Labconco Labconco-7343200-rev-j-console-freeze-dryers FreeZone Console Freeze Dryer User's Manual
Original instructions
Models
70061**** 6L -50C Series
71061**** 6L -84C Series
70121**** 12L -50C Series
71121**** 12L -84C Series
70181**** 18L -50C Series
Original instructions
Copyright © 2018 Labconco Corporation. The information contained in this manual and the accompanying
products are copyrighted and all rights reserved by Labconco Corporation. Labconco Corporation reserves
the right to make periodic design changes without obligation to notify any person or entity of such change.
Returned or Damaged Goods
Do not return goods without the prior authorization from Labconco. Unauthorized returns will not be
accepted. If your shipment was damaged in transit, you must file a claim directly with the freight carrier.
Labconco Corporation and its dealers are not responsible for shipping damages.
The United States Interstate Commerce Commission rules require that claims be filed with the delivery
carrier within fifteen (15) days of delivery.
Limitation of Liability
The disposal and/or emission of substances used in connection with this equipment may be governed by
various federal, state, or local regulations. All users of this equipment are required to become familiar with
any regulations that apply in the user’s area concerning the dumping of waste materials in or upon water,
land, or air and to comply with such regulations. Labconco Corporation is held harmless with respect to
user’s compliance with such regulations.
Contacting Labconco Corporation
If you have questions that are not addressed in this manual, or if you need technical assistance, contact
Labconco’s Customer Service Department or Labconco’s Product Service Department at 1-800-821-5525
or 1-816-333-8811, between the hours of 7:30 a.m. and 5:30 p.m., Central Standard Time.
Part #7343200, Rev. J
ECO N290
Warranty
Labconco Corporation provides a warranty to the original buyer for the repair or replacement of parts and
reasonable labor as a result of normal and proper use of the equipment with compatible chemicals. Broken
glassware and maintenance items, such as filters, gaskets, light bulbs, finishes and lubrication are not
warranted. Excluded from warranty are products with improper installation, erratic electrical or utility supply,
unauthorized repair and products used with incompatible chemicals.
The warranty for FreeZone® Freeze Dry Systems will expire one year from date of installation or two years
from date of shipment from Labconco, whichever is sooner. Warranty is non-transferable and only applies to
the owner (organization) of record.
Buyer is exclusively responsible for the set-up, installation, verification, decontamination or calibration of
equipment. This limited warranty covers parts and labor, but not transportation and insurance charges. If the
failure is determined to be covered under this warranty, the dealer or Labconco Corporation will authorize
repair or replacement of all defective parts to restore the unit to operation. Repairs may be completed by 3rd
party service agents approved by Labconco Corporation. Labconco Corporation reserves the rights to limit this
warranty based on a service agent’s travel, working hours, the site’s entry restrictions and unobstructed access
to serviceable components of the product.
Under no circumstances shall Labconco Corporation be liable for indirect, consequential, or special damages
of any kind. This warranty is exclusive and in lieu of all other warranties whether oral, or implied.
Original instructions
TABLE OF CONTENTS
CHAPTER 1: INTRODUCTION 1
Intended Use 1
Typographical Conventions 1
Safety Information 2
Freeze Dry Process 3
Freeze Dry Rates 3
Freeze Dry Capacity 4
Samples Containing Volatile Substances 5
About This Manual 5
CHAPTER 2: PREREQUISITES 6
Electrical Requirements 6
Location Requirements 7
Vacuum Pump Requirements 7
Chamber or Manifold Requirements 7
CHAPTER 3: GETTING STARTED 8
Unpacking Your Freeze Dryer 8
Freeze Dryer Components 9
Setting Up Your Freeze Dryer 9
Component Identification 10
Vacuum Pump Connection 11
Electrical Connection 12
Baffle Installation 12
Drying Chamber or Manifold Installation 14
Chemical Resistance of Freeze Dryer Components 15
Solvent Safety Precautions 16
CHAPTER 4: LYO-WORKS™ OPERATING SYSTEM 17
Control Panel 17
Initial Power Up 18
Touch Screen Operation 18
Home Screen 18
Main Menu Icons 19
Moving Between Menu Screens 19
Function Indicator Bar 19
System Parameters Display 19
Original instructions
Operation Buttons 20
Programs Screen 21
Data Logging Screen 23
Settings Screen 24
Language 24
Time & Date 24
Units 25
Security 25
Alerts 25
Configure Email Settings 26
Maintenance 28
Vacuum Pump Settings 28
Refrigeration System Settings 28
Freeze Dryer Line Voltage Offset 28
Vacuum Pump Protection 28
Calibration 29
Display 30
Network 31
Sensors Screen 32
Drying Accessory Screen 32
End Point Detection Screen 33
Help Screen 34
About 34
Diagnostics 34
Resources 34
Backup/Restore 35
CHAPTER 5: USING YOUR FREEZE DRYER 36
Operation Checklist 36
Vacuum Pump Ballast Setting 37
Purge Valve (optional feature) 37
Operating the Freeze Dryer 37
Auto Start-Up (without Purge Valve option) 37
Auto Start-Up (with Purge Valve option) 38
Manual Start-Up 38
Setting the Operating Vacuum Level 38
Pre-Freezing Samples 39
Adding Sample 39
Starting a Program 40
Shut Down 41
Defrosting 41
Operating the Shell Freezer (optional feature) 42
Operating the Mini Chamber (optional feature) 43
Alerts 44
Power Fail 44
Line Voltage Range 44
Collector Temp 44
Collector Moisture 44
Original instructions
Service Vacuum Pump 45
Vacuum Leak 45
Vacuum Set Point 45
Status Email Messages 45
End Point Detection 45
System Temp Variation 45
System Temp Set Point 45
Shelf Temp Variation 45
Shelf Temp Set Point 46
Power Fail 46
Program Complete 46
Copy (export) a Data Log File 46
Downloading Data Log Files via Ethernet 46
Copy a Program 47
CHAPTER 6: MAINTAINING YOUR FREEZE DRYER 48
Service Safety Precautions 48
Routine Maintenance Schedule 48
CHAPTER 7: TROUBLESHOOTING 50
Vacuum Pump 50
Gaskets, Tubing, Connections, Sample Valves 51
System Components & Collector Chamber Isolation 53
Refrigeration Module Operation 55
APPENDIX A: FREEZE DRYER COMPONENTS 56
APPENDIX B: FREEZE DRYER DIMENSIONS 61
APPENDIX C: FREEZE DRYER SPECIFICATIONS 62
Electrical Specifications 62
Environmental Conditions 63
APPENDIX D: FREEZE DRYER ACCESSORIES 64
Product Service 816-333-8811 or 1-800-522-7658
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Original instructions
CHAPTER 1
INTRODUCTION
Congratulations on your purchase of a Labconco FreeZone® Freeze Dry System,
which is designed for laboratory lyophilization procedures. The refrigerant used in
the refrigeration system is HCFC-free so it will not endanger the environment.
The unit is easy to install and maintain. Proper care and maintenance of this
product will result in many years of dependable service.
Intended Use
The Labconco Freeze Dryers described in this manual are intended for laboratory
use to facilitate the lyophilization process.
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.
!
Chapter 1: Introduction
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Original instructions
Safety Information
For Hydrocarbon Refrigeration Only See Below:
• DANGER – Risk of fire or explosion. Flammable refrigerant used. Do not
use mechanical devices to defrost refrigerator. Do not puncture refrigerant
tubing.
• DANGER – Risk of fire or explosion. Flammable refrigerant used. To be
repaired only by trained service personnel.
• WARNING – Keep all ventilation openings in the enclosure or, in the
structure for building-in, clear of obstruction.
• CAUTION – Risk of fire or explosion. Flammable refrigerant used.
Consult repair manual/owner’s guide before attempting to service this
product. All safety precautions must be followed.
• CAUTION – Risk of fire or explosion. Dispose of properly in accordance
with federal or local regulations. Flammable refrigerant used.
• CAUTION – Risk of fire or explosion due to puncture of refrigerant
tubing. Follow handling instructions carefully. Flammable refrigerant
used.
Replacement components and servicing
• Component parts shall be replaced with like components.
• Servicing shall be performed by authorized service personnel to minimize
the risk of possible ignition due to incorrect parts or improper service.
!
!
Chapter 1: Introduction
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Original instructions
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.
A listing of selected materials and their approximate drying times are shown in
Table 1 for your reference.
