User`s Manual

User`s Manual
User’s Manual
FreeZone® Plus™ 4.5 Liter Cascade
Freeze Dry Systems
Models
73820 Series
73860 Series
73870 Series
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Labconco Corporation
8811 Prospect Avenue
Kansas City, MO 64132-2696
800-821-5525, 816-333-8811
FAX 816-363-0130
E-MAIL [email protected]
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Please read the User’s Manual before operating the equipment.
Copyright © 2008, 2009, 2012 Labconco Corporation. All rights reserved.
The information contained in this manual and the accompanying products are copyrighted and all rights
reserved by Labconco Corporation. Labconco Corporation reserves the right to make periodic design
changes without obligation to notify any person or entity of such change.
Warranty
Labconco provides a warranty on all parts and factory workmanship. The warranty includes areas of
defective material and workmanship, provided such defect results from normal and proper use of the
equipment.
The warranty for all Labconco products will expire one year from date of installation or two years
from date of shipment from Labconco, whichever is sooner, except the following;
•
Purifier® Logic™ Biosafety Safety Cabinets and PuriCare® Lab Animal Research Stations
carry a three-year warranty from date of installation or four years from date of shipment
from Labconco, whichever is sooner.
•
SteamScrubber® & FlaskScrubber® Glassware Washers carry a two-year warranty from
date of installation or three years from date of shipment from Labconco, whichever is sooner.
•
Blood Drawing Chairs carry a ten year warranty.
•
Carts carry a lifetime warranty.
•
Glassware is not warranted from breakage when dropped or mishandled.
This limited warranty covers parts and labor, but not transportation and insurance charges. In the
event of a warranty claim, contact Labconco Corporation or the dealer who sold you the product. If
the cause is determined to be a manufacturing fault, the dealer or Labconco Corporation will repair or
replace all defective parts to restore the unit to operation. Under no circumstances shall Labconco
Corporation be liable for indirect, consequential, or special damages of any kind. This statement may
be altered by a specific published amendment. No individual has authorization to alter the provisions
of this warranty policy or its amendments. Lamps and filters are not covered by this warranty.
Damage due to corrosion or accidental breakage is not covered.
Returned or Damaged Goods
Do not return goods without the prior authorization from Labconco. Unauthorized returns will not be
accepted. If your shipment was damaged in transit, you must file a claim directly with the freight carrier.
Labconco Corporation and its dealers are not responsible for shipping damages.
The United States Interstate Commerce Commission rules require that claims be filed with the delivery
carrier within fifteen (15) days of delivery.
Limitation of Liability
The disposal and/or emission of substances used in connection with this equipment may be governed by
various federal, state, or local regulations. All users of this equipment are required to become familiar with
any regulations that apply in the user’s area concerning the dumping of waste materials in or upon water,
land, or air and to comply with such regulations. Labconco Corporation is held harmless with respect to
user’s compliance with such regulations.
Contacting Labconco Corporation
If you have questions that are not addressed in this manual, or if you need technical assistance, contact
Labconco’s Customer Service Department or Labconco’s Product Service Department at 1-800-821-5525
or 1-816-333-8811, between the hours of 7:00 a.m. and 6:00 p.m., Central Standard Time.
Part #7387900, Rev. B
ECO G733
TABLE OF CONTENTS
CHAPTER 1: INTRODUCTION
Freeze Dry Process
Freeze Dry Rates
Freeze Dry Capacity
Samples Containing Volatile Substances
Safety Symbols
1
1
2
3
4
4
CHAPTER 2: PREREQUISITES
Electrical Requirements
Location Requirements
Vacuum Pump Requirements
Chamber or Manifold Requirements
6
6
6
7
7
CHAPTER 3: GETTING STARTED
Unpacking Your Freeze Dryer
Freeze Dryer Components
Setting Up Your Freeze Dryer
Vacuum Pump Connection
Electrical Connection
Drying Chamber or Drying Manifold Installation
Chemical Resistance of Freeze Dryer Components
Solvent Safety Precautions
8
9
9
11
11
11
11
12
13
CHAPTER 4: USING YOUR FREEZE DRYER
Freeze Dryer Controls
Operation Checklist
Vacuum Pump Ballast Setting
Operating the Freeze Dryer
Set-Up
Automatic Start-Up
Manual Start-Up
Setting the Operating Vacuum Level
Pre-Freezing Samples
Adding Sample
Shut Down
Defrosting
14
15
16
16
17
17
19
19
20
20
21
22
22
Alarms
Power Failure
Line Voltage Out of Range
Temperature Out of Range
Service Vacuum Pump
Moisture in Collector
23
23
23
24
24
24
CHAPTER 5: MAINTAINING YOUR FREEZE DRYER
25
CHAPTER 6: USING THE RS232 RECEPTACLE
Computer Connection for Computer Interface
27
27
CHAPTER 7: TROUBLESHOOTING
Vacuum Pump
Gaskets, Tubing, Connections, Sample Valves
System Components & Collection Chamber Isolation
Refrigeration Module Operation
31
31
32
34
36
CHAPTER 8: MODIFYING YOUR FREEZE DRYER DISPLAY
Temperature and Vacuum Display
Line Voltage Alarm Points
Moisture Sensor Alarm
Modifying the Display
37
37
37
38
38
APPENDIX A: FREEZE DRYER COMPONENTS
42
APPENDIX B: FREEZE DRYER DIMENSIONS
44
APPENDIX C: FREEZE DRYER SPECIFICATIONS
Electrical Specifications
Environmental Conditions
47
47
48
APPENDIX D: FREEZE DRYER ACCESSORIES
49
DECLARATION OF CONFORMITY
56
CHAPTER 1
INTRODUCTION
Congratulations on your purchase of a Labconco FreeZone® Freeze Dry
System, which is designed for laboratory lyophilization procedures. The
refrigerant used in the refrigeration system is CFC-free so it will not
endanger the environment. The unit is easy to install and maintain. Proper
care and maintenance of this product will result in many years of dependable
service.
Freeze Dry Process
Freeze drying is an important process in sample preparation and for the
preservation and storage of biologicals, pharmaceuticals and foods. Of the
various methods of dehydration, freeze drying (lyophilization) is especially
suited for substances that are heat sensitive. Other than food processing (e.g.,
coffee, whole dinners), freeze drying has been extensively used in the
development of pharmaceuticals (e.g., antibiotics) and preservation of
biologicals (e.g., proteins, plasma, viruses and cell lines). The nondestructive
nature of this process has been demonstrated by the retention of viability in
freeze dried viruses and microorganisms.
