Labconco FreeZone 2.5 User Manual
FreeZone
2.5 Liter Freeze Dry Systems
Models
74200 Series
76700 Series
76705 Series
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User’s Manual
Please read the User’s Manual before operating the equipment.
Labconco Corporation
HOME PAGE www.labconco.com
8811 Prospect Avenue
Kansas City, MO 64132-2696
800-821-5525, 816-333-8811
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E-MAIL labconco@labconco.com
Copyright © 2004, 2007, 2012, 2013, 2014 Labconco Corporation. All rights reserved.
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. Glassware is not warranted from breakage when dropped or mishandled.
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.
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.
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.
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 #7426100, Rev. H
ECO J323
TABLE OF CONTENTS
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 5
Your Next Step 5
CHAPTER 2: PREREQUISITES 6
Electrical Requirements 6
Location Requirements 6
Vacuum Pump Requirements 7
Chamber or Manifold Requirements 7
CHAPTER 3: GETTING STARTED 8
Unpacking Your Freeze Dryer 9
Freeze Dryer Components 9
Setting Up Your Freeze Dryer 11
Component Orientation 11
Vacuum Pump Connection 11
Electrical Connection 12
Drying Chamber or Drying Manifold Installation 12
Chemical Resistance of Freeze Dryer Components 12
Solvent Safety Precautions 14
CHAPTER 4: USING YOUR FREEZE DRYER 15
Freeze Dryer Controls 16
Operation Checklist 17
Vacuum Pump Ballast Setting 17
Operating the Freeze Dryer 17
Set-Up 17
Baffle 20
Automatic Start-Up 20
Manual Start-Up 20
Setting the Operating Vacuum Level 20
Pre-Freezing Samples 21
Adding Sample 21
Shut Down 22
Defrosting 23
Alarms 23
Power Failure 23
Line Voltage Out of Range 24
Temperature Out of Range 24
Service Vacuum Pump 25
Moisture in Collector 25
CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 26
CHAPTER 6: USING THE RS232 RECEPTACLE 28
Computer Connection for Computer Interface 28
CHAPTER 7: TROUBLESHOOTING 32
Vacuum Pump 32
Gaskets, Tubing, Connections, Sample Valves 33
System Components & Collection Chamber Isolation 35
Refrigeration Module Operation 37
CHAPTER 8: MODIFYING YOUR FREEZE DRYER DISPLAY 38
Temperature and Vacuum Display 38
Line Voltage Alarm Points 38
Moisture Sensor Alarm 39
Modifying the Display 39
APPENDIX A: FREEZE DRYER COMPONENTS 43
APPENDIX B: FREEZE DRYER DIMENSIONS 48
APPENDIX C: FREEZE DRYER SPECIFICATIONS 51
Electrical Specifications 51
Environmental Conditions 52
APPENDIX D: FREEZE DRYER ACCESSORIES 53
1
CHAPTER 1
INTRODUCTION
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.
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.
Product Service 1-800-522-7658
Chapter 1: Introduction
2
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
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 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.
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Chapter 1: Introduction
4
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: 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 RS232 Receptacle describes how to connect a 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.
Chapter 8: 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.
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Chapter 1: Introduction
5
!
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.
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 7: Troubleshooting if you are experiencing problems with your
Freeze Dryer.
Product Service 816-333-8811 or 1-800-522-7658
6
CHAPTER 2
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.
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.
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.
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.
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Chapter 2: Prerequisites
7
IT IS RECOMMENDED THAT THE CONSOLE MODEL
FREEZE DRYER IS SECURELY ATTACHED TO THE FLOOR
AFTER IT IS LOCATED WHERE IT WILL BE USED. THIS
WILL PREVENT ACCIDENTAL TIPPING AND POSSIBLE
INJURY. SEE INSTRUCTIONS IN CHAPTER 3 GETTING
STARTED.