SAFE TEMPERATURE AND DRYING TIMES
FOR SELECTED MATERIALS
Material
10mm Thick
Safe
Temperature
°C
Collector
Temperature
°C
Hours
(Approx.)
Milk
-5
-40
10
Urea
-7
-40
10
Blood Plasma
-10 to -25
-40
16
Serum
-25
-40
18
Vaccinia
-30 to -40
-50
22
Influenza Vaccine
-30
-50
24
Human Tissue
-30 to -40
-50
48
Vegetable Tissue
-50
-80
60
*Total sample quantities are contingent on various freeze dryer capacities.
Table 1
Chapter 1: Introduction
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Original instructions
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.
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
Chapter 1: Introduction
Product Service 816-333-8811 or 1-800-522-7658
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Original instructions
temperature decreases, the vapor pressure decreases but the rate of heat absorption
by the sample does not change. This tends to promote melting of the sample,
which leads to a marked increase in vapor pressure and ultimately overloads the
collector and vacuum pump. Samples that have eutectic temperatures of –20°C or
lower should be placed on the freeze dry system one flask at a time so that the
vacuum in the system may recover before adding another sample to the system. If
the vacuum does not recover, the capacity of the freeze dry system has been
exceeded and the sample should be removed.
If there is a problem with a particular type of sample melting when placed on the
freeze dry system, dilution of the sample with more water or providing some
insulation around the flask to decrease the rate of heat absorption by the sample
may help. If the eutectic temperature of the sample is –40 to –60°C, the freeze dry
system selected for use must be equipped with cascade type refrigeration so that
the collector temperature can be cooled to below –75°C, or a dry ice/solvent trap
may be used between the collector and the vacuum pump.
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.
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Original instructions
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:
• Electrical supply requirements.
• Vacuum pump requirements.
Refer to Appendix C: Freeze Dryer Specifications for complete Freeze Dryer
electrical and environmental conditions, specifications and requirements.
Electrical Requirements
• 115V models
o 20 Amp dedicated single phase circuit.
o Properly grounded receptacle for
NEMA 5-20P plug.
• 230V models
o 15 Amp dedicated single phase circuit.
o Properly grounded receptacle that matches the plug supplied with
the unit, (230V models are supplied with one of the following
plugs):
US EU China UK India
(NEMA 6-15P)
o If the plug does not match the available receptacle, remove the plug
and replace it with an approved plug of the suitable style.
US
NEMA 5-20P
Chapter 2: Prerequisites
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Original instructions
Do not use any detachable power cord that is not adequately
rated for the unit.
Frequency must agree with the serial tag rating.
Improper frequency will damage the compressor.
ADDITIONAL APPLIANCES ON THE SAME CIRCUIT MAY
CAUSE THE CURRENT TO EXCEED THE RATING OF THE
CIRCUIT BREAKER OR FUSE.
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 side panels and exhausts it through the back panel. 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.
Refer to Appendix B: Freeze Dryer Dimensions for dimensional drawings of 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 0.007 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 vacuum set point, 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 (included with 230V pumps purchased from Labconco).
This will allow the vacuum pump to be plugged into the receptacle on the back
panel of the freeze dryer.
Chamber or Manifold Requirements
A freeze drying chamber or manifold is not included and must be purchased
separately. These accessories allow samples to be attached to the Freeze Dryer.
See Chapter 3: Getting Started for installation instruction.
!
!
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Original instructions
CHAPTER 3
GETTING STARTED
Now that the site for your Freeze Dryer is properly prepared, you are ready to
unpack, inspect, install and test your Freeze Dryer. Read this chapter to learn how
to:
• Unpack and move your Freeze Dryer.
• Set up your Freeze Dryer.
• Connect the electrical supply source to your Freeze Dryer.
• Properly exhaust your Freeze Dryer.
• Safely use solvents with your Freeze Dryer.
The FreeZone Console Freeze Dryer may weigh up to 330 lbs
(150 kg) depending on the model. 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.
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.
!
The United
States
Interstate
Commerce
Commission
rules require
that claims be
filed with the
delivery carrier
within fifteen
(15) days of
delivery.
Chapter 3: Getting Started
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Original instructions
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
Verify that the components listed below are present and undamaged.
(1) Freeze Dryer
(1) Collector Chamber Lid Assembly
o Acrylic Lid Assembly for -50C models
o Stainless Steel Lid Assembly for -84C models
(1) Mini Chamber Lid (if equipped)
(1) Shell Freezer Lid (if equipped)
6L
12L
18L
Part #
Description
Comments
1 1 1
1089005
User’s Manual
USB Flash Drive
1 1 1 Power Cord
See parts list (Appendix A)
1 1 1
7373436
Vacuum Hose
2 2 2
1488800
Hose Clamp
1
7213200
Baffle 6L (SSTL)
-84C SSTL Models
1
7213201
Baffle 6L (PTFE)
-84C PTFE Models
1
7213300
Baffle 12L (SSTL)
-84C SSTL Models
1
7213301
Baffle 12L (PTFE)
-84C PTFE Models
1
7390700
Baffle 18L (SSTL)
-50C SSTL Models
1
7390703
Baffle 18L (Polypro)
-50C PTFE Models
1 1 1
7205304
Drain Hose
If you did not receive one or more of the components listed for your Freeze Dryer,
or if any of the components are damaged, contact Labconco Corporation
immediately for further instructions.
Setting Up Your Freeze Dryer
After you verify receipt of the proper components, move your Freeze Dryer to the
location where you want to install it. Then, follow the steps listed below.
Chapter 3: Getting Started
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Original instructions
Component Identification
USB port
Vacuum Pump
Viewing Window
Power Inlet
Vacuum Pump Outlet
Quick-Connect drain coupling(s)
Upper = Shell Freezer (if equipped)
Lower = Collector Chamber
Circuit Breaker Reset
Touch Screen Display
On/Standby Button
& LED Indicator
Serial Tag (& Elect. Rating)
Collector Chamber
& Coil
3” Vacuum Port
Shell Freezer or
Mini Chamber
(if equipped)
Chapter 3: Getting Started
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Original instructions
Vacuum Pump Connection
A vacuum pump (as described in Chapter 2: Prerequisites) is required to operate
your Freeze Dryer properly. The Freeze Dryer is equipped with a 3/4" ID 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.
1. Remove the front left stainless steel panel and
lower rear panel from the Freeze Dryer.
2. Remove protective caps from inlet and outlet
ports of vacuum pump.
3. Place the vacuum pump inside the console
Freeze Dryer.
4. Some vacuum pumps have inlet fittings that
clamp to the pump. Place the centering ring
with filter screen on the inlet fitting.
5. Place the hose barb fitting on top of the
centering ring and secure with the clamp.
6. CHECK THE VACUUM PUMP OIL LEVEL.
Fill the pump with oil so the level is between
the lines on the sight gauge on the end of the
pump housing.
7. Attach one end of the vacuum hose to the port
inside the Freeze Dryer and the other end to the
inlet port of the vacuum pump with the hose
clamps provided. If necessary, cut the hose to
proper length to allow for gentle bends without
kinks.
!
Hose Barb
Clamp
Inlet Fitting
Vacuum Pump
Inlet Port
Console
Inlet Port
Chapter 3: Getting Started
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Original instructions
8. VERIFY THE VACUUM PUMP VOLTAGE SETTING AGREES WITH
THE FREEZE DRYER VOLTAGE SHOWN ON THE SERIAL
NUMBER LABEL. Reconfigure if necessary (see vacuum pump
instructions).
9. Connect the vacuum pump power cord to the receptacle labeled “vacuum
pump” on the back of the Freeze Dryer. Models rated for use on 230V
have a reverse IEC receptacle for attaching the vacuum pump power cord.
10. If the vacuum pump has an ON/OFF switch, turn the switch ON. The
vacuum pump will be controlled by the Freeze Dryer.
IT IS HIGHLY RECOMMENDED THAT AN OIL MIST
EXHAUST FILTER BE INSTALLED ON ROTORY VANE
VACUUM PUMPS TO MINIMIZE OIL MIST EXITING THE
PUMP. AN OIL RETURN KIT CAN ALSO BE USED IN
CONJUNCTION WITH THE EXHAUST FILTER TO RETURN
TRAPPED OIL BACK TO THE VACUUM PUMP.
Electrical Connection
Make sure that the outlet that you intend to use meets the voltage and amperage
requirements listed on the serial tag of the Freeze Dryer. Plug the power cord into
the receptacle on the back of the Freeze Dryer and plug the other end into a
suitable power outlet. It will take approximately 90 seconds for the operating
system to fully load.