Freeze drying is a process whereby water or other solvent is removed from
frozen material by converting the frozen water directly into vapor without the
intermediate formation of liquid water. The basis for this sublimation
process involves the absorption of heat by the frozen sample in order to
vaporize the ice; the use of a vacuum pump to enhance the removal of water
vapor from the surface of the sample; the transfer of water vapor to a
collector; and the removal of heat by the collector in order to condense the
water vapor. In essence, the freeze dry process is a balance between the heat
absorbed by the sample to vaporize the ice and the heat removed from the
collector to convert the water vapor into ice.
Product Service 816-333-8811 or 1-800-522-7658
1
Chapter 1: Introduction
Freeze Dry Rates
The efficiency of the freeze drying process is dependent upon the surface
area and the thickness of the sample, the collector temperature and vacuum
obtained, the eutectic point and solute concentration of the sample. It is
important to remember these factors when trying to obtain efficient
utilization of your freeze dry system. A listing of selected materials and their
approximate drying times are shown in Table 1 for your reference.
Table 1
SAFE TEMPERATURE AND DRYING TIMES
FOR SELECTED MATERIALS
Material
Safe
Collector
Hours
10mm Thick
Temperature Temperature (Approx.)
°C
°C
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.
2
Product Service 816-333-8811 or 1-800-522-7658
Chapter 1: Introduction
In order for lyophilization to occur, ice must be removed from the frozen
sample via sublimation. This is accomplished by the collector and the
vacuum pump. The collector, which should be at least 15 to 20°C colder than
the eutectic temperature (melting temperature) of the sample, traps vapor as
ice. Since the vapor pressure at the collector is lower than that of the sample,
the flow of water vapor is from the sample to the collector. Since this vapor
diffusion process occurs very slowly under normal atmospheric conditions, a
good vacuum is essential to maintain an efficient rate. In many applications,
the maintenance of a vacuum of 0.133 mBar or less is recommended.
The rate of freeze drying is directly proportional to the vapor pressure and the
vapor pressure is dependent upon both eutectic temperature and solute
concentration of the sample. For example, a solution of sodium chloride and
water would freeze dry at a slower rate than pure water. The eutectic
temperature of a sodium chloride solution is about –21°C and at this
temperature the vapor pressure is about 1/16 that of water at 0°C. Although
the eutectic temperature is not dependent upon the concentration of sodium
chloride, the vapor pressure of the water would decrease as the concentration
of sodium chloride increased. This is due to the fact that as the solute
concentration increases, less of the surface area of the frozen sample is
occupied by water. In general, most solutions or biological samples will have
a eutectic temperature of –10 to –25°C. However, if the sample contains a
simple sugar such as glucose or if the sample is animal or plant tissue, the
eutectic temperature may be as low as –30° to –50°C.
Freeze Dry Capacity
The volume of a sample that can be freeze dried at one time is related to
factors discussed previously and the size and design of the freeze dry system.
With any given instrument, the capacity is based on the surface area of the
sample; the eutectic temperature and concentration of the sample; and the rate
and amount of heat transferred to the frozen sample. Of these factors, the
eutectic temperature is the most important factor in determining the amount
of sample that can be freeze dried at one time, particularly when flasks are
used. This is because as the eutectic temperature decreases, the vapor
pressure decreases but the rate of heat absorption by the sample does not
change. This tends to promote melting of the sample, which leads to a
marked increase in vapor pressure and ultimately overloads the collector and
vacuum pump. Samples that have eutectic temperatures of –20°C or lower
should be placed on the freeze dry system one flask at a time so that the
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.
Product Service 816-333-8811 or 1-800-522-7658
3
Chapter 1: Introduction
If there is a problem with a particular type of sample melting when placed on
the freeze dry system, dilution of the sample with more water or providing
some insulation around the flask to decrease the rate of heat absorption by the
sample may help. If the eutectic temperature of the sample is –40 to –60°C,
the freeze dry system selected for use must be equipped with cascade type
refrigeration so that the collector temperature can be cooled to below –75°C,
or a dry ice/solvent trap may be used between the collector and the vacuum
pump.
Samples Containing Volatile
Substances
In certain cases the solvent in a sample to be freeze dried may contain
volatile components such as acetonitrile, methanol, acetic acid, formic acid or
pyridine. In addition to these substances having an effect on the eutectic
temperature, they may increase the vapor pressure at the surface of the
sample. Also, compared to water, they will require the absorption of less
heat for sublimation to occur. Hence, samples that contain volatile
substances will have a greater tendency to melt, particularly when placed in
flasks or exposed to room temperature. If a sample containing a volatile
substance tends to melt when placed on a freeze dry system, dilution of the
sample with more water will help keep the sample frozen. For example, a
0.2M solution of acetic acid is much easier to freeze dry than a 0.5M
solution.
Safety Symbols
Your freeze dry system was designed with safety in mind, however
conditions may exist that could be hazardous.
4
Product Service 816-333-8811 or 1-800-522-7658
Chapter 1: Introduction
Throughout this manual potentially hazardous conditions are identified using
the following words and symbols.
It is important that you understand the warnings listed throughout this manual
before you operate the freeze dry system.
Product Service 816-333-8811 or 1-800-522-7658
5
CHAPTER 2
PREREQUISITES
Before you install your freeze dryer, you need to prepare your site for
installation. Carefully examine the location where you intend to install your
freeze dryer. You must be certain that the area is level and of solid
construction. An electrical source must be located near the installation site.
Carefully read this chapter to learn:
•
•
the electrical supply requirements.
the vacuum pump requirements.
Refer to Appendix C: Freeze Dryer Specifications for complete freeze dryer
electrical and environmental conditions, specifications and requirements.
Electrical Requirements
The freeze dryer requires a dedicated electrical outlet. This outlet requires a
20 Amp circuit breaker or fuse for models rated at 115V (60 Hz). An outlet
equipped with a 15 Amp circuit breaker or fuse is required for models rated
at 230V (50/60 Hz). See Freeze Dryer Components in Chapter 3 for detail
plug specifications. If the plug supplied with the Freeze Dryer does not
match the available receptacle, remove this plug and replace it with an
approved plug of the suitable style.
Location Requirements
The freeze dryer should be located in an area that provides an unobstructed
flow of air around the cabinet. This air cools the refrigeration system. The
refrigeration system draws air through the rear panel and exhausts it through
the sides. A minimum of 3" must be allowed between the back and both
sides of the freeze dryer and adjacent wall surfaces. Restriction of airflow
during operation could adversely affect performance.
6
Product Service 816-333-8811 or 1-800-522-7658
Chapter 2: Prerequisites
Refer to Appendix C: Freeze Dryer Specifications for dimensional drawings
of the Freeze Dryer. The space for benchtop models must be large enough to
accommodate the vacuum pump, which will be used with the freeze dryer.
