Labconco FreeZone 7949020, FreeZone 7949040, FreeZone 7949030 User Manual
FreeZone
Models
User’s Manual
®
Benchtop Shell Freezers
7949020
7949030
7949040
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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
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Please read the User’s Manual before operating the equipment.
Copyright © 2004, 2007 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® Delta® Series 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 #7392209, Rev. A
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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
Sample Surface Area and Thickness of the Sample 4
About This Manual 5
Typographical Conventions 7
CHAPTER 2: PREREQUISITES 8
Electrical Requirements 8
Location Requirements 9
CHAPTER 3: GETTING STARTED 10
Unpacking Your Benchtop Shell Freezer 10
Benchtop Shell Freezer Components 11
Installing Your Benchtop Shell Freezer 12
Electrical Connection 12
Solvent Safety Precautions 12
CHAPTER 4: USING YOUR BENCHTOP SHELL FREEZER 14
Benchtop Shell Freezer Controls 15
Operating the Benchtop Shell Freezer 15
CHAPTER 5: MAINTAINING YOUR BENCHTOP
APPENDIX A: BENCHTOP SHELL FREEZER COMPONENTS 19
APPENDIX B: BENCHTOP SHELL FREEZER DIMENSIONS 21
APPENDIX C: BENCHTOP SHELL FREEZER
Electrical Specifications 22
Environmental Conditions 22
Wiring Diagram (115V) 24
Wiring Diagram (230V) 25
DECLARATION OF CONFORMITY 26
O
O
SHELL FREEZER 17
SPECIFICATIONS 22
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Congratulations on your purchase of a Labconco FreeZone®
Benchtop Shell Freezer, which is designed to prepare samples for
laboratory lyophilization procedures. 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.
Sample Surface Area and
Thickness of the Sample
The volume and configuration of the suspension to be freeze dried
often determines how the material will be freeze dried. For
example, the greater the ratio of the surface area to the volume of
the suspension, the faster drying will occur. This is because a
greater area for the water molecules to leave the product exists
compared to the distance they have to travel to reach the surface of
the frozen matrix. Drying occurs from the top of the product and
initially the removal of water molecules is efficient. However, as
the drying front moves down through the product, drying becomes
more and more difficult. The water molecules must now travel
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Chapter 1: Introduction
through the dried portions of the product, which impedes their
progress. As the drying front moves further and further down the
matrix, the application of heat to the product becomes more
important.
Shell freezing as a method of prefreezing the product can increase
the surface area-to-volume ratio by spreading out the frozen
product inside the vessel. Shell freezing is accomplished by
rotating the vessel in a low temperature bath causing the product to
freeze in a thin layer on the inside surface of the vessel. The
thickness of the frozen suspension depends on the volume of the
product in comparison to the size of the vessel. The diagram
below shows how a Shell Freezer operates.
About This Manual
This manual is designed to help you learn how to install, use, and
maintain your Benchtop Shell Freezer. Instructions for performing
routine maintenance and making minor modifications to your
Benchtop Shell Freezer are also included.
Chapter 1: Introduction provides a brief overview of the freeze dry
process, 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 Benchtop Shell Freezer.
Electrical requirements are discussed.
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5
Chapter 1: Introduction
Chapter 3: Getting Started contains the information you need to
properly unpack, inspect and install your Benchtop Shell Freezer.
Chapter 4: Using Your Benchtop Shell Freezer discusses the basic
operation and information on how to load samples.
Chapter 5: Maintaining Your Benchtop Shell Freezer explains how
to perform routine maintenance.
Chapter 6: Troubleshooting contains information about problems
you may encounter while using your Benchtop Shell Freezer,
including the probable causes of the problems, and suggested
corrective actions.
Appendix A: Benchtop Shell Freezer Components contains labeled
diagrams of the key components of the Benchtop Shell Freezer.
Appendix B: Benchtop Shell Freezer Dimensions contains
diagrams showing the dimensions for the Benchtop Shell Freezer.
Appendix C: Benchtop Shell Freezer Specifications contains
product specifications and wiring diagrams.
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