Baffle Installation
A baffle is shipped with 6 & 12L -84C Freeze Dryers and 18L -50C Freeze Dryers
(Models 71061xxxx, 70121xxxx & 70181xxxx). The 6 & 12L models come with
a 2 piece baffle (stainless steel cylinder with a plastic top). The 18L models come
with a one piece baffle (either stainless steel or polypropylene). The baffles are
designed to evenly distribute collected ice over the entire collector coil. Proper
positioning of the baffle is required to achieve maximum ice loading capabilities.
6 & 12L Baffle
1. Place the baffle into the collector chamber. The cylinder should be
concentric (centered) with the collector chamber.
2. Align the 1.75” hole in the rear channel of the baffle with the 1.5” vacuum
port in the side wall of the collector chamber.
Chapter 3: Getting Started
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Original instructions
18L Baffle
1. Place the baffle into the collector chamber.
2. Position the baffle so that the arrow points directly toward the front.
18L Baffle Top View
Align hole in baffle channel
with rear vacuum port
Properly Installed
6 & 12L Baffle
Chapter 3: Getting Started
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Original instructions
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.
4 or 8 Port Manifold Installation
12 or 16 Port Drying Chamber Installation
7307300 GASKET
7307300 GASKET
7742800 SPACER
7206400 THUMB SCREW
MANIFOLD
CONSOLE
FREEZE DRYER
7202300 SADDLE BRACKET
GASKET
DRYING CHAMBER
SPACER(SSTL)
LATCH
DRYING CHAMBER
LID
Chapter 3: Getting Started
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Original instructions
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:
Acids
Buffers Solvents
Component
Material
Acetic Acid 20% Formic Acid Trifluoroacetic Acid (TFA)
Calcium Chloride Sodium Phosphate
Acetone Acetonittirle Carbon Tetrochloride Cyclohexane Dioxane Methyl t
-Butyl Ether (BTBE)
Pyridine
Valve Stem
Acetal
C D D D D
Collector
Lid
Acrylic
D D D D
Hoses,
Gaskets &
Valve
Bodies
Neoprene
C D D C C D D D C
D
Flask Top
Silicon
Rubber
C D D D D D C D Chamber &
Fittings
Stainless
Steel
C
C – Moderate degradation; Limited use
D – Severe degradation; infrequent use recommended; immediate thorough
cleaning required.
• Most common compounds used in freeze drying processes, if allowed to enter
the vacuum pump, will degrade the oil and cause damage to the vacuum pump.
• Sugars and proteins typically will have minimal negative effect on any of the
materials of construction.
When using compounds in the Freeze Dryer that are hostile to the materials of
construction, it is imperative the equipment is thoroughly cleaned after use.
• Rubber and plastic components that have been exposed to damaging
compounds should be removed and flushed with water.
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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. 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: labconco@labconco.com.
Solvent Safety Precautions
Solvents used in the Freeze Dryer may be flammable or
hazardous to your health. Use extreme caution and keep
sources of ignition away from the solvents. When using
flammable or hazardous solvents, the vacuum pump must be
vented to or operated inside a fume hood.
Hazardous materials such as strong acids or bases, radioactive
substances and volatile organics must be handled carefully and
promptly cleaned up if spilled. If a sample is spilled in the
collector chamber it must immediately be cleaned up.
WARNING: The disposal of substances used in connection with
this equipment may be governed by various Federal, State or
local regulations. All users of this equipment are urged to
become familiar with any regulations that apply in the user’s
area concerning the dumping of waste materials in or upon
water, land or air and to comply with such regulations.
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CHAPTER 4
LYO-WORKS™ OPERATING SYSTEM
After your Freeze Dryer has been installed as detailed in Chapter 3: Getting
Started, read this chapter to learn how to:
• Operate the controls.
• Understand the display.
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.
Control Panel
The control panel for the Freeze Dryer is shown below with a description of its
functions.
1. Touch Screen Display – Capacitive touch screen displays system operating
parameters, set-up parameters and alarm messages. All user interface will take
place via the touch screen.
!
2 3 1
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2. On / Standby Button – If the display is illuminated pressing this button will
put the display into low power mode (display backlight will be turned off). If
the display is in low power mode, pressing this button will illuminate the
display (Note: the display can also be brought out of low power mode by
touching any location on the screen).
3. On / Standby LED Indicator – Blue LED indicator light to designate the
current status of the system.
o 1 flash per second = Initial power up (loading operating system)
o Slow pulse = Touch screen in low power mode (screen timeout)
o ON = Unit is plugged in and touch screen is in active mode
o Off = Unit is unplugged
Initial Power Up
When the Freeze Dryer is initially plugged into a power source, the On / Standby
LED will begin flashing (1 flash per second). The display will remain OFF for the
first 10 to 15 seconds, then the FreeZone animated graphics will appear. It will
take approximately 90 seconds for the operating system to fully load.
Touch Screen Operation
Home Screen
After initial power up, the Home screen will be displayed. Most of the general
operation and system monitoring can be done from the Home screen.
Indicator Bar
Time / Date
Operation
Buttons
Menu
Line 2
Line 1
Line 3
Line 4
Line 5
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Main Menu Icons
Menu icons are displayed across the top of the screen. Their descriptions from left
to right are as follows:
1. Home
2. Programs
3. Data Logging
4. Settings
5. Sensors
6. Drying Accessory
7. End Point Detection
8. Help
Moving Between Menu Screens
You can move between menu screens by either touching the menu icons or
swiping across the screen from left to right or right to left.
The Following system parameters are displayed in the center portion of the screen:
Function Indicator Bar
A thin blue indicator bar will appear under the icon of the menu screen that is
currently being displayed. The same type of indicator bar will appear above the
operation buttons to signify if each function is ON or OFF.
System Parameters Display
Line 1
COLLECTOR & VACUUM HEADING – Describes the measurement
that is displayed directly below the text.
Line 2
COLLECTOR MEASUREMENT- Displays the temperature of the
collector coil in °C or °F (as selected in Settings). The value displayed
will be RED if the temperature is:
> -40° C (for -50C models)
> -60° C (for -84C models)
> -75° C (for -105C models)
The value displayed will be GREEN if the temperature is:
≤ -40° C (for -50C models)
≤ -60° C (for -84C models)
≤ -75° C (for -105C models)
VACUUM MEASUREMENT– Displays the Freeze Dryer vacuum level
in mbar, Pa, or Torr (as selected in Settings). The display will read “High”
if the vacuum level is > 5 mbar. If the vacuum level is ≤ 5 mbar, a
numerical value will be displayed. The value displayed will be RED if the
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vacuum is > 1.500 mbar. The value displayed will be GREEN is the
vacuum is ≤ 1.500 mbar.
Line 3
Shell Freezer or Mini Chamber (factory installed options) – Only one
of these two options may be installed on a single Console Freeze Dryer. If
your Freeze Dryer has either of these two options installed, the left hand
side of Line 3 will show the current measurement from its temperature
sensor.
Vacuum Set Point – Displays the current vacuum set point in mbar, Pa, or
Torr (as selected in Settings) on the right hand side of Line 3.
Line 4
Operation Mode – Indicates the current status of the Freeze Dryer. One of
the following will always be displayed on this line:
1. Standby – Collector and Vacuum are both OFF
2. Manual – Collector and/or Vacuum are ON, but no Program is
currently running.
3. Program – If a program is currently running this line will
display the actual Program Name, Step #, and Time Remaining
(hh:mm) in the current step of the program.
4. Defrost – Defrost will be displayed when the hot gas defrost
function is turned ON.
Line 5
Data Logging Status – On or Off
Operation Buttons
Operation buttons are displayed across the bottom of the Home screen.
• AUTO – Use this button to initiate an auto start up sequence.
When auto start is initiated the refrigeration system (collector)
will be started immediately, and the vacuum pump will start when
the collector temperature has cooled down to -40° C.
• COLLECTOR/DEFROST – Use this button to turn the collector
ON/OFF or turn the Defrost ON/OFF. The wording on this button will
change from COLLECTOR to DEFROST depending on whether the
defrost function is currently running. The defrost function will turn off
automatically if the collector temperature reaches +60°C or if defrost has
been running for 2 hours.
• VACUUM – Use this button to turn the vacuum pump ON/OFF or change
the vacuum set point value.
• PURGE – Use this button to turn the purge valve ON/OFF.
• SHELL FREEZER or MINI CHAMBER – Use this button to turn the
Shell Freezer or Mini Chamber ON/OFF and to change the temperature set
point value for the Mini Chamber.
