements
A vacuum pump must be provided by the user. A vacuum pump
with a displacement of 86 liters per minute and 0.002 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.
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. This
plug is included with 230V models. This will allow the vacuum
pump to be plugged into the receptacle on the back panel 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 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.
8
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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 FreeZone 1 Liter Freeze Dry System weighs
!
over 82 lbs. (37 Kg). If you must lift the Freeze
Dryer manually, use at least two (2) persons and
follow safe lifting guidelines.
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TTAARRTTEEDD
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.
The United States
Interstate Commerce
Commission rules
require that claims be
filed with the delivery
carrier within fifteen (15)
days of delivery.
9 Product Service: Domestic 1-800-522-7658, International 816-333-8811
Chapter 3: Getting Started
Freeze Dryer Components
Locate the model of Freeze Dryer you received in the following
table. Verify that the components listed are present and
undamaged.
)
)
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.
Power Cords
PTFE
Coated
Catalog # Description Volts Hz
7740020 1L Freeze Dryer 115 60 X
7740021 1L Freeze Dryer 115 60 X X
7740030 1L Freeze Dryer 230 50 X
7740031 1L Freeze Dryer 230 50 X X
7740040 1L Freeze Dryer 230 60 X
7740041 1L Freeze Dryer 230 60 X X
7740060 1L Freeze Dryer 230 50 X
7740061 1L Freeze Dryer 230 50 X X
7740070 1L Freeze Dryer 230 50 X
7740071 1L Freeze Dryer 230 50 X X
Chamber
1336400
1336500
1342100
1332601
Plus the following:
Part # Component Description
7429300 User’s Manual
1291000 Plug (230V models only)
7373450 Vacuum Hose
1488800 Hose Clamps (2)
7395801 Chamber Lid
7395800 Lid Gasket
7386901 Fitting
1332701
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Chapter 3: Getting Started
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.
Vacuum Pump Connection
A vacuum pump as described in Chapter 2: Prerequisites is
required to operate your Freeze Dry System properly. The Freeze
Dryer is equipped with a 3/4" ID, heavy wall, vacuum hose for
connecting to the collector chamber to the vacuum pump.
Make certain that the oil in the vacuum pump is
!
Place the vacuum pump near the Freeze Dryer. Connect the
vacuum pump power cord to the receptacle on the back of the
cabinet labeled “vacuum pump”. If the vacuum pump has an
off/on switch, turn the switch on. The vacuum pump will be
controlled by the Freeze Dryer. Connect the vacuum pump inlet
port to the vacuum tube on the back of the cabinet with the vacuum
hose and clamps provided. If necessary, cut the hose to proper
length to allow for gentle bends without kinks.
Models rated for use on 230V have a reverse IEC connector for
attaching the vacuum pump power cord. A plug is supplied that
can be installed on the vacuum pump power cord, if necessary.
at the proper level.
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.
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Chapter 3: Getting Started
Drying Chamber or Drying Manifold
Installation
The drying chamber or drying manifold, purchased separately, may
be positioned directly above the 3-inch hole in the collector
chamber lid. When vacuum is applied to the system, the chamber
will be held securely in place.
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 FreeZone Freeze
Dry System that are susceptible to degradation are as follows:
Acids Buffers Solvents
Component
Valve Stem Acetal C D D D D
Collector
Lid
Hoses,
Gaskets &
Valve
Bodies
Flask Top Silicon
Chamber &
Fittings
C – Moderate degradation; Limited use
D – Severe degradation; Infrequent use recommended; Immediate
thorough cleaning required.
Material
Acrylic D D D D
Neoprene C D D C C D D D C D
Rubber
Stainless
Steel
Acetic Acid 20%
Formic Acid
Trifluoroacetic Acid (TFA)
C D D D D D C D
C
Calcium Chloride
Sodium Phosphate
Acetone
Acetonittirle
Carbon Tetrochloride
Cyclohexane
Dioxane
Methyl t-Butyl Ether (BTBE)
Pyridine
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