Labconco 7752020, 7752021, 7752030, 7752031, 7752040 User guide

FreeZone Legacy™ 6 Liter

Benchtop Freeze Dry Systems

Models

77520 Series

Copyright © 2018 Labconco Corporation. The information contained in this manual and the accompanying

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.

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 #7400209, Rev. H

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CHAPTER 1: INTRODUCTION 1

Freeze Dry Process 1
Freeze Dry Rates 1
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 10

Vacuum Pump Connection 10
Electrical Connection 10
Drying Chamber or Drying Manifold Installation 10
Chemical Resistance of Freeze Dryer Components 11

Solvent Safety Precautions 12

CHAPTER 4: USING YOUR FREEZE DRYER 13

Freeze Dryer Controls 14
Operation Checklist 15
Vacuum Pump Ballast Setting 15
Operating the Freeze Dryer 15

Set-Up 15
Automatic Start-Up 18

Manual Start-Up 18
Setting the Operating Vacuum 18
Pre-Freezing Samples 19
Adding Sample 19
Shut Down 21

Defrosting 21
Alarms 22

Power Failure 22
Line Voltage Out of Range 22
Temperature Out of Range 23
Service Vacuum Pump 23
Moisture in Collector 23

CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 24

CHAPTER 6: USING THE RS232 RECEPTACLE 26

Computer Connection for Computer Interface 26

CHAPTER 7: TROUBLESHOOTING 31

Vacuum Pump 31
Gaskets, Tubing, Connections, Sample Valves 32
System Components & Collection Chamber Isolation 34
Refrigeration Module Operation 36

CHAPTER 8: MODIFYING YOUR FREEZE DRYER DISPLAY 37

Temperature and Vacuum Display 37
Line Voltage Alarm Points 37
Moisture Sensor Alarm 38
Modifying the Display 38

APPENDIX A: FREEZE DRYER COMPONENTS 42

APPENDIX B: FREEZE DRYER DIMENSIONS 45

APPENDIX C: FREEZE DRYER SPECIFICATIONS 46

Electrical Specifications 46
Environmental Conditions 47

APPENDIX D: FREEZE DRYER ACCESSORIES 48

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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.

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.

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.

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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

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
efficient rate. In many applications, the maintenance of a vacuum of 0.133 mBar
or less is recommended.

Product Service 816-333-8811 or 1-800-522-7658

Chapter 1: Introduction

3

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
can be used between the collector and the vacuum pump.

Product Service 816-333-8811 or 1-800-522-7658

Chapter 1: Introduction

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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 describes how to calibrate the
vacuum display and restore factory settings.

Product Service 816-333-8811 or 1-800-522-7658

Chapter 1: Introduction

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

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.

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.

Refer to Chapter 7: Troubleshooting if you are experiencing problems with your
Freeze Dryer.

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Before you install your Freeze Dryer, you need to prepare your site for installation.
Carefully examine the location where you intend to install your Freeze Dryer. You
must be certain that the area is level and of solid construction. An electrical source
must be located near the installation site.

Carefully read this chapter to learn:

 the electrical supply requirements.
 the vacuum pump requirements.

Refer to Appendix C: Freeze Dryer Specifications for complete Freeze Dryer
electrical and environmental conditions, specifications and requirements.

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 is equipped with a 20 Amp NEMA 5-20P
plug. Various power cord configurations are provided with 230V models. If this
does not match with the available receptacle, remove this plug and replace it with
an approved plug of the suitable style.

Product Service 1-800-522-7658

Chapter 2: Prerequisites

7

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 in through the rear and exhausts it through the sides. A minimum
of 3" must be allowed between the rear 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 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 98 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 an 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 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

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The United
States
Interstate
Commerce
Commission
rules require
that claims be
filed with the
delivery
carrier within
fifteen (15)
days of
delivery.



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 6 Liter Benchtop Freeze Dry System weighs over
135 lbs. 61 kg). If you must lift the Freeze Dryer manually, use
at least two (2) persons and follow safe lifting guidelines.

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.

Product Service 1-800-522-7658

Chapter 3: Getting Started

9

Power Cords

Catalog #

Description

Volts

Hz

PTFE

Coated

Chamber

1336400 1336500 1342100 1332601 1332701

7752020

6 Liter Benchtop Freeze Dryer

115

60 X

7752021

6 Liter Benchtop Freeze Dryer

115

60 X X

7752030

6 Liter Benchtop Freeze Dryer

230

50 X

7752031

6 Liter Benchtop Freeze Dryer

230

50 X X

7752040

6 Liter Benchtop Freeze Dryer

230

60 X

7752041

6 Liter Benchtop Freeze Dryer

230

60 X X

7752060

6 Liter Benchtop Freeze Dryer

230

50 X

7752061

6 Liter Benchtop Freeze Dryer

230

50 X X

7752070

6 Liter Benchtop Freeze Dryer

230

50 X

7752071

6 Liter Benchtop Freeze Dryer

230

50 X X

Part #

Component Description

7400209

User’s Manual

1291000

Plug (230V models only)

7373450

Vacuum Hose

1488800

Hose Clamps (2)

7532900

Chamber Lid

7690800

Lid Gasket





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.

Plus the following:

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.

Product Service 816-333-8811 or 1-800-522-7658

Chapter 3: Getting Started

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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 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.

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 port on the top of the Freeze Dryer. Follow the
instructions supplied with the selected accessory.

Product Service 816-333-8811 or 1-800-522-7658

Chapter 3: Getting Started

11

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

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:

*An accessory glass lid is available.
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.

Product Service 816-333-8811 or 1-800-522-7658

Chapter 3: Getting Started

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 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. This is accomplished by closing all sample
valves on a clean, dry freeze dry system and turning on the vacuum pump. If
the pump is operated at an elevated vacuum level (> 10mBar), oil may be
expelled from the pump and damage could occur.

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: [e-mail].

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

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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

14

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12

8 6 3

11

5 2 10

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. The operator must start each function.

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.

11. Collector Temperature Graph Display – This display indicates the temperature of the

collector. The highest LED indicates the collector temperature is warmer than 10°C.

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Chapter 4: Using Your Freeze Dryer

15

The indicators will sequence down when the temperature reaches 10, 0, -10, -20, -30, ­40°C. When the collector temperature is –40°C or lower the green indicator will light.

12. Alarm Indicator – This red LED indicates that a system alarm has occurred. Press the

Menu Switch to display the alarm message on the LCD display.

13. Main Power Switch – Turns the Freeze Dryer on or off. (Not shown, located on the left

side of the cabinet.)