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Programs Screen
The Programs screen will allow you to create and store programs that are used to
control the shelf temperature and vacuum level. When no program has been
selected the “New” button will be the only active button along the bottom of the
screen. A program can be selected from the program list by pressing the program
name. When a program has been selected, the program row will be highlighted
(blue). With a program selected, the rest of the buttons along the bottom of the
screen will become active (Start, Edit/View, Copy & Delete).
• New – Use this button to add a new program to the program list. The new
program name will be defaulted to a two-digit sequential number (starting
with “Program 01”) that will be incremented as new programs are added to
the list (i.e., Program 02, Program 03…). The default name can be edited
as desired in the New or Edit/View screen.
• Start/Stop – Use this button to start or stop a program. The wording on
this button will change from “Start” to “Stop” depending on whether a
program is currently running.
A DRYING ACCESSORY MUST BE ATTACHED TO THE FREEZE
DRYER (VIA THE COMMUNICATION CABLE) TO RUN A
PROGRAM. IF NO DRYING ACCESSORY IS ATTACHED TO THE
FREEZE DRYER, THE START BUTTON WILL BE INACTIVE.
• Edit/View – Use this button to Edit or View the parameters of a saved
program (the wording on this button will change from “Edit” to “View”
depending on whether the program is locked or unlocked for editing.
• Copy – Use this button to Copy a selected program. The default name will
be “Program Name_copy”. The program name can be edited as desired.
• Delete – Use this button to delete a saved program from the list.
When a program is currently in progress, a “running man” icon will appear to the
left side of the program name. If the running program is selected (highlighted), the
“Stop” button will be active, and the “Delete” button will be inactive.
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“New” program
When the “New” button is selected, one of the following program templates will
be displayed, depending on the type of accessory connected to the Freeze Dryer.
Bulk TD, Tray Dryer, Heated Product Shelves Stoppering Tray Dryer
Pressing the program name field will allow you to edit the program name. The
“Add” button will add a new Step to the program and take you through a series of
screens to set the Ramp Rate, Shelf Temp., Time, and Vacuum. Values can be
edited by pressing any of the cells. Pressing the “Delete” button will delete the
selected step from the program. Changes will not be saved until the “Save” button
is pressed. Pressing the “Back” button will return to the Programs screen without
saving changes.
• Ramp Rate – (Stoppering Tray Dryer only) This allows the temperature
of the system to be increased or decreased at any desired rate within the
capacity of the heating and cooling systems of the Stoppering Tray Dryer.
Without samples on shelves, the system is capable of cooling at a rate of
approximately 0.5°C/min and can heat at approximately 1.3°C/min. The
cooling ramp rate may be slower as the temperature approaches –40°C.
Ramp Rate may be set anywhere from 0.1°C to 1.5°C/min.
• Shelf Temp. – Stoppering Tray Dryers may be set anywhere from +40°C
to –40°C in 1°C increments. There is also a Max Cold (MC) setting that
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will turn off the heater control and allow the system to reach its lowest
possible temperature (approximately -45°C). Bulk Tray Dryer, Small Tray
Dryer & Heated Product Shelves may be set from -20°C to +60°C
• Time – This time represents how long the system will hold at the Shelf
Temp. that has been programmed for each Step. The time can be set from
00:01 to 99:59 (1 min to 99 hrs 59 min). It can also be set to an indefinite
amount of time, which is represented by the infinity symbol (∞).
• Vacuum – Vacuum control can be set from 0.000 to 1.500 mbar.
Data Logging Screen
If no data log file has been selected the “New” button will be the only active
button along the bottom of the screen. A data log file can be selected from the list
by pressing the data log file name. When a data log file has been selected, the row
will be highlighted (blue). With a data log file selected, the rest of the buttons
along the bottom of the screen will become active (View, Chart, Export & Delete).
If a data log file is currently running (collecting data), the “running man” icon will
appear to the left of data log file name. If the currently running data log file is
selected (highlighted), the Delete button will be inactive.
• New/Stop – Use this button to start a new data log file or to stop a running
data log file. The wording on this button will change from “New” to
“Stop” depending on whether a data log file is currently running. The new
data log file name will be defaulted to the format shown above that
includes the date the file was started and an incremental number to
distinguish multiple files with the same date. The default name can be
edited as desired in the New or Edit screen.
• View – Use this button to view the data from a saved data log file in table
format.
• Chart – Use this button to view data from a saved data log file in chart
format (1 temperature sensor & 1 vacuum sensor can be graphed at a time.
Temperature and vacuum sensors can be selected from pop-up menus.
• Export – Use this button to export a selected data log file to a USB flash
drive or computer via the USB port on the left side of the Freeze Dryer.
• Delete – Use this button to delete a saved data log file from the list.
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Settings Screen
Many of the user preferences may be configured from the Settings menu.
Before operating the freeze dryer you may want to configure some of the available
preferences.
1. Language – Chose from 5 languages: English, Spanish, French, German,
Italian
2. Time/Date – Chose Clock Format (12 or 24 hour), Set Time, Set Date for
manually setting the time and date. The Auto Update time & date feature can
be used if a valid network connection has been established. With Auto Update
the following settings need to be entered:
• Time Zone – Enter the Greenwich Mean Time (GMT) offset value for
your location (integer value between -12 & +12).
• NTP server – Enter the “web address” (URL) of the NTP server (of
your choice) that will provide clock synchronization data to the Freeze
Dryer via the Ethernet connection.
• Daylight Savings (ON/OFF) – When Auto Update is ON, this feature
can be used to adjust the time for areas observing Daylight Savings
Time (DST).
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3. Units – Select your desired unit of measure for Temperature (°C, °F) and
Vacuum (mbar, Pa, Torr)
4. Security – A four-digit security code can be set that will require users to enter
the code to gain access to selected screens. A security code will always be
required to enter the “Security” screen.
THE FACTORY DEFAULT SECURITY CODE IS “1234”
• System – If the System security feature is turned ON, users will be
required to enter the security code to gain access to the touch screen
controls when the screen is reactivated from a screen timeout or
power failure (screen timeout described in the Settings/Display
section).
• Programs, Email Alerts, Calibration, Network, Data Options –
Users will be required to enter the security code to gain access to
each individual screen that has been selected (box checked).
5. Alerts – If a network valid connection has been established (via the Settings /
Network screen) and Email Settings have been configured, alerts can be
emailed to selected users, by entering the appropriate email address(es) and
selecting the type of alerts that will be sent to each email address.
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The Edit & Delete buttons will be inactive until an email address is selected
from the list. When an email address has been selected, it will be
highlighted (blue).
• Add – Use this button to add a new email address to the list.
• Edit – Use this button to edit an existing email address.
• Delete – Use this button to delete an existing email address.
• Device Name – The default name for this field will be “Freeze
Dryer”. The name can be edited by pressing the name field.
• Configure Email Settings – Pressing this button will bring up the
following screen where the appropriate email settings can be
entered.
Add email
address
Delete email
address
Configure
email
settings
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Original instructions
If you do not know the proper information to enter into each of the SMTP
fields, consult your IT personnel or email service provider.
After entering the appropriate information in all of the SMTP fields, press
the Save button. The system will check the information entered into each
field to make sure each entry is valid. If one or more invalid entries are
found the following message will appear: EMAIL SETTINGS ERROR –
Unable to test email: (followed by more description depending on type of
entry error).
If all the SMTP fields entered are valid, but the network connection is not
working (or Ethernet cable is not connected) the following message will
appear after pressing the Save button: EMAIL SETTINGS ERROR –
Network connection is not active
• Test – After the Email Settings and Network Settings have been
correctly entered, pressing this button will send a test email to the
selected email address.
• Alerts – The type of alerts that will be sent to each individual email
address can be customized. Pressing the Alerts button will bring up
the following selection list. Alerts can be selected or deselected by
pressing the check box in front of each alert. Scroll list up or down
by swiping screen up or down. Alerts for the Freeze Dryer will be
at the top of the list. Alerts for attached accessories (Tray Dryer or
Heated Product Shelves) will appear at the bottom of the list.
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6. Maintenance – This screen contains data and settings pertaining to the
operation hours and maintenance period for the vacuum pump and refrigeration
system. Scroll up and down to view the entire page.