Vacuum Pump Requirements
A vacuum pump must be provided by the user. A vacuum pump with a
displacement of 86 liters per minute and 0.002 mBar ultimate pressure is
adequate for most samples. The inlet fitting on the vacuum pump must be
suitable for 3/4" ID vacuum hose, which is provided. It is recommended that
the vacuum pump is equipped with an exhaust filter to minimize oil mist
exhausting from the vacuum pump. The operating vacuum level may be set
on the freeze dryer. The higher the pressure is set, the more likely it is that
oil mist will be exhausted.
Vacuum pumps used with 115V models should be equipped with a 115V, 15
Amp NEMA 5-15P plug. Vacuum pumps used with 230V models should be
equipped with a reverse IEC plug. This plug is included with 230V models.
This will allow the vacuum pump to be plugged into the receptacle on the
back panel of the freeze dryer. See Appendix D: Freeze Dryer Accessories
for vacuum pumps available from Labconco.
Chamber or Manifold Requirements
A 12-port drying chamber is included with the unit. This allows 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
7
CHAPTER 3
GETTING STARTED
Now that the site for your freeze dryer is properly prepared, you are ready to
unpack, inspect, install and test your freeze dryer. Read this chapter to learn
how to:
•
•
•
•
•
8
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.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
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.
The Benchtop FreeZone Plus Cascade 4.5 Liter Freeze Dry System weighs
over 125 lbs. (57 Kg). The Console FreeZone Plus Cascade 4.5 Liter Freeze
Dry System weighs over 176 lbs. (80 Kg). If you must lift the freeze dryer
manually, use at least two (2) persons and follow safe lifting guidelines.
If your freeze dryer was damaged in transit, you must file a claim directly
with the freight carrier. The United States Interstate Commerce Commission
rules require that claims be filed with the delivery carrier within fifteen (15)
days of delivery. Labconco Corporation and its dealers are not responsible
for shipping damage.
Do not return goods without the prior authorization of Labconco.
Unauthorized returns will not be accepted.
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 FreeZone Plus Cascade 4.5 Liter Freeze Dry System you
received in the following table. Verify that the components listed are present
and undamaged.
Product Service 816-333-8811 or 1-800-522-7658
X
1332701
Hz
60
60
50
50
60
60
50
50
50
50
1332601
Volts
115
115
230
230
230
230
230
230
230
230
1342100
Description
4.5L Benchtop Cascade Freeze Dryer
4.5L Benchtop Cascade Freeze Dryer
4.5L Benchtop Cascade Freeze Dryer
4.5L Benchtop Cascade Freeze Dryer
4.5L Benchtop Cascade Freeze Dryer
4.5L Benchtop Cascade Freeze Dryer
4.5L Benchtop Cascade Freeze Dryer
4.5L Benchtop Cascade Freeze Dryer
4.5L Benchtop Cascade Freeze Dryer
4.5L Benchtop Cascade Freeze Dryer
1336500
Catalog #
7386020
7386021
7386030
7386031
7386040
7386041
7386060
7386061
7386070
7386071
Teflon
Coated
Chamber
1336400
Power Cords
X
X
X
X
X
X
X
X
X
X
X
X
X
X
9
Chapter 3: Getting Started
7387071
4.5L Console Cascade Freeze Dryer
230
50
7382020
7382021
7382030
7382031
7382032
7382033
7382034
7382035
7382040
4.5L -105C Benchtop Freeze Dryer
4.5L -105C Benchtop Freeze Dryer
4.5L -105C Benchtop Freeze Dryer
4.5L -105C Benchtop Freeze Dryer
4.5L -105C Benchtop Freeze Dryer
4.5L -105C Benchtop Freeze Dryer
4.5L -105C Benchtop Freeze Dryer
4.5L -105C Benchtop Freeze Dryer
4.5L -105C Benchtop Freeze Dryer
115
115
230
230
230
230
230
230
230
60
60
50
50
50
50
50
50
60
7382041
4.5L -105C Benchtop Freeze Dryer
230
60
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Component Description
7387900
7373450
1488800
7395801
7395800
7522800
1291000
User’s Manual
Vacuum Hose
Hose Clamps (2)
Chamber Lid
Lid Gasket
Drying Chamber (12-port)
Plug
X
X
X
X
X
X
X
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.
10
X
X
X
Plus the following:
Part #
1332701
Hz
60
60
50
50
60
60
50
50
50
1332601
Volts
115
115
230
230
230
230
230
230
230
1342100
Description
4.5L Console Cascade Freeze Dryer
4.5L Console Cascade Freeze Dryer
4.5L Console Cascade Freeze Dryer
4.5L Console Cascade Freeze Dryer
4.5L Console Cascade Freeze Dryer
4.5L Console Cascade Freeze Dryer
4.5L Console Cascade Freeze Dryer
4.5L Console Cascade Freeze Dryer
4.5L Console Cascade Freeze Dryer
1336500
Catalog #
7387020
7387021
7387030
7387031
7387040
7387041
7387060
7387061
7387070
Teflon
Coated
Chamber
1336400
Power Cords
Product Service 816-333-8811 or 1-800-522-7658
X
Chapter 3: Getting Started
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.
Place the vacuum pump near the benchtop freeze dryer models. For console
models, from the back of the unit, place the vacuum pump on the floor of the
cabinet.
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. Make certain that the oil in the
vacuum pump is at the proper level.
Electrical Connection
Plug the power cord into the receptacle on the back of the freeze dryer and
plug the other end into a suitable power receptacle.
Drying Chamber or Drying Manifold Installation
Install the clear lid with 3.0 inch hole on top of the collector chamber.
The supplied drying chamber or drying manifold, which may be purchased
separately, may be positioned directly above the 3-inch hole in the collector
chamber lid. Center the rubber gasket that came with the chamber over the
hole in the lid. Then place the chamber over the gasket. When vacuum is
applied to the system, the chamber will be held securely in place.
Product Service 816-333-8811 or 1-800-522-7658
11
Chapter 3: Getting Started
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:
Silicon Rubber
Stainless Steel
D
Dioxane
Methyl t-Butyl Ether (BTBE)
Pyridine
D
Cyclohexane
C
Carbon Tetrochloride
D
D
Acetonittirle
C
D
D
D
Solvents
Acetone
D
Sodium Phosphate
C
Calcium Chloride
Formic Acid
Material
Acetal (Delrin)
Acrylic
Neoprene
Acetic Acid 20%
Component
Valve Stem
Collector Lid
Hoses, Gaskets
& Valve
Bodies
Flask Top
Chamber &
Fittings
Buffers
Trifluoroacetic Acid (TFA)
Acids
D
D
C
D
C
D
D
D
D
C
D
D
D
D
C
D
C
C – Moderate degradation; Limited use
D – Severe degradation; infrequent use recommended; immediate thorough
cleaning required.