Operation Checklist

The following checklist should be followed prior to each use of your Freeze Dryer:

1. Wipe the interior of the collector chamber with a soft cloth or paper towel to

remove any accumulated moisture.

2. Check the collector chamber drain hose to ensure that the hose is free of

moisture and that the drain plug is securely installed. The Freeze Dryer will
not start if moisture is detected.

3. Using a soft, lint-free cloth or paper towel, wipe the collector chamber lid

gasket to remove any dirt and contaminants that could cause a vacuum leak.
Vacuum grease is not required on the lid gasket to obtain a proper vacuum seal.

4. Remove the accessory drying chamber or manifold from the connection port

and using a soft, lint-free cloth or paper towel, wipe the port gasket and sealing
surfaces of the drying chamber/manifold to remove any dirt and contaminants
that could cause a vacuum leak. Reinstall the drying chamber or manifold on
the port. Vacuum grease is not required on the port gasket to obtain a proper
vacuum seal.

5. Inspect each sample valve on the accessory drying chamber or manifold and

check for any visible damage and for improper installation that might cause a
vacuum leak. Also check that each sample valve is closed or in the “vent”
position.

Vacuum Pump Ballast Setting

Most vacuum pumps are equipped with a gas ballast mechanism. The freeze dry
process requires high vacuum. Therefore, it is recommended that the gas ballast be
closed during the operation of the Freeze Dry System. If the gas ballast is left
open for extended periods of operation, the oil can be pumped out the exhaust,
causing the pump to fail.

Operating the Freeze Dryer

Set-Up

The Freeze Dryer may be configured to automatically start the vacuum pump when
the collector temperature reaches –40°C. The display units for vacuum may be
selected to be mBar, Pascal (Pa) or Torr and the temperature may be displayed as
°F or °C. The run time of the refrigeration system and the vacuum pump may be
monitored.

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Chapter 4: Using Your Freeze Dryer

16

VACUUM UNITS

mBar Pa Torr

TEMPERATURE UNITS

°C °F

REFRIG TOTAL HOUR: XXXX
SERVICE HOUR: XXXX

VACUUM SET POINT

XXXX YYY

To configure your Freeze Dryer, turn the main power switch ON and press MENU.
The display will show:

 Press SELECT until the desired units are flashing.
 Press MENU.
 The display will show:

Where YYY is the units selected above.

 Press SELECT until the desired vacuum operating level is displayed. See

“Setting the Operating Vacuum Level” for guidelines

 If “O” is selected, the vacuum control is disabled and the vacuum level in

the Freeze Dry System will be determined by the capabilities of the
vacuum pump.

 Press MENU.
 The display will show:

 Press SELECT until the desired units are flashing.
 Press MENU.
 The display will show:

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Chapter 4: Using Your Freeze Dryer

17

REFRIG TOTAL HOUR: XXXX
RESET SERVICE HOUR: ?

VACUUM TOTAL HOUR: XXXX
SERVICE HOUR: XXXX

RS-232 TRANSMISSION RATE

10 SECONDS

VACUUM TOTAL HOUR: XXXX
RESET SERVICE HOUR: ?

 To reset the SERVICE HOUR to 0 press SELECT. This allows you to

keep track of the time the refrigeration system operated since it was
serviced.

 The display will show the refrigeration system hours.

 To reset the service hours to 0, continue to hold SELECT 5 seconds until

hours are reset.

 TOTAL HOUR cannot be reset.
 Press SELECT.
 The display will show the vacuum pump hours.

 To reset the SERVICE HOUR to 0, press SELECT.
 The display will show:

If you want to reset the service hours to 0, continue to hold SELECT five seconds
until hours are reset.

 Press SELECT.
 The display will show the RS-232 data transmission rate.

 To change the rate press SELECT until the desired time interval is shown.

The time between data transmissions may be set to occur at 10, 30, 60, 300
or 600 second intervals.

 Press MENU to return to display operating parameters or after a short

delay, the display will automatically switch to show operating parameters.

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Chapter 4: Using Your Freeze Dryer

18

Automatic Start-Up

To run the Auto Mode, press the panel switch labeled REFRIGERATION AUTO.
The green LED above the switch will illuminate. This will start the refrigeration
system. When the collector reaches –40°C, the vacuum pump will start. The
Temperature and Vacuum Graphs will indicate collector temperature and system
vacuum. The LCD display will show the actual temperature of the collector.
When the vacuum in the system is above 5 mBar the vacuum display will indicate
“HI.” At 5 mBar and below, the display will show the actual vacuum.

When the system vacuum is between 0.450 and 0.133 mBar, the lower green
vacuum graph LED will flash. When the system vacuum level is <0.133 mBar, the
green LED will be lit steadily indicating that most samples may be added.

Manual Start-Up

To manually run the freeze dry process, press the REFRIGERATION MAN
switch. This will start the refrigeration system. The green LED above the switch
will illuminate. When the collector temperature reaches –40°C, the vacuum pump
may be started by pressing the VACUUM switch. The Temperature and Vacuum
Graphs will indicate collector temperature and system vacuum. The LCD display
will show the actual temperature of the collector. When the vacuum in the system
is above 5 mBar the vacuum display will indicate “HI.” At 5 mBar and below, the
display will show the actual vacuum.

When the system vacuum is between 0.450 and 0.133 mBar, the lower green
vacuum graph LED will flash. When the system vacuum level is <0.133 mBar, the
green LED will be lit steadily indicating that samples may be added.

Setting the Operating Vacuum Level

The vacuum level may be set by the user to optimize the freeze dry process.
Normally, the sublimation rate will increase if there is less vacuum (a higher
pressure) in the Freeze Dryer. A good starting place is to set the vacuum so its
level is equivalent to about 10°C colder than the eutectic or collapse temperature
of the sample. Adjustments to the vacuum level must be made for various freeze
drying conditions. Factors that must be considered are whether the sample is
freeze dried on heated shelves or in glassware attached to manifold valves, the
volatility of the sample itself, the size of the sample and the heat energy supplied
to the sample.

When the vacuum control is set to operate at less vacuum, the ice holding capacity
of the collector may be decreased. This can be improved by installing a baffle in
the collector. See Appendix D Freeze Dryer Accessories for the baffle part
number. Position the baffle so it rests on the top of the collector coil. The arrow
should point toward the front.