• Line Voltage Offset - These offset values determine the acceptable voltage
range for electrical power supplied to the Freeze Dryer. If the supply line
voltage is outside of the acceptable range, then the Line Voltage Range alert
will be displayed. The default range is +/- 12.5% of the nominal rated voltage
(115V or 230V depending on model). The LOW Line Voltage Offset can be
adjusted from 0 to -10V (115V models) or 0 to -20V (230V models). The
HIGH Line Voltage Offset can be adjusted from 0 to +10V (115V models) or
0 to + 20V (230V models). Scroll up and down to view the entire page.
• Vacuum Pump Protection – If vacuum pump protection is turned ON, the
vacuum pump will automatically be turned off if a “Vacuum Leak” alert is
presented. This will protect oil filled pumps from losing their oil and
potentially damaging the pump in the event of a major vacuum leak. The
factory default setting for vacuum pump protection is ON, and it is highly
recommended that it remains in the ON setting. If vacuum pump
protection is turned OFF, the pump will continue to run after a “Vacuum
Leak” alert is presented (i.e., there is no protection for the pump in the event
of a major vacuum leak).
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Original instructions
7. Calibration – Some sensors in the Freeze Dryer can be calibrated. This
process should be done by a qualified technician or metrologist with reference
sensors that are known with certainty. An external reference sensor must be
placed at the same measurement point (as close as physically possible) as the
sensor being calibrated. The Collector temperature sensor has its own
reference thermocouple (type T) built into the sensor. The thermocouple is a
brown wire that is coiled inside the housing of the Freeze Dryer and can be
accessed by removing the lower stainless steel front panel. A thermocouple
meter can be used to read the thermocouple value as a reference value.
• Current Reading (uncorrected) – This gives the raw sensor reading
with no offset applied to the reading.
• Offset – This is the value that will be added to the Current Reading
(uncorrected) to give the proper adjusted reading that matches the
reference sensor being used for calibration. The adjusted reading
(uncorrected + Offset) is the value that will be presented on all screens
outside of the Sensor Calibration screen. Pressing the Offset field of
the desired sensor will bring up a dialog box for entering the offset
value for the selected sensor.
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• Calibrate - Pressing this button will save the entered offset value.
Temperature sensor offset values can range from -5 to +5° C.
Vacuum Sensor offset values can range from -0.020 to +0.020
mbar.
8. Display – This screen contains settings for controlling various functions of the
touch screen display.
• Brightness Slider Moving the slider to the right will increase the
brightness level, moving to the left will decrease the brightness level
of the display.
• Touch Sounds – With Touch Sounds turned ON, there will be an
audible sound each time the display is touched. Pressing the Touch
Sounds button will toggle between ON & OFF.
• Alarm Sounds – With Alarm Sounds turned ON, there will be an
audible sound each time an alert message is displayed.
• Screen Timeout Function – If this function is turned ON, the screen
will go into low power mode (sleep) when no screen touches have
been detected for the allotted set time (Screen Timeout). Pressing the
Screen Timeout Function button will toggle between ON & OFF.
• Screen Timeout – This value can be set to 5, 10, 15, 30 min, 1, 2, or 3
hours.
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9. Network – If the DHCP Enabled button is turned ON, and an Ethernet cable is
connecting the Freeze Dryer to an active network, then the IP Address, Subnet
Mask, and Default Gateway fields will be populated automatically. If the
DHCP Enabled button is turned OFF, the IP Address, Subnet Mask, and
Default Gateway fields can then be manually entered to establish a network
connection. If you do not know the proper information to enter into each of the
Network fields, consult your IT personnel.
10. Data Logs – Allows user to make changes to default settings for Data
Acquisition Rate, Log File Deletion and Data Export Options.
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Sensors Screen
This screen contains a list of all sensors currently installed on the Freeze Dryer and
any attached accessory. The screen can be scrolled up and down if the list is too
long to be viewed on a single page. The Sensors screen is for viewing only (there
are no selectable fields on this screen).
Drying Accessory Screen
If an electrically controlled Drying Accessory is NOT connected to the Freeze
Dryer (via the communication cable), the Drying Accessory icon will NOT appear
in the main menu bar. If one of these accessories has been properly connected to
the Freeze Dryer, the Drying Accessory icon will appear in the main menu bar and
you will be able to control and monitor the Drying Accessory from this screen.
Dryer Accessory Sensor Table – The middle section of the screen displays a
list of all the sensors that are available for the connected Drying Accessory.
Sensors that are disconnected will have three dashes (---) for their value.
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Drying Accessory Status Box – The status box is located directly below the
sensor table. The text on the left side will indicate the current operation mode
of the Drying Accessory (OFF, Manual, or Program). When in Manual mode,
the word “Manual” and the current Shelf Temp Set Point value will be
displayed in this location. If a program is running the program name, Step #,
and Time Remaining (TR) in the current Step will be displayed in this location.
The right side of the status box will indicate if Data Logging is currently ON or
OFF.
• PROGRAM – Pressing this button will take you to the Programs
screen, where you can create a new program, or start, edit, view, export
or delete a saved program.
• MANUAL – Use this button to enter a Shelf Set Point Temp and/or
start the Drying Accessory in manual mode.
End Point Detection Screen
If the communication cable is NOT connected or if NONE of the vacuum sensors
are connected to the End Point Detection Enclosure, the End Point Detection icon
(checkered flag) will NOT appear in the menu bar. If the End-Zone end point
detection accessory is properly connected to the Freeze Dryer, this screen will be
used to control the End Point Detection settings for up to five individual freeze dry
flasks.
• End Point Detection status – Shows the current status for each flask.
The status will be one of the following: ON, OFF or COMPLETE.
Touching the end point detection cell for any given flask will allow you
to turn the end point detection ON/OFF. The End Point Detection
status will display COMPLETE automatically when an End Point
Detection alert is achieved for any given flask.
• Offset from Ref. Vacuum – This allows the user to determine the level
of dryness at which the system will declare that the primary drying end
point has been reached. The offset from Ref. Vacuum represents the
difference between the Reference vacuum sensor and the individual
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Original instructions
flask sensor. This value can be set from 0.010 to 0.050 mbar (0.010
being the most dry & 0.050 being the least dry).
•
END POINT DETECTION INDICATES THE END OF THE PRIMARY
DRYING PHASE. SOME SAMPLES MAY REQUIRE ADDITIONAL
FREEZE DRYING TIME (SECONDARY DRYING PHASE) TO
ACHIEVE THE DESIRED MOISTURE CONTENT.
Help Screen
• About – Displays the catalog number of the Freeze Dryer and the
software versions currently installed.
• Diagnostics – This screen will give information about the power supply
to the Freeze Dryer (Voltage, Current & Frequency) and allow the user
to run Manual or Auto Diagnostics on the unit.
• Resources – Scan QR codes with smart phone to take you to specific
pages of the Labconco website (Labconco.com).
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• Backup/Restore – Log files & User Programs can be exported to a
USB flash drive. Only user program can be imported to the Freeze
Dryer from a USB flash drive.
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Original instructions
CHAPTER 5
USING YOUR FREEZE DRYER
Operation Checklist
The following checklist should be followed prior to each use of your Freeze Dryer:
1. 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(s) and
sealing surfaces of the drying chamber/manifold and connection port to remove
any dirt or contaminants that could cause a vacuum leak.
2. Remove the baffle (if equipped) and wipe with a soft cloth or paper towel to
remove any remaining moisture.
3. Ensure that the collector chamber and drain line are free of water. Place the
drain hose in a suitable container to collect the condensate from the collector
chamber. Insert the quick connect drain fitting into the quick connect drain
coupling located on the front of the Freeze Dryer. If equipped with the Shell
Freezer option, the lower drain coupling is used to drain the collector chamber
and the top is use to drain the Shell Freezer. Note: Freeze Dryer (Collector or
Vacuum) will not start if moisture is detected in the drain line.
4. After completely draining the system, disconnect the quick connect drain
fitting from the quick connect drain coupling.
DISCONNECT THE QUICK CONNECT DRAIN FITTING BEFORE
STARTING THE VACUUM PUMP. FAILURE TO REMOVE THE
FITTING WILL RESULT IN A LARGE VACUUM LEAK.
5. Wipe the interior of the collector chamber with a soft cloth or paper towel to
remove any remaining moisture.
6. Reinstall baffle (if equipped) in collector chamber.
7. Reinstall the drying chamber or manifold on the connection port. Note:
Vacuum grease is NOT required on the drying chamber lid, collector
chamber lid or port gasket(s) to obtain a proper vacuum seal.