•
•
Most common compounds used in freeze drying processes, if allowed to
enter the vacuum pump, will degrade the oil and cause damage to the
vacuum pump.
Sugars and proteins typically will have minimal negative effect on any of
the materials of construction.
When using compounds in the freeze dryer that are hostile to the materials of
construction, it is imperative the equipment is thoroughly cleaned after use.
•
12
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
•
The oil in the vacuum pump should be checked often. It must be changed
if it is cloudy, shows particles or is discolored. The useful life of vacuum
pump oil can be extended if the vacuum pump is operated for an extended
period of time after a freeze dry run. This allows contaminants to be
purged from the hot oil. This must be done with the inlet to the pump
blocked off to prevent air from free flowing through the pump. If the
pump is operated at an elevated vacuum level (> 10mBar), oil may be
expelled from the pump and damage could occur.
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 816-333-8811 or e-mail:
[email protected]
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.
NOTE: 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
13
CHAPTER 4
USING YOUR FREEZE
DRYER
After your Freeze Dryer has been installed as detailed in Chapter 3: Getting
Started, you are ready to begin using your Freeze Dryer. Read this chapter to
learn how to:
•
•
•
operate the controls.
understand the display.
connect samples.
Do not use the freeze dryer in a manner not specified by the
manufacturer (refer to Appendix C: Freeze Dryer Specifications). The
electrical protection properties of the freeze dryer may be impaired if the
freeze dryer is used inappropriately.
14
Product Service 816-333-8811 or 1-800-522-7658
Chapter 4: Using Your Freeze Dryer
Freeze Dryer Controls
The control panel for the freeze dryer is shown below with a description
about its function.
1
2
5
10
7
11
9
8
12
6
4
3
1. LCD Display – Displays system operating parameters, set-up parameters
and alarm messages.
2. Menu Switch – This switch is used to change the display from operating
system parameters to set-up parameters.
3. Select Switch – Used to select set-up parameters.
4. Vacuum Switch – Used to start or stop the vacuum pump when operating in
manual start-up mode.
5. Vacuum Indicator – This green LED indicates that power is being supplied to the
vacuum pump receptacle on the back of the freeze dryer.
6. Manual Refrigeration Switch – Used to start only the refrigeration module.
7. Manual Operation Indicator – When lit, the green LED indicates the freeze dryer
is being controlled manually by the operator. Each function must be started by the
operator.
8. Auto Mode Switch – Used to start or stop the refrigeration and the Auto Mode
process.
9. Auto Mode Indicator – When lit, the green LED indicates that the freeze dryer is
in Auto Mode. In this mode, the vacuum pump will start when the collector
temperature reaches –40°C.
10. Vacuum Graph Display – This display indicates the relative system vacuum level.
The highest LED indicates that the vacuum level is above 2.0 mBar. The
indicators will sequence down when the vacuum level reaches 2.0, 1.0, 0.8, 0.6,
0.45, 0.12 mBar. The lower green LED flashes when the system vacuum level is
0.45 to 0.12 mBar and illuminates steadily below 0.133 mBar.
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Chapter 4: Using Your Freeze Dryer
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. The indicators will sequence down when the temperature reaches 10, 0,
-10, -20, -30, -40°C (-10, -20, -30, -40, -50, -60 for Models 73820xx). When the
collector temperature is –40°C (-60°C for Models 73820xx) 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 drying chamber or accessory 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. 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.
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Chapter 4: Using Your Freeze Dryer
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.
To configure your freeze dryer, turn the main power switch ON and press
MENU. The display shows:
VACUUM UNITS
mBar
•
•
•
Pa
Torr
Press SELECT until the desired units are flashing.
Press MENU.
The display shows:
VACUUM SET POINT
XXXX
YYY
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 “0” 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 shows:
TEMPERATURE UNITS
°C
°F
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Chapter 4: Using Your Freeze Dryer
•
•
•
Press SELECT until the desired units are flashing.
Press MENU.
The display shows:
REFRIG TOTAL HOUR: XXXX
SERVICE HOUR: XXXX
•
•
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 shows the refrigeration system hours.
REFRIG TOTAL HOUR: XXXX
RESET SERVICE HOUR: ?
•
•
•
•
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 shows the vacuum pump hours.
VACUUM TOTAL HOUR: XXXX
SERVICE HOUR: XXXX
•
•
To reset the SERVICE HOUR to 0, press SELECT.
The display shows:
VACUUM TOTAL HOUR: XXXX
RESET SERVICE HOUR: ?
If you want to reset the service hours to 0, continue to hold SELECT five
seconds until hours are reset.
• Press SELECT.
• The display shows the RS-232 data transmission rate.
RS-232 TRANSMISSION RATE
10
18
SECONDS
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Chapter 4: Using Your Freeze Dryer
•
•
To change the rate press and hold 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 SELECT to return to display operating parameters or after a
short delay, the display will automatically switch to show operating
parameters.
Automatic Start-Up
To run the Auto Mode, press the panel switch labeled REFRIGERATION
AUTO. The green LED above the switch illuminates and the refrigeration
system starts. When the collector reaches –40°C, the vacuum pump will
start. The Temperature and Vacuum Graph indicate collector temperature
and system vacuum. The LCD display shows the actual temperature of the
collector. When the vacuum in the system is above 5 mBar the vacuum
display indicates “HI.” At 5 mBar and below, the display shows 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 starts the refrigeration system. The green LED above the switch
illuminates. When the collector temperature reaches –40°C, the vacuum
pump may be started by pressing the VACUUM switch. The Temperature
and Vacuum Graph indicate collector temperature and system vacuum. The
LCD display shows the actual temperature of the collector. When the
vacuum in the system is above 5 mBar the vacuum display indicates “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.
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Chapter 4: Using Your Freeze Dryer
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.
Some guidelines for setting the freeze dryer are shown below. These show
pre-freezing temperatures and vacuum levels. Exact protocols must be
determined by the user for the specific samples that are being freeze dried.
When the vacuum control is set to operate at less vacuum, the ice holding
capacity of the collector may be decreased.
Solidification/Eutectic
Temperature
-40°C and Colder
Material
Bacteria,Virus
Milk
Fungi
Vegetable Tissue
Human Tissue
Blood Plasma
Vaccine
-5 to -13
-40 and Colder
-25 to -50
-30 to –40
-10 to –25
-30 to –40
Pre-Freeze
Temperatures
-50°C &
Colder
-15 to -23
-50 & Colder
-35 to -60
-40 to –50
-20 to –35
-40 to –50
Vacuum Set Point
0.040 mBar &
Lower
1.65 to 0.77
0.04 and lower
0.22 to 0.01
0.12 to 0.04
1.03 to 0.22
0.12 to 0.04
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 or in the center of the collector chamber.