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Chapter 4: Using Your Freeze Dryer

19

Material

Solidification/Eutectic

Temperature

Pre-Freeze

Temperatures

Vacuum Set Point

Bacteria,Virus

-40°C and Colder

-50°C &
Colder

0.040 mBar &
Lower

Milk

-5 to -13

-15 to -23

1.65 to 0.77

Fungi

-40 and Colder

-50 & Colder

0.04 and lower

Vegetable Tissue

-25 to -50

-35 to -60

0.22 to 0.01

Human Tissue

-30 to –40

-40 to –50

0.12 to 0.04

Blood Plasma

-10 to –25

-20 to –35

1.03 to 0.22

Vaccine

-30 to –40

-40 to –50

0.12 to 0.04

Some guidelines for setting the Freeze Dryer are shown below. These show pre­freezing temperatures and vacuum levels. Exact protocols must be determined by
the user for the specific samples that are being freeze dried.

Pre-Freezing Samples

Appropriate containers for freeze drying include ampules, serum bottles, and wide
mouth freeze drying flasks. Shell freezing of samples is recommended for wide
mouth freeze drying flasks. Smaller samples in ampules and serum bottles may be
frozen in a freezer. The sample container size should always be at least two to
three times the sample size (i.e., 40 ml samples should be prepared in 80 ml
containers or larger). The temperature required for pre-freezing is dependent on
the characteristics of the sample. Pre-freezing temperature typically is at least 10°
to 20°C below the eutectic or collapse temperature of the sample.

Adding Sample

The following procedure should be followed when using sample valves in the
freeze dry process:

1. Connect a pre-frozen sample to a sample valve on the drying chamber or manifold

using an adapter. Turn the plastic valve knob to the “VACUUM” position to open

the valve. The bevel on the knob should be positioned toward the sample port to
apply vacuum to the sample.

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Chapter 4: Using Your Freeze Dryer

20

Vent/Backfill Port

Bevel in “vent” position

Bevel in “vacuum”

position

Adapter

2. Before adding another sample, allow system vacuum to return to 0.133 mBar

or lower. Any combination of valves and sample sizes may be utilized at one
time provided that the system vacuum and collector temperature remain
sufficiently low to prevent melting of the frozen sample.

3. When all the frost has disappeared from the outer surface of the sample

container and no cold spots can be detected by handling the container, the
sample is nearly dry. To be certain of low final moisture content, dry the
sample for several hours past this point.

4. To remove a container after drying is complete, turn the plastic knob on the

valve to the “VENT” position, which closes the valve and vents the container.
Should backfilling with an inert gas be required, connect the gas supply line to
the vent port on the valve before turning the plastic knob on the valve to vent
position. The sample container may now be removed. In the vent position the
bevel on the valve knob should point away from the sample port.

5. Ampules may be flame sealed while connected to a valve by using a sealing

torch. Care must be taken not to burn the valve. An insulation material placed
between the valve and the torch is recommended.

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Chapter 4: Using Your Freeze Dryer

21

!

Shut Down

At the end of a run or when a sufficient amount of condensate accumulates on the
collector coil to obstruct the flow of vapor to the collector chamber, the Freeze
Dryer should be defrosted. First, release system vacuum by turning the plastic
knob on a valve to the open position or by pulling the collector chamber drain plug
out of the drain hose. Now press the Vacuum Switch on the control panel to turn
the vacuum pump OFF. Press the Refrigeration Switch next to the illuminated
LED to turn OFF the refrigeration system. Turn OFF the Main Power Switch on
the left hand side of the cabinet.

Defrosting

The following procedure should be followed when defrosting the collector coil:

1. Pull the collector chamber drain hose out from the right hand side of the Freeze

Dryer and remove the drain plug. Place the drain hose in a suitable container
to collect the condensate that will melt off the collector coil.

2. Remove the collector chamber lid and allow ambient room air to melt the ice.

Dispose of the liquid appropriately.

3. Flush the collector chamber with water and wipe chamber dry.

4. If rapid defrost is desired, pour warm water over the collector coil. Do not

allow the liquid to enter the vacuum port on the upper rear of the chamber.

5. Reinstall the drain hose plug and slide drain hose back into the side of the

cabinet. Dispose of the liquid appropriately.

Utilization of acid requires immediate cleaning and
neutralization after defrost or physical damage to the collector
chamber and collector coil will result.

Do not attempt to chip ice from the collector coil as damage
may occur to the coil.

Never attempt to start the vacuum pump when there is liquid in
the collector chamber. This could result in damage to the
vacuum pump.

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Chapter 4: Using Your Freeze Dryer

22

POWER FAIL
HOLD SELECT TO CLEAR IT

LINE VOLTAGE ERROR

Alarms

A number of unusual events may occur during a lyophilization procedure that can
adversely affect the operation of the Freeze Dryer. If an event occurs, the alarm
indicator will flash and the beeper will sound.

The beeper will automatically mute itself after one minute. The specific alarm can
be identified by pressing MENU. Pressing MENU multiple times will display

multiple alarms if they have occurred. The following “out of specification”

conditions will initiate an alarm.

Power Failure

If a power failure occurs during a Freeze Dry process, the vacuum control valve
will allow air to bleed into the Freeze Dryer System. If the failure is of a short
duration and the collector does not warm up excessively, when power is restored
the Freeze Dryer will restart and resume operation of the refrigeration and vacuum
systems. If the power failure lasts for a longer duration and the collector warms
above safe limits, when the power is restored, the Freeze Dryer will not
automatically restart. This prevents melted sample from being drawn into the
collector and prevents liquid from being sucked into the vacuum pump.

When power is restored, the alarm indicator will flash and the alarm beeper will
sound. When the MENU button is pressed the display will show:

Press and hold SELECT for five seconds until the error message is cleared from
the display.

Line Voltage Out of Range

If the voltage supplied to the Freeze Dryer varies beyond allowable limits, the
alarm will be activated. When an alarm occurs, press MENU and the display will
show:

The alarm will self-cancel when the proper voltage is restored. The high and low
alarm points are preset at the factory to correspond to the normal allowable voltage
variations based on the nominal voltage specified for the freeze dryer. Some
models may be operated outside the normal voltage limits. See Appendix C. If
necessary, the high and low alarm points may be adjusted for these models. See

Chapter 8.

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Chapter 4: Using Your Freeze Dryer

23

COLLECTOR TEMPERATURE
HOLD SELECT TO CLEAR IT

CHANGE VACUUM OIL
HOLD SELECT TO CLEAR IT

MOISTURE IN COLLECTOR

Temperature Out of Range

An alarm will be activated if the collector temperature rises above –40°C. If this
occurs, the display will show:

Press and hold SELECT for five seconds until the error message is cleared from
the display.

Service Vacuum Pump

The vacuum pump normally plugs into the vacuum pump electrical receptacle on
the back of the Freeze Dryer. When the Freeze Dryer has accumulated a total of
1000 operating hours, the alarm indicator will flash. Press MENU to display the
alarm:

Press and hold SELECT for five seconds until the error message is cleared from
the display.