8. Check that each sample valve is closed or in the “vent” position.
9. Start COLLECTOR and allow the refrigeration system to reach its specified
operating temperature (-50°C or -84°C depending on model)
10. Start VACUUM when collector temperature is -40°C or colder.
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Original instructions
11. Attach a pre-frozen sample to sample valve on drying chamber or manifold.
Note: If using a Clear Chamber, Tray Dryer or Heated Product Shelves, the
vacuum chamber must be fully vented (to atmospheric pressure) in order to
remove acrylic chamber or open door before loading sample into the drying
chamber.
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 Dryer. 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.
Purge Valve
The optional purge valve is installed between the Freeze Dryer collector chamber
and the vacuum pump. When the blue indicator bar is shown above the PURGE
button (on the Home screen), the purge valve is closed and the vacuum pump is
isolated from the Freeze Dryer collector chamber.
During Freeze Dryer start-up, the refrigeration system cools the collector coil
down to its working temperature. While the collector coil cools, the purge valve
can be closed and the vacuum pump allowed to run. This allows the vacuum pump
oil to heat up, which will evaporate and expel condensed solvents from the oil.
When the collector coil is at its working temperature and the freeze dry process is
started, the warm pump oil is less likely to condense solvent vapors that are not
trapped by the collector coil. When the Freeze Dryer is operated in the Auto Start
Mode, the purge valve and vacuum pump will operate automatically to perform
this function. In Manual Mode the user must manually activate the purge valve
and vacuum pump to perform this function.
Before shut down the vacuum pump can be run for several minutes with the purge
valve closed. This will allow the warm pump oil to evaporate and expel solvent
vapors that condensed in the pump oil during the freeze dry process. Whether the
Freeze Dryer is run in Auto Start Mode or Manual Mode, the user must manually
activate the purge valve and vacuum pump to perform this function at shut down.
If power to the Freeze Dryer is interrupted during the freeze dry process, the purge
valve will open during the power outage, and the vacuum bleed valve will open to
allow atmospheric air to enter the system.
Operating the Freeze Dryer
Auto start-up (without Purge Vale option)
1. Go to Home screen
2. Press AUTO, then press START
• COLLECTOR will start immediately
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• VACUUM will start when collector temperature reaches -40°C
Auto start-up (with Purge Valve option)
1. Go to Home screen
2. Press AUTO, then press START
• COLLECTOR will start immediately
• PURGE valve will close immediately
• VACUUM will start immediately
• Purge valve will open when collector temperature reaches -40°C
Manual start-up
1. Go to Home screen
2. Press COLLECTOR, then press START
3. When COLLECTOR temperature reaches -40°C (or colder)
• Press VACUUM, then press START
Setting the Operating Vacuum Level
To change the Vacuum Set Point
1. Go to Home screen
2. Press VACUUM,
• enter new Vacuum Set Point value
• press APPLY (or START if vacuum pump is not already running)
The vacuum level may be set by the user to optimize the freeze dry process.
Normally, the sublimation rate will increase as the pressure increases 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. The reference
table below shows the relationship between ice temperature and vapor pressure.
Vapor pressure above ice
Temp.
(°C)
Pressure
(mbar)
Temp.
(°C)
Pressure
(mbar)
Temp.
(°C)
Pressure
(mbar)
Temp.
(°C)
Pressure
(mbar)
Temp.
(°C)
Pressure
(mbar)
0
6.11
-11
2.37
-21
0.94
-31
0.34
-50
0.039
-1
5.63
-12
2.17
-22
0.85
-32
0.31
-60
0.011
-2
5.18
-13
1.98
-23
0.77
-33
0.28
-70
0.003
-3
4.76
-14
1.81
-24
0.70
-34
0.25
-80
0.001
-4
4.37
-15
1.65
-25
0.63
-35
0.22
-5
4.02
-16
1.50
-26
0.57
-36
0.20
-6
3.69
-17
1.37
-27
0.52
-37
0.18
-7
3.38
-18
1.25
-28
0.47
-38
0.16
-8
3.10
-19
1.13
-29
0.42
-39
0.14
-9
2.84
-20
1.03
-30
0.38
-40
0.13
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
Chapter 5: Using Your Freeze Dryer
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Original instructions
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 vacuum level are shown below. Exact protocols
must be determined by the user for the specific samples that are being freeze dried.
Material
Solidification/Eutectic
Temperature
Pre-Freeze
Temperatures
Vacuum Set Point
Bacteria,Virus
≤ -40°C
≤ -50°C
≤ 0.040 mbar
Milk
-5 to -13
-15 to -23
1.65 to 0.77
Fungi
≤ -40
≤ -50
≤ 0.040
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
When the vacuum control is set to operate at less vacuum (higher pressure), the ice
holding capacity of the collector may be decreased. This can be improved by
installing a baffle in the collector. See Appendix A Freeze Dry Components for the
baffle part number. See Chapter 3: Baffle Installation for proper positioning of the
baffle in the collector chamber.
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. Prefreezing temperature is typically 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 chambers or manifolds
with 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.
Chapter 5: Using Your Freeze Dryer
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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.
Starting a Program (for optional drying accessories)
If one of the electronically controlled accessory drying chambers, suitable for your
Freeze Dryer, has been properly installed, you will be able to run a program.
BEFORE STARTING A PROGRAM YOU SHOULD ALWAYS ENSURE
THAT THE COLLECTOR IS “ON” AND HAS COOLED TO -40°C OR
BELOW.
Vent/Backfill Port
Bevel in “vent” position
Bevel in “vacuum”
position
Adapter
Chapter 5: Using Your Freeze Dryer
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Original instructions
1. Go to the Programs screen. You can access the Programs screen in two
different ways, both lead to the same location.
a. Directly access the Programs screen by selecting the Programs icon
from the main menu bar at the top of the display.
b. Go to the Drying Accessory screen, then select the PROGRAM
button at the bottom of the screen.
2. Select a program from the saved programs list, or create a new program.
3. With the desired program selected from the list, press the START button.
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. Go to Home screen, press VACUUM, then STOP to
turn the vacuum pump OFF. Then release system vacuum by turning the plastic
knob on a valve (that has no sample attached) to the open position or opening the
vent valve on Tray Dryer or Clear Chamber. Press COLLECTOR, then STOP to
turn the refrigeration system OFF.
Defrosting
The following procedure should be followed when defrosting the collector coil:
1. The hot gas defrost function can be used to speed up the defrosting process.
Defrost can be activated as follows: Go to Home screen, press COLLECTOR
button, press Defrost Options, then press START.
2. To turn off Defrost: Go to Home screen, press DEFROST button, press STOP.
The defrost function will turn off automatically if the collector temperature
reaches +60°C or if defrost has been running for 2 hours.
3. 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 wall of the chamber.
4. Place the drain hose in a suitable container to collect the condensate from the
collector chamber. Insert the quick connect drain fitting into the quick connect
drain coupling located on the left hand side of the unit.
5. Flush the collector chamber with water and wipe chamber dry.
6. Disconnect the quick connect drain fitting from the quick connect drain
coupling.
DISCONNECT THE QUICK CONNECT DRAIN FITTING
BEFORE STARTING THE VACUUM PUMP. FAILURE TO
REMOVE THE FITTING WILL RESULT IN A LARGE
VACUUM LEAK.
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.
!
Chapter 5: Using Your Freeze Dryer
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Original instructions
Never attempt to start the vacuum pump when there is liquid in
the collector chamber. This could result in damage to the
vacuum pump.
Operating the Shell Freezer (optional feature)
The optional built in shell freezer is designed for shell freezing samples in flasks in
preparation for freeze-drying.
Follow the steps below each time you use the shell freezer to obtain optimum
performance:
1. Ensure that the shell freezer drain fitting has been removed from the quick
connect drain coupling on the front of the Freeze Dryer.
2. Remove the shell freezer lid and add solvent to the bath compartment.
Commonly used solvents are methanol or ethanol. Recommended solvent depth
is ¼" to ½" above the top of the rollers (approximately 2 liters).
If flammable solvents are used in the shell freezer bath, be sure to
keep away from open flame.
3. Press the “SHELL FREEZER” button, then press the “Start” button. The blue
indicator bar above the button will illuminate. The shell freezer refrigeration
module will start and the bath rollers will begin rotating. The shell freezer bath
temperature will be displayed on the Home screen (and Sensors screen).
4. Fill a freeze dry container no more than 1/3 full with sample and stopper the container
top. Lay the container on the rollers in a horizontal position. Replace the shell freezer
lid during shell freezing.