Refer to Appendix C: Freeze Dryer Specifications for dimensional drawings of the
Freeze Dryer. The space for benchtop models 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. The operating vacuum level may be set on the Freeze Dryer. The higher
the pressure is set, the more likely it is that oil mist will be exhausted.
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.
Product Service 816-333-8811 or 1-800-522-7658
8
!
CHAPTER 3
GETTING STARTED
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 2.5 Liter Benchtop Freeze Dryer System weighs
over 82 lbs. (37 kg). The Benchtop FreeZone Plus 2.5 Liter
Freeze Dry System weighs over 106 lbs. (48 Kg). The Console
FreeZone Plus 2.5 Liter Freeze Dry System weighs over 152 lbs.
(69 Kg). If you must lift the Freeze Dryer manually, use at least
two (2) persons and follow safe lifting guidelines.
Product Service 1-800-522-7658
Chapter 3: Getting Started
9
The United
States
Interstate
Commerce
Commission
rules require
that claims be
filed with the
delivery carrier
within fifteen
(15) days of
delivery.
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.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
10
Power Cords
Catalog #
Description
Volts
Hz
PTFE
Coated
Chamber
1336400
1336500
1342100
1332601
1332701
7670520
2.5L Benchtop Freeze Dryer
115
60 X
7670521
2.5L Benchtop Freeze Dryer
115
60 X X
7670530
2.5L Benchtop Freeze Dryer
230
50 X
7670531
2.5L Benchtop Freeze Dryer
230
50 X X
7670540
2.5L Benchtop Freeze Dryer
230
60 X
7670541
2.5L Benchtop Freeze Dryer
230
60 X X
7670560
2.5L Benchtop Freeze Dryer
230
50 X
7670561
2.5L Benchtop Freeze Dryer
230
50 X X
7670570
2.5L Benchtop Freeze Dryer
230
50 X
7670571
2.5L Benchtop Freeze Dryer
230
50 X X
7670020
2.5L Benchtop Cascade Freeze Dryer
115
60 X
7670021
2.5L Benchtop Cascade Freeze Dryer
115
60 X X
7670030
2.5L Benchtop Cascade Freeze Dryer
230
50 X
7670031
2.5L Benchtop Cascade Freeze Dryer
230
50 X X
7670040
2.5L Benchtop Cascade Freeze Dryer
230
60 X
7670041
2.5L Benchtop Cascade Freeze Dryer
230
60 X X
7670060
2.5L Benchtop Cascade Freeze Dryer
230
50 X
7670061
2.5L Benchtop Cascade Freeze Dryer
230
50 X X
7670070
2.5L Benchtop Cascade Freeze Dryer
230
50 X
7670071
2.5L Benchtop Cascade Freeze Dryer
230
50 X X
7420020
2.5L Console Cascade Freeze Dryer
115
60 X
7420021
2.5L Console Cascade Freeze Dryer
115
60 X X
7420030
2.5L Console Cascade Freeze Dryer
230
50 X
7420031
2.5L Console Cascade Freeze Dryer
230
50 X X
7420040
2.5L Console Cascade Freeze Dryer
230
60 X
7420041
2.5L Console Cascade Freeze Dryer
230
60 X X
7420060
2.5L Console Cascade Freeze Dryer
230
50 X
7420061
2.5L Console Cascade Freeze Dryer
230
50 X X
7420070
2.5L Console Cascade Freeze Dryer
230
50 X
7420071
2.5L Console Cascade Freeze Dryer
230
50 X X
Part #
Component Description
7426100
User’s Manual
1291000
Plug (230V models only)
7373450
Vacuum Hose
1488800
Hose Clamps (2)
7395801
Chamber Lid
7395800
Lid Gasket
7419300
Baffle (Cascade Models Only)
7386901
Fitting
Plus the following:
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
11
!
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.
Component Orientation
The refrigeration system in the Freeze Dryer draws air in through the rear of the
cabinet and exhausts air out through the sides. A minimum of 3" should be
allowed between the back and sides of the Freeze Dryer and the adjacent wall
surface. Restriction of the airflow through the cabinet during operation could
adversely affect performance.