This will reset the 1000 hour timer. It may be necessary to service the vacuum
pump more frequently than every 1000 hours depending on the operation of the
Freeze Dryer. The pump oil should be regularly monitored to verify that it is
clean.

Moisture in Collector

If there is liquid in the collector chamber and either a REFRIGERATION button or
the VACUUM button is pressed, neither function will start and an alarm will be
activated. When MENU is pressed, the display will show:

When the collector is drained, the alarm will self-cancel.

This feature prevents the inadvertent start of the vacuum pump when liquid is in
the collector and thereby can extend the life of the vacuum pump. A few drops of
liquid may remain in the drain hose after draining. When the vacuum pump is
started these drops may be sucked into the collector chamber. This is normal.

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24

C

C

HHAAPPTTEERR

5

5

M

M

AAIINNTTAAIINNIINNG

G

Y

Y

OOUURR

F

F

RREEEEZZE

E

D

D

RRYYEERR

Under normal operation, the Freeze Dryer requires little maintenance. The
following maintenance schedule is recommended:

As needed:

1. Clean up all spills; remove liquids from the chamber.

2. Clean lid and gasket using soft cloth, sponge or chamois and a mild, non-

3. Check oil level of the vacuum pump. It should be between MIN and MAX. If

4. If oil shows cloudiness, particles or discoloration, drain the pump and replace

5. Utilization of acids requires immediate cleaning and neutralization after a

6. Check the collection chamber for condensed or frozen solvents and dispose of

7. If sample valves leak or stems become difficult to turn, pull the stem out of the

abrasive soap or detergent.

the oil level is less than an inch (25.4 mm) above MIN, add oil to proper level.

with fresh oil.

run or physical damage to the collector chamber and collector coil will
result.

appropriately. Completely empty the collector chamber before the next run or
before attempting to start the vacuum pump.

rubber valve body and apply a thin coat of vacuum grease to the stem.
Reinsert the stem into the valve body.

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Chapter 5: Maintaining Your Freeze Dryer

25

Monthly:

1. The rubber components on the Freeze Dryer may eventually deteriorate and

require replacement. The effective life of rubber parts depends upon both their
usage and the surrounding environment. Check all rubber hoses and gaskets
and replace any that show signs of hardening, permanent set or deterioration.

2. Using a soft cloth, sponge or chamois and a mild, non-abrasive soap or

detergent, clean the acrylic chamber lid.

3. Using a soft cloth, sponge, or chamois and a mild, non-abrasive soap or

detergent, clean the exterior surfaces of the Freeze Dryer. Liquid spray
cleaners and polishes may be used on the exterior surfaces. Do not use
solvents to remove stains from the exterior surfaces as they may damage the
finish.

Annually:

1. Every 12 months, or more often if the Freeze Dryer is operated in a dusty

environment, the refrigeration system condenser should be cleaned. Using a
vacuum cleaner with brush attachment, clean the condenser to ensure proper
airflow for peak performance.

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26

C

C

HHAAPPTTEERR

6

6

U

U

SSIINNGG

T

T

HHEE

R

R

S

S

2

2

3

3

2

2

R

R

EECCEEPPTTAACCLLE

E

The operation of the Freeze Dryer can be monitored using a computer when it is
connected to the RS232 receptacle on the rear panel. The computer cannot control
the operation of the Freeze Dryer. The monitored parameters are the collector
temperature in °C and vacuum in microbars.

When a Labconco Stoppering Tray Dryer is connected to a Labconco Freeze Dryer

as detailed in the Stoppering Tray Dryer User’s Manual, the status of the

Stoppering Tray Dryer may be monitored simultaneously with the status of the
Freeze Dryer.

Computer Connection for Computer
Interface

Check your computer to see which type of serial port is provided, then use a
connecting cable below:

1. Computers with a 25 pin D-sub male serial connector should use Connect

Cable, Labconco part number 7537801, to connect a computer to the
Labconco Freeze Dryer.

2. Computers with a 9 pin D-sub male serial connector should use Connect

Cable, Labconco part number 7537800, to connect a computer to the
Labconco Freeze Dryer.

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Chapter 6: Using the RS232 Receptacle

27

RS-232 TRANSMISSION RATE

10 SECONDS

The purpose of the RS232 interface is to send data to a data logging computer to
monitor the state and activity of the Freeze Dryer. This data is half duplex data.
The data properties are as follows:

1. Data Rate 2400 Baud

2. 8 Bit word length

3. 1 Start bit, 1 Stop bit

4. No parity is transmitted

5. Standard ASCII character set

The time between data transmissions may be varied by the user to occur at 10, 30,
60, 300 or 600 second intervals. Press the MENU button until the RS232 screen
appears on the display.

Press select until the desired time interval is shown.

The format of the transmitted message is as follows:

B<T= -48 V= 18 SF = 999 C=999 PG=9 >

Where:

B = Base Unit
T = Collector Temperature

-48 = Collector Temperature in °Celsius
V = Vacuum
18 = Vacuum Level in Micro Bars
SF = Shell Freezer Temperature (not available on 6L

Benchtop models)
9 = Feature not installed or out of range
C = Vacuum Chamber Temperature (not available on
6L Benchtop models)
PG = Purge (not available on 6L Benchtop models)

If a Stoppering Tray Dryer is attached to the Freeze Dryer and the data
interconnect cable is installed, additional data about that accessory will be
transmitted from the Freeze Dryer. See the User’s Manual for the Stoppering Tray
Dryer for a description of the data.

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Chapter 6: Using the RS232 Receptacle

28

There are several commercially available software packages, which can read
RS232 data and enter the data into a computer program such as a word processor
(to create a text file) or spreadsheet (to tabulate and plot the data). Consult your
laboratory supply dealer regarding the latest software available. The following

describes how to use an IBM compatible computer with Hyper Terminal™

software (included with Windows® 95, 98, XP or 2000 operating systems) to
collect the RS232 data from your Freeze Dryer:

1. Make sure that the Freeze Dryer is properly connected to the communication

port on the computer.

2. Open Hyper Terminal™ software.

i)Windows® 95 or 98 use:

START/PROGRAMS/ACCESSORIES.

ii) Windows® 2000 or XP use:

START/PROGRAMS/ACCESSORIES/COMMUNICATIONS

The first time Hyper Terminal™ is opened a dialogue box requesting an area

code and phone number will appear. Enter the appropriate numbers and
continue.

3. The “Connection Description” dialogue box will open. Type in a user defined

name and select an icon for the new connection. Press “OK.”