5. When the sample is completely frozen in the container, remove the container from
the bath compartment and freeze dry the sample or place it in a suitable storage
freezer for future freeze drying.
6. Press the “SHELL FREEZER” button, then press the “Stop” button to turn the
shell freezer off.
7. If the Shell Freezer is to be used for cold bath operation, additional solvent
may be added to submerge small flasks. Do not fill pan more than 2 inches
below the top of the stainless steel pan with vessels submerged. Allow
additional time for larger volumes of solvent to pull down in temperature.
8. Always drain flammable solvents from the bath when the shell freezer is not in
use and store the solvent in a suitable container. This is accomplished by
inserting the drain fitting into the quick connect drain coupling labeled “SHELL
FREEZER” on the front of the Freeze Dryer. Place the drain hose in a suitable
container to collect the solvent.
!
!
Chapter 5: Using Your Freeze Dryer
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Original instructions
Operating the Mini Chamber (optional feature)
The Mini Chamber is designed for freeze drying small samples, either in bulk or in
small containers such as vials or 96 well plates. It may be used in conjunction with
other drying accessories that are mounted on top of the Freeze Dryer or
independently. If a manifold or chamber is mounted to the Freeze Dryer and is not
in use, close all of its valves. If no drying accessory is installed on the Freeze
Dryer, place the supplied stopper in the center of the 3.0 accessory port that is on
the top of the Freeze Dryer to seal the vacuum system. Follow the steps below to
operate the Mini Chamber.
1. Start the Freeze Dryer. Position the Vacuum Chamber valve on the top of the
Freeze Dryer to the VENT position. Press the “AUTO” or “COLLECTOR”
button, then press the “Start” button.
IF THE COLLECTOR CHAMBER WILL BE USED TO PRE-FREEZE THE
SAMPLE, DO NOT USE “AUTO” TO START THE REFRIGERATION AND
VACUUM PUMP, SINCE VACUUM SHOULD NOT BE APPLIED TO THE
COLLECTOR CHAMBER WHILE PRE-FREEZING SAMPLES.
2. Freeze the sample. Before the freeze dry process can occur, the product to be
freeze dried must be in a frozen state. This can be done in a separate freezer or
in the Freeze Dryer collector chamber.
3. Load the samples. The Freeze Dryer collector temperature must be –40°C or
colder before starting the freeze dry process. Replace the chamber lid.
4. Start primary drying. Turn the vacuum control valve on the top of the Freeze
Dryer to VACUUM. Start the vacuum pump (if it is not already running).
5. Set the Mini Chamber temperature. Press the “MINI CHAMBER” button, then
enter a “Temp Set Point” value, and press the “Start” button. The set
temperature should be lower than the eutectic temperature of the sample.
THE MINI CHAMBER IS NOT REFRIGERATED. IF THE OPERATING
TEMPERATURE IS SET BELOW AMBIENT, THE ONLY SOURCE
COOLING THE CHAMBER IS THE FROZEN SAMPLE AND THE
COOLING EFFECT FROM THE FREEZE DRYING (SUBLIMATION)
PROCESS.
6. Start secondary drying. After all the free moisture is removed in the primary
drying phase, the temperature of the chamber may be increased. Press the
“MINI CHAMBER” button, enter a new “Temp Set Point” value, and press the
“Apply” button.
7. Shut Down. After completion of the freeze dry procedure:
a. Press the “MINI CHAMBER” button, then press the “Stop” button to
turn off the chamber heater.
b. Release vacuum in the chamber by turning the valve on the top of the
Freeze Dryer to VENT.
c. Remove the sample.
d. Turn off the vacuum pump
e. Release vacuum from the Freeze Dryer by either opening the Vacuum
Chamber valve (when the chamber lid is off) or by opening a valve on a
chamber or manifold mounted on top of the Freeze Dryer.
Chapter 5: Using Your Freeze Dryer
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Original instructions
f. Turn off the Freeze Dryer, defrost and drain the collector chamber per
instructions in this manual.
Alerts
A number of events may occur during a lyophilization procedure that will cause an
alert to be displayed on the Freeze Dryer touch screen. An audible alarm (beeper)
will also be sounded that will automatically be muted after one minute.
The specific alert type can be identified by observing the message box on the
display. The alert message box and audible alarm can be dismissed by pressing the
“Back” button on the alert message box. The following conditions will initiate an
alert.
Power Fail
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 above -30°C, 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 drawn into the vacuum pump.
When power is restored, the “Power Fail” alert message will be displayed on the
touch screen.
Line Voltage Range
If the voltage supplied to the Freeze Dryer varies beyond allowable limits, the
LINE VOLTAGE RANGE alert will be activated. 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 LINE VOLTAGE OFFSETS may be adjusted from the Settings /
Maintenance screen.
Collector Temp
After the collector temperature has cooled to below -40°C, an alert will be
activated if the collector temperature rises above –40°C for more than 5 minutes.
Collector Moisture
If there is liquid in the collector chamber and either the COLLECTOR or
VACUUM start button is pressed, neither function will start and an alert will be
activated. 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.
Chapter 5: Using Your Freeze Dryer
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Original instructions
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, an alert will be activated. 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. The “Set hours between oil change” can be reprogrammed from the
Settings / Maintenance screen for any value from 0 to 9999 hours.
Vacuum Leak
If the vacuum level in the freeze dryer has not reached at least 5 mbar within 30
minutes of starting the vacuum, an alert will be activated and the vacuum pump
will be turned off (if it is plugged into the Freeze Dryer vacuum pump outlet).
Vacuum Set Point
If the system is unable to achieve the vacuum set point (during Manual or Program
mode), an alert will be activated. This alert will be activated if the vacuum level is
not within 0.500 mbar of the vacuum set point in 20 minutes.
Status Email Messages
If this option has been turned on, the selected email addresses will receive
STATUS alert messages containing the current operating parameters of the Freeze
Dryer. Status alert messages will not be displayed on the touch screen. The
Freeze Dryer can be configured to send email status alert messages from the
Settings / Alerts / Select Alerts screen.
End Point Detection (optional accessory)
An alert will be activated when the primary drying phase end point has been
detected for any of the active flask sensors connected to the End-Zone end point
detection accessory.
System Temp Variation (optional accessory)
If a Stoppering Tray Dryer accessory is connected to the Freeze Dryer this alert
will be activated if the system temperature varies more than ± 2°C from the Shelf
Temp Set Point.
System Temp Set Point (optional accessory)
If a Stoppering Tray Dryer accessory is connected to the Freeze Dryer this alert
will be activated if the system temperature stabilized without reaching the Shelf
Temp Set Point.
Shelf Temp Variation (optional accessory)
If a Bulk Tray Dryer, Tray Dryer or Heated Product Shelves accessory is
connected to the Freeze Dryer this alert will be activated if the shelf temperature
varies more than ± 3°C from the shelf set point temperature.
Chapter 5: Using Your Freeze Dryer
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Original instructions
Shelf Temp Set Point (optional accessory)
If a Bulk Tray Dryer, Tray Dryer or Heated Product Shelves accessory is
connected to the Freeze Dryer this alert will be activated if the shelf temperature
stabilized without reaching the Shelf Temp Set Point.
Power Fail (optional accessory)
If an electronically controlled drying accessory is connected to the Freeze Dryer
this alert will be activated if a power failure occurs to the accessory.
Program Complete (optional accessory)
If an electronically controlled drying accessory is connected to the Freeze Dryer
this alert will be activated when the last step of a running program has been
completed.
Export a Data Log File
Data Log Files can be copied (exported) to a USB flash drive via the USB port on
the left side of the Freeze Dryer. The file will be exported as a “comma separated
values” file (.csv file extension), which can be easily opened with a spreadsheet
application program for data analysis and graphing. To export a file:
1. Insert USB flash drive into the Freeze Dryer USB port
2. Go to Data Logging screen
3. Select the file that you want to export by pressing the Data Log File name
4. Press the Export button
Downloading Data Log Files via Ethernet
Data log files that are stored in the Freeze Dryer can be downloaded via an
Ethernet connection. In order for this to be possible, a working Ethernet
connection must first be established. The following steps must be completed:
1. An Ethernet cable must be connected to the Ethernet port on the back of the
Freeze Dryer and to a Local Area Network (LAN) with working internet
service.
2. The proper settings must be entered into the Settings>Network screen to
establish a valid network connection (see description of Network screen in
Chapter 4).
3. Write down the “IP Address” shown on the Settings>Network screen of the
Freeze Dryer (this number will be used in Step 5)
4. Open an internet browser of your choice from a computer that is connected
to your LAN.