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.
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Chapter 4: Using Your Freeze Dryer
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, which connects the attached sample to system
vacuum. The bevel on the knob should be positioned toward the sample port to
apply vacuum to the sample.
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.
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Chapter 4: Using Your Freeze Dryer
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.
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 right 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
Alarms
A number of unusual events may occur during a lyophilization procedure that
can adversely effect the operation of the freeze dryer. If an event occurs, the
alarm indicator flashes and the beeper sounds.
The beeper automatically mutes itself after one minute. The specific alarm
can be identified by pressing MENU. Pressing MENU multiple times
displays multiple alarms if they have occurred. The following “out of
specification” conditions initiate an alarm:
Power Failure
If a power failure occurs during a freeze dry process, the vacuum control
valve allows 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 restarts 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 flashes and the alarm beeper
sounds. When the MENU button is pressed the display shows:
POWER FAIL
HOLD SELECT TO CLEAR IT
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
shows:
LINE VOLTAGE ERROR
The alarm self-cancels 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
Temperature Out of Range
An alarm activates if the collector temperature rises above –40°C (-60°C for
Models 73820xx). If this occurs, the display shows:
COLLECTOR TEMPERATURE
HOLD SELECT TO CLEAR IT
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:
CHANGE VACUUM OIL
HOLD SELECT TO CLEAR IT
Press and hold SELECT for five seconds until the error message is cleared
from the display.
This resets 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 shows:
MOISTURE IN COLLECTOR
When the collector is drained, the alarm self-cancels.
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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Product Service 816-333-8811 or 1-800-522-7658
CHAPTER 5
MAINTAINING YOUR FREEZE
DRYER
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, nonabrasive soap or detergent.
3. Check oil level of the vacuum pump. It should be between MIN and
MAX. If the oil level is less than an inch (25.4 mm) above MIN, add oil
to proper level.
4. If oil shows cloudiness, particles or discoloration, drain the pump and
replace with fresh oil.
5. Utilization of acids requires immediate cleaning and neutralization
after a run or physical damage to the collector chamber and collector
coil will result.
6. Check the collection chamber for condensed or frozen solvents and
dispose of appropriately. Completely empty the collector chamber before
the next run or before attempting to start the vacuum pump.
7. If sample valves leak or stems become difficult to turn, pull the stem out
of the 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
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.
Front Access Panel Removal (Console Models)
The front stainless steel panel can be removed by placing a flat blade
screwdriver in the rectangular hole in the center of the kick panel. Pivot the
handle downward to disengage the latch and simultaneously pull the bottom
edge of the lower panel forward. The lower panel is installed by first sliding
the top edge under the lip on the plastic control panel. Pivot the bottom
inward and push until the latch is secure.
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CHAPTER 6
USING THE RS232
RECEPTACLE
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.
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 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 freeze dryer.
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.
2.
3.
4.
5.
Data Rate 2400 Baud
8 Bit word length
1 Start bit, 1 Stop bit
No parity is transmitted
Standard ASCII character set
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Chapter 6: Using the RS232 Receptacle
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.
RS-232 TRANSMISSION RATE
10
SECONDS
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
T
-48
V
18
SF
9
C
PG
= Base Unit
= Collector Temperature
= Collector Temperature in °Celsius
= Vacuum
= Vacuum Level in Micro Bars
= Shell Freezer Temperature (not available on 4.5L models)
= Feature not installed or out of range
= Vacuum Chamber Temperature(not available on 4.5L models)
= Purge (not available on 4.5L models)
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 use:
START/ROGRAMS/ACCESSORIES/COMMUNICATIONS
The first time Hyper Terminal™ is opened a dialogue box requesting an area
code and phone number appears. Enter the appropriate numbers and
continue.
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Chapter 6: Using the RS232 Receptacle
3. The “Connection Description” dialogue box opens. Type in a user
defined name and select an icon for the new connection. Press “OK.”
4. The “Connect To” dialogue box opens. Using the down arrow selection
button, select the communication port to which the cable has been
connected. Press “OK.”
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Chapter 6: Using the RS232 Receptacle
5. The “Com X Properties” dialogue box opens. Enter the appropriate data
properties and press “OK.”
6. When the freeze dryer main power switch is on, the data is transmitted
and updated at the time intervals selected by the user.
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CHAPTER 7
TROUBLESHOOTING
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.
FreeZone 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 0.033 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
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 and knob and stem assembly.
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Chapter 7: Troubleshooting
The illustrations below show how the sample valve installs on a chamber and
a manifold.
Knob & Stem
Assembly
Valve Body
Valve Assembly (Clear Chamber with Valves)
Manifold Assembly
Valve Body
Bulkhead Nut
Thrust Washer
Valve Body
Knob & Stem
Assembly
Valve Body
Trim Ring
Valve Assembly (Manifold)
Knob & Stem
Assembly
Thrust Washer
Gasket
(No grease
required)
Bulkhead
Fitting
Valve Assembly (Stainless Steel Chamber)
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Chapter 7: Troubleshooting
III. System Components and Collection Chamber
Isolation
This test determines if the source of a leak is in the drying chamber.
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.
Isolating the freeze dryer from the accessory chamber/manifold
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Chapter 7: Troubleshooting
The following test determines if a vacuum leak is in the collection chamber.
1. Insert a rubber stopper in the small hole in the rear of the collector
chamber and another in the drain port in the bottom.
2. Start the freeze dryer and observe the vacuum indication. If the
vacuum is good, the problem is in the collection chamber. If it is bad,
the problem is in the plumbing connections from the collection
chamber to the vacuum pump.
3. If the leak is in the chamber, check the bulkhead fittings where the
collection coil passes through the button of the chamber.
4. If the leak is in the plumbing connections, check all rubber parts, the
drain hose, the drain plug, fittings and clamps.
Checking the connections to the pump and the vacuum tube
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Chapter 7: Troubleshooting
Refrigeration Module Operation
Under a no-load condition, FreeZone Plus Cascade Freeze Dry Systems
should achieve a collector temperature of –84°C (models 73860xx and
73870xx) or -105°C (models 73820xx) or lower when the vacuum pump is
operating. If the collector temperature does not reach the design temperature
within 30 minutes, then the refrigeration module is not functioning properly.
Cascade Systems consist of two vapor-compression refrigeration systems in
series connected together via a heat exchanger. Each system has a
compressor, condenser, capillary tube metering device and an evaporator.