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Chapter 6: Using the RS232 Receptacle

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4. The “Connect To” dialogue box will open. Using the down arrow selection

button, select the communication port to which the cable has been connected.
Press “OK.”

5. The “Com X Properties” dialogue box will open. Enter the appropriate data

properties and press “OK.”

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Chapter 6: Using the RS232 Receptacle

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6. When the Freeze Dryer main power switch is on, the data will be transmitted

and updated at the time intervals selected by the user.

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31

C

C

HHAAPPTTEERR

7

7

T

T

RROOUUBBLLEESSHHOOOOTTIINNG

G

Refer to the following if your Freeze Dryer fails to operate properly. If the
suggested corrective actions do not solve your problem, contact Labconco for
additional assistance.

Labconco Freeze Dry Systems that are clean, dry and without samples attached
should reach a vacuum of 0.133 mBar within 10 minutes and should achieve an
ultimate vacuum of 0.040 mBar within 18 hours when the refrigeration is
operating. If the Freeze Dryer does not obtain a satisfactory vacuum, perform the
following maintenance tests.

I. Vacuum Pump

First make sure that the vacuum pump operates. If it fails to operate, check the
electrical connections of the Freeze Dryer to the power source and then check the
electrical connection of the vacuum pump to the Freeze Dryer. If the vacuum
pump has a power switch, make sure that it is turned on. If the vacuum is not
adequate when the vacuum pump is operating, proceed with the following steps:

1. Check the oil and ensure it is clear and clean. If the oil looks cloudy or has

any particulates, replace the pump oil. Sometimes it may be necessary to
flush the pump with clean oil several times. To flush the pump, run the
pump 5 to 10 minutes to allow the oil to warm up. Drain the oil and refill
with clean oil. Repeat as necessary.

2. Check the oil level in the pump. Ensure it is filled to the correct level.

3. Check vacuum hose connections from the pump to the Freeze Dryer and try

running the unit.

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Chapter 7: Troubleshooting

32

If vacuum problems continue, consider obtaining a second vacuum gauge capable
of reading a vacuum of 0.010 mBar. It is often useful in determining if the
vacuum pump is operating properly and the vacuum sensor reading is accurate.

4. Isolate the pump by disconnecting the vacuum hose from the Freeze Dryer.

Deadhead the pump by inserting the vacuum sensor from a secondary
vacuum gauge into the end of the vacuum hose and observe the vacuum
reading obtained. Confirm that the pump is capable of achieving an
ultimate vacuum less than 0.010 mBar or approximately 10 microns. If an
inadequate vacuum reading is obtained, the pump has most likely failed
and may need to be replaced or rebuilt.

II. Gaskets, Tubing, Connections, Sample Valves

1. Check all sample valves on the drying chamber/manifold and ensure all

valves are closed or in the vent position. Check to ensure all fittings are
tight and sealed properly against the chamber. Inspect valves for cracks or
cuts.

2. Inspect gasket(s) for cracks or defects. Ensure the gasket is clean. Apply a

thin coat of vacuum grease to the gasket. Keep in mind too much vacuum
grease can actually cause leaks.

3. Check the drain line and ensure the drain plug is installed and the tube

appears to be in good condition.

4. Check all rubber vacuum tubing for signs of deterioration or cracking.

5. Check all connections and make sure they are secure and leak tight.

6. When checking the sample valves, pull as much vacuum as possible. If a

vacuum indication is displayed, wiggle or rotate the valves and watch the
gauge for any fluctuations. Fluctuations can indicate a potential vacuum
leak. If the valve seems to be in good condition, remove the valve and
apply a thin coat of vacuum grease to the stem and the outside sealing
surface of the valve body, and reinstall the valve. DO NOT APPLY

VACUUM GREASE TO THE SAMPLE VALVE GASKETS, WHICH
SEAL TO THE WALL OF THE DRYING CHAMBER. If the valve

still seems to be the source of the problem, remove the valve and stopper
the hole with a rubber stopper. Continue checking the other valves.

7. Make sure that the sample valve bulkhead nuts are tight. Either tighten by

hand or use the wrench supplied with chambers. To use the wrench, first
remove the knob and stem assembly and also the valve body. The pins on
the wrench fit into the round holes of the nut. The nut should be snug, but
avoid over-tightening. Replace the valve body, knob and stem assembly.

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Chapter 7: Troubleshooting

33

Thrust Washer

Valve Body

Knob & Stem

Assembly

Trim Ring

Manifold Assembly

Knob & Stem

Assembly

Bulkhead Nut

Gasket
(No grease
required)

Bulkhead

Fitting

Valve Body

Valve Assembly (Manifold)

Valve Assembly (Stainless Steel Chamber)

Knob & Stem

Assembly

Valve Body

The illustrations below show how the sample valve installs on a chamber and a
manifold.

Valve Assembly (Clear Chamber with Valves)

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Chapter 7: Troubleshooting

34

III. System Components and Collection Chamber
Isolation

1. Remove the drying chamber or manifold.

2. Leave the gasket on and turn a large freeze dry flask upside down to cover

the connection port.

3. Start the freeze dryer and observe the vacuum indication. If the vacuum

indication is good, then the problem is in the drying chamber or manifold
and you should return to Section II, Gaskets, Tubing, Connections, Sample
Valves.

The following test allows you to check the pump and the connections from the
pump to the vacuum tube.

1. Place a rubber stopper in the vacuum port in the left side of the collector

chamber and another in the drain port in the bottom.

2. Restart the vacuum system and check your vacuum indication. Insufficient

vacuum indicates a bad pump or a leak in the connections from the pump to
the side of the chamber.

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Chapter 7: Troubleshooting

35

The following test is used to check the collection chamber integrity. The figure
below points out potential areas to locate a leak:

1. Remove the stopper from the side of the chamber and place a freeze dry

flask over the connection port.

2. Fill the collection chamber with approximately 2 inches of water, enough

to cover all fittings. Replace the collection chamber lid and turn on the
vacuum pump. Allow the vacuum pump to run for approximately 5 to 10
seconds. (If the vacuum pump is left on, the water will begin to boil and
the test will not be effective.) Look inside the chamber for any bubbling
while the pump is running and after you shut the pump off.

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Chapter 7: Troubleshooting

36

3. If bubbling is observed around the bulkhead fittings, access the bottom of

the chamber and remove the insulation. Tighten the appropriate fitting by
placing a wrench on the fitting inside the chamber and use a second wrench
to turn the nut on the bottom of the chamber. Be careful not to damage the
evaporator coils or the brazed joints to the refrigeration system. Once the
fitting is tightened, perform the test again. Should the bubbling still be
present, loosen the bulkhead fittings and apply vacuum grease to the O­rings, then reassembly and test.