After the console model is positioned at the location where it will be operated, it
should be securely attached to the floor. Use (2) 1/4" x 5.0 long wood screws or
lag bolts if the floor is wood or concrete anchors if the floor is concrete. Two .312
diameter holes are located in the floor of the lower cabinet. Using these holes as a
template, mark the floor directly under the two holes. Roll the Console Freeze
Dryer aside and drill suitable pilot holes for the selected screws/anchors. Install the
vacuum pump prior to securing the Console Freeze Dryer to the floor. Roll the
Console Freeze Dryer back into position and install the screws/anchors through the
holes in the cabinet floor and into the building floor.
FAILURE TO ATTACH THE CONSOLE FREEZE DRYER TO
THE FLOOR COULD RESULT IN ACCIDENTAL TIPPING
AND POSSIBLE INJURY
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 the collector chamber to the vacuum
pump.
Make certain that the oil in the vacuum pump is at the proper
level.
Place the vacuum pump near the benchtop Freeze Dryer models. For console
models, from the back of the unit, place the vacuum pump on the floor of the
cabinet.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
12
TO MAXIMIZE THE STABILITY OF THE CONSOLE FREEZE
DRYER, POSITION THE VACUUM PUMP AS CLOSE TO THE
CENTER OF THE CABINET FLOOR AS POSSIBLE.
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.
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.
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:
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Chapter 3: Getting Started
13
Acids
Buffers Solvents
Component
Material
Acetic Acid 20%
Formic Acid
Trifluoroacetic Acid (TFA) Calcium Chloride
Sodium Phosphate 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.
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Chapter 3: Getting Started
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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.
With prudent maintenance the FreeZone Freeze Dry System 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 816-3338811 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
15
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CHAPTER 4
USING YOUR FREEZE DRYER
After your Freeze Dryer has been installed as detailed in Chapter 3: Getting
Started, you are ready to begin using your Freeze Dryer. Read this chapter to learn
how to:
operate the controls.
understand the display.
connect samples.
Do not use the Freeze Dryer in a manner not specified by the
manufacturer (refer to Appendix C: Freeze Dryer
Specifications). The electrical protection properties of the
Freeze Dryer may be impaired if the Freeze Dryer is used
inappropriately.
Product Service 1-800-522-7658
Chapter 4: Using Your Freeze Dryer
16
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4
7
9
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11
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Freeze Dryer Controls
The control panel for the Freeze Dryer is shown below with a description about its
function.
1. LCD Display – Displays system operating parameters, set-up parameters and
alarm messages.
2. Menu Switch – This switch is used to change the display from operating
system parameters to set-up parameters.
3. Select Switch – Used to select set-up parameters.
4. Vacuum Switch – Used to start or stop the vacuum pump when operating in manual
start-up mode.
5. Vacuum Indicator – This green LED indicates that power is being supplied to the
vacuum pump receptacle on the back of the Freeze Dryer.
6. Manual Refrigeration Switch – Used to start only the refrigeration module.
7. Manual Operation Indicator – When lit, the green LED indicates the Freeze Dryer is
being controlled manually by the operator. Each function must be started by the
operator.
8. Auto Mode Switch – Used to start or stop the refrigeration and the Auto Mode process.
9. Auto Mode Indicator – When lit, the green LED indicates that the Freeze Dryer is in
Auto Mode. In this mode, the vacuum pump will start when the collector temperature
reaches –40°C.
10. Vacuum Graph Display – This display indicates the relative system vacuum level. The
highest LED indicates that the vacuum level is above 2.0 mBar. The indicators will
sequence down when the vacuum level reaches 2.0, 1.0, 0.8, 0.6, 0.45, 0.12 mBar. The
lower green LED flashes when the system vacuum level is 0.45 to 0.12 mBar and
illuminates steadily below 0.133 mBar.
Product Service 816-333-8811 or 1-800-522-7658
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