During the operation the evaporator of the “high stage” system refrigerates
the condenser of the “low stage” system. This takes place in the heat
exchanger. The low stage and high stage systems are balanced by design,
however, sometimes that balance can be disrupted during operation and the
unit will not function properly. If the unit is overloaded, or if the unit is
defrosted and restarted in a short time interval, system unbalance is possible.
If system unbalance occurs, turn the freeze dryer off and allow the unit to
stabilize at ambient temperature for 2 to 4 hours.
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 refrigeration technician or through an authorized Labconco service
agency.
36
Product Service 816-333-8811 or 1-800-522-7658
CHAPTER 8
MODIFYING YOUR FREEZE
DRYER DISPLAY
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 known 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.
High line limit may be raised in 5 increments of approximately 2 to
3V increments for 115V models or disabled.
Product Service 816-333-8811 or 1-800-522-7658
37
Chapter 8: Modifying Your Freeze Dryer Display
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:
PRODUCTION MENU
MASTER RESET?
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 shows:
COLLECTOR TEMP OFFSET:
OC
Press SELECT until the appropriate offset is shown. Each number
represents 1°C
38
Product Service 816-333-8811 or 1-800-522-7658
Chapter 8: Modifying Your Freeze Dryer Display
Press MENU and if the drying chamber has been installed, the display shows:
SDC TEMP. OFFSET:
OC
Press SELECT until the appropriate offset is shown. Each number represents
1°C.
Press MENU and the display shows:
VACUUM OFFSET:
O uBar
Press SELECT until the appropriate offset is shown. Each number
represents 0.001mBar.
Press MENU and the display shows:
LOW LINE OFFSET:
0
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 activates 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
activates 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
HIGH LINE OFFSET:
0
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 activates 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 activates when the voltage drops to approximately 266V,
for example. 254+(4x3)=266V. There will be no alarm indicated if
DISABLED is selected.
Product Service 816-333-8811 or 1-800-522-7658
39
Chapter 8: Modifying Your Freeze Dryer Display
Press MENU and the display shows:
DRYING CHAMBER:
NOT INSTALLED
Press and hold SELECT to change the status.
Press MENU and the display shows:
PURGE VALVE:
NOT INSTALLED
Press and hold SELECT to change the status.
Press MENU and the display shows:
DEFROST HEATER:
NOT INSTALLED
Press and hold SELECT to change the status.
Press MENU and the display shows:
MOISTURE SENSOR:
INSTALLED
Press and hold SELECT if you want to disable the moisture
sensor.
Press MENU and the display shows:
SHELL FREEZER:
NOT INSTALLED
Press and hold SELECT to change the status
Press MENU and the display shows:
HOLD SELECT TO CLEAR
ALL TOTAL HOURS?
If you want to reset Total Hours, press and hold SELECT until an audible
beep is heard. The display defaults to the main freeze dry display
information.
If you do not want to set Total Hours, press MENU and the display shows:
PRODUCTION MENU:
MASTER RESET?
40
Product Service 816-333-8811 or 1-800-522-7658
Chapter 8: Modifying Your Freeze Dryer Display
The routine repeats by pressing MENU or wait approximately 10 seconds for
the display to default to the main freeze dry information display information.
In order to store offsets in memory, you Must Press and Hold MENU until
display shows,
PASSWORD:
Wait approximately 10 seconds and the display defaults 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
41
APPENDIX A
FREEZE DRYER
COMPONENTS
The following is a list of 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.
Item
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
Models
73860xx, 73870xx
Part No.
7395800
7395801
7388400
7388401
7406600
7406601
7406602
7591805
7591806
7591807
7591805
7591806
7591807
1302300
7426000
7445500
7728000
1643600
7645900
7373450
1336400
1342100
1336500
1332601
1332701
7445400
7515300
7389402
7389403
7432700
7429700
7389700
42
Model
73820xx
Part No.
7395800
7395801
7383600
7383601
7383500
7383501
7383502
7382100
7382101
7382102
7382100
7382101
7382102
1302300
7426000
7445500
7728000
1643600
7645900
7373450
1336400
1342100
1336500
1332601
1332701
7445400
7515300
7383300
7382301
7432700
7429700
7389700
Description
Lid Gasket
Lid
Back Panel Assembly, 115V
Back Panel Assembly, 230V
Motor Fan, 115V
Motor Fan, 230V, 60 Hz
Motor Fan, 230V, 50 Hz
Compressor, 115V, 60 Hz Lo Stage
Compressor, 230V, 50 Hz Lo Stage
Compressor, 230V, 60 Hz Lo Stage
Compressor, 115V, 60 Hz Hi Stage
Compressor, 230V, 50 Hz Hi Stage
Compressor, 230V, 60 Hz Hi Stage
Switch
Control Panel Label
Printed Circuit Board
Drain Plug
O-Ring
Drain Hose
Vacuum Hose (Not Shown)
Power Cord, 115V (Not Shown) NEMA 5/20
Power Cord, 230V, 60 Hz (Not Shown) NEMA 6/20
Power Cord, 230V, 50 Hz (Not Shown) CEE 7/7
Power Cord, 230V, 50 Hz (Not Shown) BS 1363
Power Cord, 230V, 50 Hz (Not Shown) CH2-16P
Vacuum Sensor
Temperature Sensor, Collector (Not Shown)
Wire Harness, 115V (Not Shown)
Wire Harness, 230V (Not Shown)
Vacuum Control/Bleed Valve
Moisture Sensor
Wire Harness, Control, 115V & 230V (Not Shown)
Product Service 816-333-8811 or 1-800-522-7658
Appendix A: Freeze Dryer Components
Models 73860xx and 73870xx
Product Service 816-333-8811 or 1-800-522-7658
43
APPENDIX B
FREEZE DRYER
DIMENSIONS
Model 73860xx
44
Product Service 816-333-8811 or 1-800-522-7658
Appendix B: Freeze Dryer Dimensions
Model 73870xx
Product Service 816-333-8811 or 1-800-522-7658
45
Appendix B: Freeze Dryer Dimensions
Model 73820xx
46
Product Service 816-333-8811 or 1-800-522-7658
APPENDIX C
FREEZE DRYER
SPECIFICATIONS
This Appendix contains technical information about the freeze dryer
including electrical specifications, environmental operating conditions and
wiring diagrams.