4. If bubbling was observed on the chamber surface, the chamber must be

replaced. This type of leak cannot be successfully repaired. The leading
cause of a chamber surface leak is corrosive residue left in the chamber
after use.

Refrigeration Module Operation

Under a no-load condition, the FreeZone Single Stage Freeze Dry System can
achieve a collector temperature of –50°C or lower when the system is under
vacuum, within 30 minutes when the vacuum pump is running, depending on
ambient temperature and humidity.

If any repairs are required on the refrigeration module, contact your local
laboratory supply dealer. If your laboratory supply dealer is unable to provide
assistance, please call Labconco. Repairs should only be undertaken by a
competent refrigeration technician or through an authorized Labconco service
agency.

Product Service 816-333-8811 or 1-800-522-7658

37

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Your Freeze Dryer has been carefully calibrated and tested before shipping,
however under certain circumstances it may be necessary to adjust the calibration
of the temperature and/or vacuum display or to modify alarm points. Adjustments
may be necessary if the Freeze Dryer requires service or if it is operating on a line
voltage outside the voltage range at which the alarm was preset. This DOES NOT
mean that the Freeze Dryer may be operated at a voltage outside the ranges shown
in Appendix C.

Temperature and Vacuum Display

An offset may be added to the collector temperature or vacuum display. Use an
accurate traceable reference to compare the readings.

Temperature offset may be varied ±5°C in 1°C increments. Vacuum offset may be
varied ±0.020 mBar in 0.001 mBar increments.

Line Voltage Alarm Points

The Freeze Dryer is designed to alarm if the line voltage varies more than ±10%
from nominal line voltage. Models rated to operate on 115V are preset to alarm if
the voltage drops below approximately 103V or rises above approximately 127V.
Models rated to operate on 230V will alarm if the voltage drops below
approximately 206V or rises above approximately 254V. Some models are
designed to operate below these ranges (see Appendix C). In these cases it is
permissible to lower the low voltage alarm point to prevent nuisance alarms from
occurring.

Low line limit may be lowered in 5 increments of approximately 2 to 3V
increments for 115V models or disabled.

Low line limit may be lowered in 5 increments of approximately 4 to 5V
increments for 230V models or disabled.

Product Service 1-800-522-7658

Chapter 8: Modifying Your Freeze Dryer Display

38

PRODUCTION MENU
MASTER RESET?

COLLECTOR TEMP OFFSET
O C

High line limit may be raised in 5 increments of approximately 2 to 3V
increments for 115V models or disabled.

High line limit may be raised in 5 increments of approximately 4 to 5V
increments for 230V models or disabled.

Moisture Sensor Alarm

The moisture sensor alarm may be disabled. It is shipped enabled as the factory
default setting.

Modifying the Display

To enter an offset or to configure the alarms, perform the following steps:

Press and hold MENU button (approximately 10 seconds) until the display
shows:

It is recommended that you do NOT perform a Master Reset because all
offsets and configurations that have been entered will be lost. If you must
perform a Master Reset, hold SELECT approximately 5 seconds.

This will reset:

Vacuum units to mBar
Vacuum set point to 0 mBar
Temperature units to °C
Refrigeration total hours to 0
Vacuum pump total hours to 0
RS232 transmission rate to 10 seconds
Temperature offset to 0°C
Vacuum offset to 0 mBar
Low line voltage to 0 V offset
High line voltage to 0 V offset
Moisture sensor to enabled
Refrigeration to operate in Manual Mode

The display will default to the main freeze dry display information.

If you do not want to restore all factory settings, but want to adjust offsets, press
MENU briefly and the display will show:

Press SELECT until the appropriate offset is shown. Each number
represents 1°C

Product Service 816-333-8811 or 1-800-522-7658

Chapter 8: Modifying Your Freeze Dryer Display

39

SDC TEMP. OFFSET:
O C

VACUUM OFFSET:
O uBar

LOW LINE OFFSET:
0

HIGH LINE OFFSET:
0

DRYING CHAMBER:
NOT INSTALLED

Press MENU and if the drying chamber has been installed, the display will show:

Press SELECT until the appropriate offset is shown. Each number represents 1°C
Press MENU and the display will show:

Press SELECT until the appropriate offset is shown. Each number
represents 0.001mBar.

Press MENU and the display will show:

Press SELECT until the appropriate offset is shown. If the Freeze Dryer is
operating on nominal 115V, each number represents 2V. If 3 is entered
into the display, the low line alarm will alarm when the voltage drops to
approximately 97V, for example 103-(2x3)=97V. If the Freeze Dryer is
operating on nominal 230V each number represents 4V (if 3 is entered into
the display, the low line alarm will alarm when the voltage drops to
approximately 194V for example 206-(4x3)=194V. There will be no alarm
indicated if DISABLED is selected.

Press MENU and the display will show:

Press SELECT until the appropriate offset is shown. If the Freeze Dryer is
operating on nominal 115V, each number represents 2V. If 3 is entered
into the display, the high line alarm will alarm when the voltage raises to
approximately 133V, for example. 127+(2x3)=133V. If the Freeze Dryer
is operating on nominal 230V each number represents 4V (if 3 is entered
into the display, the low line alarm will alarm when the voltage drops to
approximately 266V, for example. 254+(4x3)=266V. There will be no
alarm indicated if DISABLED is selected.

Press MENU and the display will show:

Press and hold SELECT to change the status.

Product Service 816-333-8811 or 1-800-522-7658

Chapter 8: Modifying Your Freeze Dryer Display

40

DEFROST HEATER:
NOT INSTALLED

SHELL FREEZER:
NOT INSTALLED

PURGE VALVE:
NOT INSTALLED

MOISTURE SENSOR:
INSTALLED

HOLD SELECT TO CLEAR
ALL TOTAL HOURS?

PRODUCTION MENU:
MASTER RESET?

Press MENU and the display will show:

Press and hold SELECT to change the status.

Press MENU and the display will show:

Press and hold SELECT to change the status.

Press MENU and the display will show:

Press and hold SELECT if you want to disable the moisture sensor.

Press MENU and the display will show:

Press and hold SELECT to change the status

Press MENU and the display will show:

If you want to reset Total Hours, press and hold SELECT until an audible beep is
heard. The display will default to the main freeze dry display information.

If you do not want to set Total Hours, press MENU and the display will show:

The routine will repeat by pressing MENU or wait approximately 10 seconds for
the display to default to the main freeze dry information display information.

Product Service 816-333-8811 or 1-800-522-7658

Chapter 8: Modifying Your Freeze Dryer Display

41

PASSWORD:

In order to store offsets in memory, you Must Press and Hold MENU until display
shows:

Wait approximately 10 seconds and the display will default to the main freeze dry
display information. This can be done anytime throughout the Modifying the
Display routine.

