Labconco FreeZone 70020 Series User manual

FreeZone®Benchtop
Freeze Dryers
User's Manual
Please read the User’s Manual before operating the equipment.
LABCONCO CORPORATION
8811 Prospect Avenue
Kansas City, MO 64132
[phone], [phone]
(816) 363 -0130 fa x
[e-mail]
Models
70020**** 2.5L -50°C Series
71020**** 2.5L -84°C Series
70040**** 4.5L -50°C Series
71040**** 4.5L -84°C Series
72040**** 4.5L -105°C Series
70080**** 8L -50°C Series
T
o receive important product updates,
complete your product registration card
online at register.labconco.com

Original instructions
Copyright © 2017 Labconco Corporation. 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 7:30 a.m. and 5:30 p.m., Central Standard Time.
Part #7343000, Rev. A
ECO K623
Warranty
Labconco Corporation provides a warranty to the original buyer for the repair or replacement of parts and
reasonable labor as a result of normal and proper use of the equipment with compatible chemicals. Broken
glassware and maintenance items, such as filters, gaskets, light bulbs, finishes and lubrication are not
warranted. Excluded from warranty are products with improper installation, erratic electrical or utility supply,
unauthorized repair and products used with incompatible chemicals.
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.
Buyer is exclusively responsible for the set-up, installation, verification, decontamination or calibration of
equipment. This limited warranty covers parts and labor, but not transportation and insurance charges. If the
failure is determined to be covered under this warranty, the dealer or Labconco Corporation will authorize
repair or replacement of all defective parts to restore the unit to operation. Repairs may be completed by 3rd
party service agents approved by Labconco Corporation. Labconco Corporation reserves the rights to limit this
warranty based on a service agent’s travel, working hours, the site’s entry restrictions and unobstructed access
to serviceable components of the product.
Under no circumstances shall Labconco Corporation be liable for indirect, consequential, or special damages
of any kind. This warranty is exclusive and in lieu of all other warranties whether oral, or implied.

Original instructions
TABLE OF CONTENTS
CHAPTER 1: INTRODUCTION 1
Intended Use 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
CHAPTER 2: PREREQUISITES 6
Electrical Requirements 6
Location Requirements 7
Vacuum Pump Requirements 7
Chamber or Manifold Requirements 7
CHAPTER 3: GETTING STARTED 8
Unpacking Your Freeze Dryer 8
Freeze Dryer Components 9
Setting Up Your Freeze Dryer 9
Component Identification 10
Vacuum Pump Connection 11
Electrical Connection 12
Baffle Installation 12
Drying Chamber or Manifold Installation 13
Chemical Resistance of Freeze Dryer Components 14
Solvent Safety Precautions 16
CHAPTER 4: LYO-WORKS™OPERATING SYSTEM 17
Control Panel 18
Initial Power Up 18
Touch Screen Operation 19
Home screen 19
Main Menu Icons 19
Moving between Menu Screens 19
Function Indicator Bar 19
System Parameters Display 20

Original instructions
Operation Buttons (Auto, Collector, Vacuum) 21
Programs screen 21
Data Logging screen 23
Settings screen 24
Language 24
Time & Date 25
Units 25
Security 25
Alerts 26
Configure Email Settings 27
Maintenance 28
Vacuum Pump Settings 28
Refrigeration System Settings 29
Freeze Dryer Line Voltage Offset 29
Calibration 29
Display 30
Network 31
Sensors screen 32
Drying Accessory screen 32
End Point Detection screen 33
Help screen 34
Diagnostics 34
User’s Manual 35
About 35
CHAPTER 5: USING YOUR FREEZE DRYER 36
Operation Checklist 36
Vacuum Pump Ballast Setting 37
Operating the Freeze Dryer 37
Auto Start-Up 37
Manual Start-Up 37
Setting the Operating Vacuum Level 37
Pre-Freezing Samples 38
Adding Sample 39
Starting a Program 40
Shut Down 40
Defrosting 40
Alerts 41
Copy (export) a Data Log File 43
Download a Data Log File via Ethernet 43
Copy a Program 44
CHAPTER 6: MAINTAINING YOUR FREEZE DRYER 45
Service Safety Precautions 45
Routine Maintenance Schedule 45
CHAPTER 7: TROUBLESHOOTING 47
Vacuum Pump 47

Original instructions
Gaskets, Tubing, Connections, Sample Valves 48
System Components & Collector Chamber Isolation 50
Refrigeration Module Operation 52
APPENDIX A: FREEZE DRYER COMPONENTS 53
APPENDIX B: FREEZE DRYER DIMENSIONS 60
APPENDIX C: FREEZE DRYER SPECIFICATIONS 63
Electrical Specifications 63
Environmental Conditions 64
APPENDIX D: FREEZE DRYER ACCESSORIES 65

Product Service 816-333-8811 or 1-800-522-7658
1
Original instructions
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 HCFC-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.
Intended Use
The Labconco Freeze Dryers described in this manual are intended for laboratory
use to facilitate the lyophilization process.
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.

Chapter 1: Introduction
Product Service 816-333-8811 or 1-800-522-7658
2
Original instructions
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
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.
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
Table 1

Chapter 1: Introduction
Product Service 816-333-8811 or 1-800-522-7658
3
Original instructions
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.

Chapter 1: Introduction
Product Service 816-333-8811 or 1-800-522-7658
4
Original instructions
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: Lyo-Works Operating System describes the display screens and user
interface software that controls the Freeze Dryer.
Chapter 5: 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 6: Maintaining Your Freeze Dryer explains how to perform routine
maintenance on your Freeze Dryer.
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.

Chapter 1: Introduction
Product Service 816-333-8811 or 1-800-522-7658
5
Original instructions
Appendix B: Freeze Dryer Dimensions contains diagrams showing the dimensions
for the Freeze Dryer.
Appendix C: Freeze Dryer Specifications contains product specifications.
Appendix D: Freeze Dryer Accessories see www.labconco.com for a complete list
of Freeze Dry accessories.
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.

!