Electrical Specifications
Catalog #
7386020
7386021
7386030
7386031
7386040
7386041
7386060
7386061
7386070
7386071
7387020
7387021
7387030
7387031
7387040
7387041
7387060
7387061
7387070
7387071
Voltage
Frequency
Phase
Nominal
Operating
Range
115V
100V
115V
100V
230V
230V
230V
230V
230V
230V
230V
230V
103-127
90-110
103-127
90-110
198-254
198-254
187-253
187-253
198-254
198-254
198-254
198-254
60
50
60
50
50
50
60
60
50
50
50
50
1
1
1
1
1
1
1
1
1
1
1
1
115V
100V
115V
100V
230V
230V
230V
230V
230V
230V
230V
230V
103-127
90-110
103-127
90-110
198-254
198-254
187-253
187-253
198-254
198-254
198-254
198-254
60
50
60
50
50
50
60
60
50
50
50
50
1
1
1
1
1
1
1
1
1
1
1
1
Amperage
Nominal
Max. with
w/o
Vacuum
Vacuum
Pump
Pump
11
16
11
16
11
16
11
16
5.5
10
5.5
10
5.5
10
5.5
10
5.5
10
5.5
10
5.5
10
5.5
10
11
11
11
11
5.5
5.5
5.5
5.5
5.5
5.5
5.5
5.5
Product Service 816-333-8811 or 1-800-522-7658
16
16
16
16
10
10
10
10
10
10
10
10
47
Appendix C: Freeze Dryer Specifications
Catalog #
7382020
7382021
7382030
7382031
7382032
7382033
7382034
7382035
7382040
7382041
Voltage
Nominal
Operating
Range
115V
115V
230V
230V
230V
230V
230V
230V
230V
230V
103-127
103-127
198-254
198-254
198-254
198-254
198-254
198-254
187-254
187-254
Frequency
Phase
60
60
50
50
50
50
50
50
60
60
1
1
1
1
1
1
1
1
1
1
Amperage
Nominal
Max. with
w/o
Vacuum
Vacuum
Pump
Pump
11.5
16
11.5
16
6.3
10
6.3
10
6.3
10
6.3
10
6.3
10
6.3
10
6.3
10
6.3
10
Environmental Conditions
•
•
•
•
•
•
•
•
48
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 overvoltages according to Installation Categories II
(Overvoltage 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.
Heat rejected from freeze dyer excluding the vacuum pump: Less
than 4320 BTU/HR.
Product Service 816-333-8811 or 1-800-522-7658
APPENDIX D
FREEZE DRYER
ACCESSORIES
The following accessories are available for the freeze dryer.
PART #
1472100
DESCRIPTION
Vacuum Pump
Two stage direct drive pump, 117 liters/minute. 115 VAC,
50/60 Hz, single phase, 4.6 amps. Includes Pump Exhaust Filter
1473400. (Cat. # 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
1473400. (Cat. # 1473400)
1467700
Vacuum Pump
Two stage direct drive pump, 195 liters/minute. 115 VAC,
50/60 Hz, single phase. Includes Pump Exhaust Filter.
(Cat. # 1473400)
7739403
Vacuum Pump
Two stage direct drive pump, 195 liters/minute. 230 VAC,
50/60 Hz, single phase. Includes Pump Exhaust Filter.
(Cat. # 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.
Product Service 816-333-8811 or 1-800-522-7658
49
Appendix D: Freeze Dryer Accessories
PART #
1472200
DESCRIPTION
Pump Inlet Filter
Disposable filter that prevents oil back streaming and protects
vacuum pump from submicron particles. Fits Vacuum Pumps
1472100 and 7739402.
1473400
Pump Exhaust Filter
Disposable filter that removes visible oil mist and odor from
vacuum pump exhaust. Fits Vacuum Pumps 1472100 and
7739402.
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 1472100
and 7739402.
1988000
Vacuum Pump Oil, 1 Liter
A molecularly distilled hydrocarbon oil with low vapor pressure.
For Vacuum Pumps 1472100 and 7739402.
7772000
Soda Acid Trap
Secondary trap that prevents migration of corrosive chemicals into
vacuum pump.
7772100
Replacement Media for Soda Acid Trap
7772700
Vacuum Pump Oil, 1L
A mineral oil with low vapor pressure.
For Vacuum Pumps 7438700, 7438800, 7769600, 7769800.
7670400
Replacement Filter Element
Disposable filter that removes oil mist from the vacuum pump
exhaust.
Fits Vacuum Pumps 7438700, 7438800, 7469600 and 7469800.
7584300
Vacuum Pump Oil
For Hybrid vacuum pumps 7584000, 7584002.
7772500
Carbon Solvent Trap
Secondary trap that prevents migration of organic solvents into
vacuum pump.
50
Product Service 816-333-8811 or 1-800-522-7658
Appendix D: Freeze Dryer Accessories
PART #
7772600
DESCRIPTION
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.
7509200
Product Heater, 115V
For use in chamber 7522800. Provides 3 heated shelves operating
at 43°C (110°F).
7509201
Product Heater, 230V
For use in chamber 7522800. Provides 3 heated shelves operating
at 43°C (110°F).
7443500
Clear Drying Chamber with 8 Valves
For bulk drying or drying in flasks.
7442100
Drying Rack- Unheated
Provides three shelves. For use in Chambers 7443500 and
7522800.
7442900
Clear Drying Chamber
For bulk drying.
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.
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.
7522900
16 Port Drying Chamber
13" high x 138" diameter, 304 stainless steel with 16 freeze dry
valves.
Product Service 816-333-8811 or 1-800-522-7658
51
Appendix D: Freeze Dryer Accessories
Serum Bottles and Vials
Threaded Vials
Stoppers and threaded vials with Screw
Caps are supplied in packages of 200.
Perfect for long term storage of freeze
dried samples. Labconco Serum
Bottles and Treaded Vials are
specifically designed for lyophilization
applications. Their uniform thin wall
construction ensures even freezing
and drying. Bottles and vials are ideal
containers for use in the FreeZone
Stoppering Tray Dryer. Serum bottles
also connect to valve ports on drying
chambers and manifolds.
Serum Bottles
2 ml
3 ml
5 ml
10 ml
20 ml
30 ml
50 ml
100 ml
125 ml
52
20 mm
Corkage
7573010
7573210
7573410
7573610
7573810
7574010
7574210
Vials with
Screw Caps
Stoppers
5 ml
10 ml
7762300
7762600
7762200
7762200
Seal Crimper
Serum Bottles, Stoppers and seals
are supplied in packages of 100.
Size
Size
Secures tear-away Aluminum Seals.