Product Service 816-333-8811 or 1-800-522-7658

42

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OOMMPPOONNEENNTTSS

The following pages list components that are available for your Freeze Dryer. The
parts shown are the most common replacement parts. If other parts are required,
contact Product Service.

Product Service 1-800-522-7658

Appendix A: Freeze Dryer Components

43

Item

Part No.

Description

1

7690800

Lid Gasket

2

7532900

Lid 3 7448000

Printed Circuit Board RS232

4

7953800

Motor Fan, 115V

7953801

Motor Fan, 230V

5

7750607

Compressor, 115V, 60 Hz

7750606

Compressor, 230V, 50 Hz

7750605

Compressor, 230V, 60 Hz

6

1302300

Switch

7

7426000

Control Panel Label

8

7445590

Printed Circuit Board

9

7728000

Drain Plug

10

1643600

O-Ring

11

7645904

Drain Hose

12

7373450

Vacuum Hose (Not Shown)

13

1336400

Power Cord 115V 60Hz (Not Shown)

1336500

Power Cord 230V 50Hz EU (Not Shown)

1342100

Power Cord 230V 60Hz (Not Shown)

1332601

Power Cord 230V 50Hz UK (Not Shown)

1332701

Power Cord 230V 50Hz China (Not Shown)

14

7445400

Vacuum Sensor

15

7515300

Temperature Sensor (Not Shown)

16

7304700

Wire Harness, Power, 115V (Not Shown)

7304701

Wire Harness, Power, 230V (Not Shown)

17

7432700

Vacuum Control/Bleed Valve

18

7429700

Moisture Sensor

19

7418400

Wire Harness, Control 115V and 230V (Not Shown)

20

1289320

Circuit Breaker 115V 20A

1289310

Circuit Breaker 230V 10A

21

1289200

Relay – Vacuum Pump 115V

1289100

Relay – Vacuum Pump 230V

22

1289200

Relay-Refrigeration

Product Service 816-333-8811 or 1-800-522-7658

Appendix A: Freeze Dryer Components

44

Product Service 816-333-8811 or 1-800-522-7658

45

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Product Service 1-800-522-7658

46

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Catalog #

Voltage

Frequency

Phase

Amperage

Nominal

Operating

Range

Nominal

w/o

Vacuum

Pump

Max. with

Vacuum

Pump

7752020

115V

103-127

60 1 9

16

100V

90-110

50 1 9

16

7752021

115V

103-127

60 1 9

16

100V

90-110

50 1 9

16

7752030

230V

198-254

50 1 3

8

7752031

230V

198-254

50 1 3

8

7752040

230V

187-253

60 1 3

8

7752041

230V

187-253

60 1 3

8

7752060

230V

198-254

50 1 3

8

7752061

230V

198-254

50 1 3

8

7752070

230V

198-254

50 1 3

8

7752071

230V

198-254

50 1 3

8

This Appendix contains technical information about the Freeze Dryer including
electrical specifications and environmental operating conditions.

Electrical Specifications

Product Service 1-800-522-7658

Appendix C: Freeze Dryer Specifications

47

Environmental Conditions

 Indoor use only.
 Maximum altitude: 6562 feet (2000 meters).
 Ambient temperature range: 41° to 104°F (5° to 40°C).
 Maximum relative humidity: 80% for temperatures up to 88°F (31°C),

decreasing linearly to 50% relative humidity at 104°F (40°C).

 Main supply voltage fluctuations not to exceed ±10% of the nominal

voltage.

 Transient over voltages according to Installation Categories II (Over

voltage Categories per IEC 1010). Temporary voltage spikes on the AC
input line that may be as high as 1500V for 115V models and 2500V for
230V models are allowed.

 Used in an environment of Pollution degrees 2 (i.e., where normally only

non-conductive atmospheres are present). Occasionally, however, a
temporary conductivity caused by condensation must be expected, in
accordance with IEC 664.

Product Service 816-333-8811 or 1-800-522-7658

48

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PART #

DESCRIPTION

1467700

Vacuum Pump

Two stage direct drive pump, 195 liters/minute. 115 VAC,
50/60 Hz, single phase, 7.8 amps. Includes Pump Exhaust Filter

1473400. (Catalog #1473400)

7739403

Vacuum Pump

Two stage direct drive pump, 195 liters/minute. 230 VAC,
50/60 Hz, single phase, 4.0 amps. Includes Pump Exhaust Filter

1473400. (Catalog #1473400)

1472100

Vacuum Pump

Two stage direct drive pump, 117 liters/minute. 115 VAC,
50/60 Hz, single phase 4.6 amps. Includes Pump Exhaust Filter.
(Catalog #1473400)

7739402

Vacuum Pump

Two stage direct drive pump, 117 liters/minute. 230 VAC,
50/60 Hz, single phase 2.4 amps. Includes Pump Exhaust Filter.
(Catalog #1473400)

7584000

Vacuum Pump, Chemical Resistant Hybrid

Combination two stage rotary vane pump and two stage chemistry
diaphragm pump 98/115 liters/minute. 115 VAC, 50/60 Hz, single
phase.

7584002

Vacuum Pump, Chemical Resistant Hybrid

Combination two stage rotary vane pump and two stage chemistry
diaphragm pump 98/115 liters/minute. 230 VAC, 50/60 Hz, single
phase.

1472200

Pump Inlet Filter

Disposable filter that prevents oil back streaming and protects
vacuum pump from sub micron particles. Fits vacuum pumps
1466700 and 7739403.

The following accessories are available for the Freeze Dryer.

Product Service 1-800-522-7658

Appendix D: Freeze Dryer Accessories

49

PART #

DESCRIPTION

1473400

Pump Exhaust Filter

Disposable filter that removes visible oil mist and odor from vacuum
pump exhaust. Fits vacuum pumps 1467700 and 7739403.

1473200

Replacement Element, Oil Mist, Pump Exhaust Filter

Fits pump exhaust filter 1473400.

1473300

Replacement Element, Odor, Pump Exhaust Filter, package of 5

Fits pump exhaust filter 1473400 or vacuum pumps 1467700 and

7739403.

1988000

Vacuum Pump Oil, 1 Liter

A molecularly distilled hydrocarbon oil with low vapor pressure.
For vacuum pumps 1467700 and 7739403

7772000

Soda Acid Trap

Secondary trap that prevents migration of corrosive chemicals into
vacuum pump.

7772100

Replacement Media for Soda Acid Trap

7584300

Vacuum Pump Oil, 1 Liter

For Hybrid vacuum pumps 7584000, 7584002

7772500

Carbon Solvent Trap

Secondary trap that prevents migration of organic solvents into
vacuum pump.

7772600

Replacement Activated Carbon Media for Carbon Solvent Trap

7538000

Secondary Vacuum Cold Trap

Provides additional protection for the vacuum pump when processing
low eutectic samples.
9 ¾" high x 7 7/8" diameter, 304 stainless steel with ¾" vacuum
connections. For use with dry ice and solvent. Cools to approximately
–75°C.

7522800

12 Port Drying Chamber

9 ¾" high x 7 7/8" diameter, 304 stainless steel with 12 freeze dry
valves.

7522900

16 Port Drying Chamber

13" high x 138" diameter, 304 stainless steel with 16 freeze dry valves.

7443500

Clear Drying Chamber with 8 Valves

For bulk drying or drying in flasks. 9.0 Dia.

7444000

Clear Drying Chamber with 8 Valves

For bulk drying or drying in flasks. 12.0 Dia.

7442900

Clearing Drying Chamber

For bulk drying. 9.0 Dia.

Product Service 816-333-8811 or 1-800-522-7658

Appendix D: Freeze Dryer Accessories

50

PART #

DESCRIPTION

7867000

Clear Drying Chamber

For Bulk Drying 12.0 Dia.

7509200

Product Heater

For use in chamber 7522800. Provides 3 heated shelves operating at
43°C (110°F). 115V

7509201

Product Heater

For use in chamber 7522800. Provides 3 heated shelves operating at
43°C (110°F). 230V

7442100

Drying Rack- Unheated

Provides three shelves. For use in chambers 7443500 and 7522800.

7441700

Drying Rack – Unheated
Provides three shelves for use in chambers 7444000, 7867000,

7522900.

7522300

20 Port Manifold

10" high x 27 ½" wide x 8 5/8" deep. Type 304 stainless steel
manifold with 20 freeze dry valves.

7522400

10 Port Manifold with support shelf
10" high x 26" wide x 6-5/8" deep. Type 304 Stainless Steel
Manifold with 10 Freeze Dry Valves & 1 Shelf.

7522500

20 Port Manifold with support shelves
10" high x 26" wide x 9-1/2" deep. Type 304 Stainless Steel
Manifold with 20 Freeze Dry valves and 2 shelves.

7868500

48 Port Ampule Manifold

28 5/8" high x 5" wide x 5" deep. Type 304 stainless steel with
48 each ¼" tube stems.

7509600

Sample Valve Kit

Includes neoprene valve body, knob and installation parts.

7439901

Glass Collector Chamber Lid

For use with solvlents that attack the acrylic lid.

7439902

Glass Collector Chamber Lid

For use with solvlents that attack the acrylic lid.

7509300

Product Heater

For use in chamber 7522900, 7444000 and 7867000. Provides 3
heated shelves operating at 43°C (110°F). 115V

7509301

Product Heater

For use in chamber 7522900, 7444000 and 7867000. Provides 3
heated shelves operating at 43°C (110°F). 230V

7509400

Product Heater with Variable Heat

For use in chamber 7522900, 7444000 and 7867000. Provides
variable heat up to 43°C (110°F). 115V

Product Service 816-333-8811 or 1-800-522-7658

Appendix D: Freeze Dryer Accessories

51

PART #

DESCRIPTION

7509401

Product Heater with Variable Heat

For use in chamber 7522900, 7444000 and 7867000

7806020

Bulk Tray Dryer

115V, 60 Hz, three shelves, 630 square inches of area, provides heat
control

7806021

Bulk Tray Dryer

115V, 60 Hz, three shelves, 630 square inches of area, provides heat
control with 6 port manifold

7806022

Bulk Tray Dryer

115V, 60 Hz, three shelves, 630 square inches of area, provides heat
control with RS232 output connection.

7806023

Bulk Tray Dryer

115V, 60 Hz, three shelves, 630 square inches of area, provides heat
control with 6 port manifold and RS232 output connection.

7806030

Bulk Tray Dryer

230V, 50/60 Hz, Three shelves, 630 square inches of area, provides
heat control.

7806031

Bulk Tray Dryer

230V, 50/60 Hz, Three shelves, 630 square inches of area, provides
heat control. With 6 port manifold.

7806032

Bulk Tray Dryer

230V, 50/60 Hz, Three shelves, 630 square inches of area, provides
heat control. With RS232 output connection.

7806033

Bulk Tray Dryer

230V, 50/60 Hz, Three shelves, 630 square inches of area, provides
heat control. With 6 port manifold and RS232 output connection.

7948020

Stoppering Tray Dryer

115V, 60 Hz, three shelves, 600 square inches of area, provides
temperature control and stoppering under vacuum.

7948030

Stoppering Tray Dryer

230V, 50 Hz, three shelves, 600 square inches of area, provides
temperature control and stoppering under vacuum.

7948040

Stoppering Tray Dryer

230V, 60 Hz, three shelves, 600 square inches of area, provides
temperature control and stoppering under vacuum.

7726500

6 Port Manifold for use with Stoppering Tray Dryer

Mounts between the Stoppering Tray Dryer and the base unit and
provides 6 freeze dry valves.

Product Service 816-333-8811 or 1-800-522-7658

Appendix D: Freeze Dryer Accessories

52

PART #

DESCRIPTION

7537800

Cable

Connect the RS232 output from the Freeze Dryer (or Freeze
Dryer/Tray Dryer combination) to an IBM compatible computer with
a 9-pin serial data port.

7537801

Cable

Connects the RS232 output from the Freeze Dryer (or Freeze
Dryer/Tray Dryer combination) to an IBM compatible computer with
a 25-pin serial data port.

7761500

Isolation Valve

Mounts between the Stoppering Tray Dryer and the base unit which
provides a way to isolate the base unit vacuum system from the
Stoppering Tray Dryer vacuum system.

7390702

Baffle

Mounts in the collector chamber to increase ice holding capacity
when operating with the vacuum control.

Product Service 816-333-8811 or 1-800-522-7658

Appendix D: Freeze Dryer Accessories

53

Fast-Freeze® Flasks

Product Service 816-333-8811 or 1-800-522-7658

Appendix D: Freeze Dryer Accessories

54

Lyph-Lock® Flasks

Product Service 816-333-8811 or 1-800-522-7658

Appendix D: Freeze Dryer Accessories

55

Serum Bottles & Vials

Product Service 816-333-8811 or 1-800-522-7658

Appendix D: Freeze Dryer Accessories

56

Ampules

Product Service 816-333-8811 or 1-800-522-7658