7578000 Seal Crimper for 13 mm corkage.
Shipping weight 3 lbs. (1.4 kg)
7578100 Seal Crimper for 20 mm corkage.
Shipping weight 3 lbs. (1.4 kg)
13 mm
Corkage
Split
Stoppers
Aluminum
Seals
Sleeve-Type
Stoppers
7575010
7575210
7576010
7576010
7576210
7576210
7576210
7576210
7576210
7576210
7576210
7577010
7577010
7577110
7577110
7577110
7577110
7577110
7577110
7577110
757710
7577510
7577510
7577510
7577510
7577510
7577510
Product Service 816-333-8811 or 1-800-522-7658
Appendix D: Freeze Dryer Accessories
Fast-Freeze® Flasks
Fast-Freeze Flasks are specially designed to be
easier to handle, faster to load and more
convenient to use than other freeze dry
glassware now in your laboratory. Compatible
with all major brands of laboratory freeze dry
equipment, Fast-Freeze Flasks eliminate the risk
of contamination from vacuum grease, reduce
spillage of valuable samples and require no
washers, gaskets or retainers.
How to select Fast-Freeze Flasks for your
Freeze Dry System
Select fast-Freeze Flasks based on your sample
sizes. Flasks should be filled no more than onethird of their volume so that maximum surface
area is achieved and efficient lyophilization is
assured. A complete Fast-Freeze Flask includes
a rubber top, glass bottom and a supply of filter
paper. Tops, bottoms and filter paper are
available separately as replacement
components. Adapters are required to attach
flasks to freeze dry valve ports.
Flask
Size
Complete
Flask
Flask
Bottom
Flask
Top
Flask Top
Adapter
Diameter*
Dimensions/
Flask Bottom
HxD
40 ml
80 ml
120 ml
150 ml
300 ml
600 ml
750 ml
900 ml
1200 ml
2000 ml
7540000
7540200
7540300
7540400
7540600
7540800
7541100
7540900
7541000
7541200
7542000
7542200
7542300
7542400
7542600
7542800
7542700
7542900
7543000
7543200
7544000
7544000
7544200
7544200
7544200
7544400
754400
7544400
7544400
7544400
½"
½"
¾"
¾"
¾"
¾"
¾"
¾"
¾"
¾"
76mm 34mm
115mm x 34mm
68mm x 59.2mm
85mm x 59.2mm
145mm x 59.2mm
135mm x 90.2mm
162mm x 90.2mm
190mm x 90.2mm
240mm x 90.2mm
380mm x 90.2mm
*Valves on the freeze dry system, drying chambers and manifolds offered in this catalog fit
adapters of both ½" and ¾" sizes. Size information is provided for selecting adapters for older
Labconco models and other freeze dryers.
Adapters
Add the adapters for connecting the
Fast-Freeze Flasks to the valve ports on
your drying chamber or manifold.
Choose borosilicate glass or stainless
steel adapters in ½" and ¾" diameters.
7544810 Replacement Filter Paper
1000 (10 packages of 100). 1" diameter
(28mm). Pore size 17 micron. Shipping
weight 0.5lb.
Product Service 816-333-8811 or 1-800-522-7658
53
Appendix D: Freeze Dryer Accessories
Lyph-Lock® Flasks
Lyph-Lock Flasks simplify your
Lyophilization procedures because they
have only three pieces per flask – a high
strength borosilicate glass top and
bottom with a silicone rubber ring seal.
The unique wide-mouth design helps you
load samples easily and lyophilize
efficiently.
How to select Lyph-Lock Flasks for
your Freeze Dry System
Select Lyph-Lock Flasks fast- based on
your sample sizes. Flasks should be filled
no more than one-third of their volume so
that maximum surface area is achieved
and efficient lyophilization is assured. A
complete Lyph-Lock Flask includes a
glass top and bottom and a rubber ring
seal. Tops, bottoms and seals are
available separately as replacement
components. Adapters are required to
attach flasks to freeze dry valve ports.
Adapters
Add the adapters for connecting the
Lyph-Lock Flasks to the valve ports on
your drying chamber or manifold.
90° Bend
Adapter
7568000
7568200
7568400
7568600
25 ml
Complete
Flask
19/38 STj
7550000
Complete
Flask
24/40 STj
7550000
50 ml
7550200
7554200
100 ml
250 ml
7550400
7550600
Flask Size
Description
Connects 19/38 STj Flask Top to ½"
valve*
Connects 19/38 STj Flask Top to
3/4"valve*
Connects 24/40 STj Flask Top to ½"
valve*
Connects 24/40 STj Flask Top to 3/4"
valve*
Dimensions/
Flask Bottom
H x ID
37mm x 34mm
Flask Top
19/38 STj
Flask Top
24/40 STj
Lyph-Lock
Seal
Flask
Bottom
7552000
7556000
7559000
7557000
7552000
7556000
7559000
7557200
67mm x 34mm
7554400
7554600
7552200
7552200
7556200
7556200
7559200
7559200
7557400
7557600
50mm x 59.2mm
110mm x 59.2mm
103mm x 90.2mm
500 ml
7550800
7554800
7552400
7556400
7559400
7557800
750 ml
7550900
7554900
7552400
7556400
7559400
7557900
145mm x 90.2mm
1000 ml
7551000
7555000
7552400
7556400
7559400
7558000
187mm x 90.2mm
*Valves on the freeze dry system, drying chambers and manifolds offered in this catalog fit adapters of
both ½" and ¾" sizes. Size information is provided for selecting adapters for older Labconco models
and other freeze dryers.
54
Product Service 816-333-8811 or 1-800-522-7658
Appendix D: Freeze Dryer Accessories
Ampules
Oxygen/Natural Gas Sealing Torch
7578500 Torch specifically designed for
flame sealing freeze dry ampules. Seals
all types of heat-resistant glass. Connects
to natural gas, butane or propane and
oxygen with ¼" ID hose connectors.
Shipping weight 3 lbs. (1.4 kg).
Labconco Ampules are fabricated of
highest quality borosilicate glass for
strength and durability. They are available
in five different configurations to provide
the ideal ampule for your specific
lyophilization requirements, from tray
drying to flame sealing applications.
Ampules
Ampules are supplied in packages of 100.
Size
Straight
1 ml
2 ml
4 ml
5 ml
10 ml
25 ml
50 ml
7572710
Pre-Scored
Flat Bottom
7570610
7570810
7571010
7571210
Ampule Valve Adapters
7593401 Adapter connects ampules
to valve ports or stainless steel
stems. Ten per package. Shipping
weight 0.5 lbs. (0.2 kg).
Trident Adapter
7762700 Three Way Adapter permits attachment of three
ampules to a single valve port. Ampules are attached
using Ampule Valve Adapters or 1/8" surgical tubing (not
provided). Cavity in adapter body can be filled with cotton
fiber media to help prevent contamination between
samples. Shipping weight 3 oz. (0.1 kg).
Product Service 816-333-8811 or 1-800-522-7658
55
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Product Service 816-333-8811 or 1-800-522-7658
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