5. Type the following into the address bar at the top of the browser screen:
http://“IP Address”:8080 where “IP Address” represents the number
written down from the Settings>Network screen in Step 3 (example =
http://10.10.9.117:8080).
Chapter 5: Using Your Freeze Dryer
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Original instructions
6. The following webpage will appear with a list of all the Data Log files that
are stored on the Freeze Dryer.
7. Single click on a file name from the list to download the file.
8. Single click on the downloaded file to open the file in Excel.
Copy a Program
If you wish to duplicate a program or quickly create a program that is similar to an
existing program, you can use the copy program function. The new program file
created by the copy function will be stored on the Freeze Dryer. To copy a
program:
1. Go to Programs screen
2. Select a program from the list by pressing the program name
3. Press the COPY button
4. Edit program name if desired (the default program name will be “program
name_copy”)
Product Service 816-333-8811 or 1-800-522-7658
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Original instructions
CHAPTER 6
MAINTAINING YOUR FREEZE
DRYER
Service Safety Precautions
• Always ensure that only authorized technicians service the refrigeration,
vacuum and electrical systems.
• If performing any electrical maintenance, always disconnect the power at
the main disconnect.
• If the refrigeration system must be operated with access panels removed
(for diagnostic purposes only), stay clear of moving fan blade.
• Always practice team lifting when moving heavy equipment.
• After servicing, verify that all access panels or covers are in place before
resuming normal operation of the equipment.
Routine Maintenance Schedule
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-
abrasive 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.
!
Chapter 6: Maintaining Your Freeze Dryer
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6. Check the collector 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.
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.
Product Service 816-333-8811 or 1-800-522-7658
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Original instructions
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.
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. Note: If the vacuum
pump is plugged directly into a wall outlet for troubleshooting purposes, the
vacuum START button must be initiated on the display screen. If the vacuum
START button is not initiated the vacuum vent valve will remain open and
the vacuum reading will remain on HIGH. 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.
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.
Chapter 7: Troubleshooting
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Original instructions
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 that the quick connect drain fitting is
disconnected from the quick connect drain coupling (on the left side of the
Freeze Dryer).
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.
Chapter 7: Troubleshooting
Product Service 816-333-8811 or 1-800-522-7658
52
Original instructions
The illustrations below show how the sample valve installs on a chamber and a
manifold.
Thrust Washer
Valve Body
Knob & Stem
Assembly
Valve Body
Trim Ring
Manifold Assembly
Knob & Stem
Assembly
Bulkhead Nut
Gasket
(No grease
required)
Bulkhead
Fitting
Valve Body
Thrust Washer
Valve Assembly (Manifold)
Valve Assembly (Stainless Steel Chamber)
Valve Body
Knob & Stem
Assembly
Valve Assembly (Clear Chamber with Valves)
Chapter 7: Troubleshooting
Product Service 816-333-8811 or 1-800-522-7658
53
Original instructions
III. System Components and Collector Chamber
Isolation
This test determines if the source of a leak is in the drying chamber or manifold.
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 dry system from the accessory chamber/manifold
FREEZE DRY
FLASK
GASKET
Chapter 7: Troubleshooting
Product Service 816-333-8811 or 1-800-522-7658
54
Original instructions
The following test determines if a vacuum leak is in the collector chamber.
1. Insert a rubber stopper (#2) in the vacuum port in the left side of the
collector chamber.
2. Start the Freeze Dryer and observe the vacuum indication. If the vacuum is
good, the problem is in the collector chamber. If it is bad, the problem is in
the plumbing connections from the collector chamber to the vacuum pump.
3. If the leak is in the plumbing connections, check all rubber parts, fittings
and clamps.
4. If the leak is in the chamber, check the drain hose, hose connections and
the quick connect drain coupling. The figure below shows other potential
leak areas where bulkhead fittings are used to seal the holes where the
collector coil penetrates the bottom of the collector chamber.
5. If a leak 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. If a leak is still present at the
bulkhead fittings, loosen the bulkhead fittings and apply vacuum grease to
the O-rings, then reassemble and test.
COLLECTOR COIL
STOPPER
COLLECTOR CHAMBER
AREAS FOR
POTENTIAL LEAKS
Chapter 7: Troubleshooting
Product Service 816-333-8811 or 1-800-522-7658
55
Original instructions
Refrigeration Module Operation
Under a no-load condition, the FreeZone Freeze Dry Systems can achieve a
collector temperature of -50°C or -84°C (based on model designation) or lower
within 30 minutes when the vacuum pump is operating, depending on ambient
temperature and humidity. If the collector temperature does not reach the design
temperature within 30 minutes, then the refrigeration module is not functioning
properly.
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
56
Original instructions
APPENDIX A
FREEZE DRYER COMPONENTS
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.
Appendix A: Freeze Dryer Components
Product Service 816-333-8811 or 1-800-522-7658
57
Original instructions
6L -50C Models (70061xxxx) 6L -84C Models (71061xxxx)
12L -50C Models (70121xxxx) 12L -84C Models (71121xxxx)
18L -50C Models (70181xxxx)
Item
6L
-50C
6L
-84C
12L
-50C
12L
-84C
18L
-50C
Part No.
Description
1 X X X X X 7690800
Lid Gasket - Collector
2 X X X X X 7532900
Lid Collector
3
X X X X X
7408400
Lid Gasket - Drying Chamber or Shell
Freezer
4
X X X X X
7408300
Lid - Drying Chamber
X
7403100
Lid - Shell Freezer
5
X
7750607
Compressor 115V, 60 Hz
X
7750606
Compressor 230V, 50 Hz
X
7750605
Compressor 230V, 60 Hz
X
7591805
Compressor 115V, 60 Hz 1ST & 2ND Stage
X
7591806
Compressor 230V, 50 Hz 1ST & 2ND Stage
X
7591807
Compressor 230V, 60 Hz 1ST & 2ND Stage
X
7592001
Compressor 230V, 50 Hz
X
7592000
Compressor 230V, 60 Hz
X
7750606
Compressor 230V, 50 Hz 1ST & 2ND Stage
X
7750605
Compressor 230V, 60 Hz 1ST & 2ND Stage
X
7391801
Compressor 230V, 50 Hz
X
7391800
Compressor 230V, 60 Hz
6
X
7750607
Compressor 115V, 60 Hz Shell Freezer
X
7750606
Compressor 230V, 50 Hz Shell Freezer
X
7750605
Compressor 230V, 60 Hz Shell Freezer
7
X
7953802
Motor Fan, 115V
X X
7953803
Motor Fan, 230V
X
7383500
Motor Fan, 115V
X X X
7383501
Motor Fan, 230V 60Hz
X X X
7383502
Motor Fan, 230V 50Hz
X
7953802
Motor Fan, 115V Shell Freezer
X
7953803
Motor Fan, 230V Shell Freezer
8 X X X X X 7316600
Display Assembly
9 X X X X X 7337300
Gasket, Display
10 X X X X X 7337400
Panel, Control
11 X X X X X 7336900
Label, Control Panel
12 X X X X X 7346400
Control Panel Assembly (Complete)
13 X X X X X 7335200
Drain Fitting (Coupling Body)
14 X X X X X 7335400
Drain Fitting (Coupling Insert, 3/8 Barb)
15 X X X X X 7337100
Retaining Ring, Drain Fitting
16 X X X X X 7337000
Lanyard, Drain Fitting
17 X X X X X 1889406
Machine Screw, 8-32 x 3/8” long
18 X X X X X 7429700
Moisture Sensor
19 X X X X X 7373436
Vacuum Hose
20 X X X X X 7403800
Filter, Female Luer-Lok
21 X X X X X 7403700
Luer, #10-32 Male
22 X X X X X 7432700
Vacuum Control/Bleed Valve
23 X X X X X 7362300
Vacuum Sensor
Appendix A: Freeze Dryer Components
Product Service 816-333-8811 or 1-800-522-7658
58
Original instructions
Item
6L
-50C
6L
-84C
12L
-50C
12L
-84C
18L
-50C
Part No.
Description
24
X
7339200
Electrical Enclosure Assembly 115V
X X X
7339201
Electrical Enclosure Assembly 230V
X
7339202
Elec. Enclosure Cascade Assy 115V
X X
7339203
Elec. Enclosure Cascade Assy 230V
X
7340300
Elec. Enclosure with Purge Assy 115V
X X X
7340301
Elec. Enclosure with Purge Assy 230V
X
7340302
Electrical Enclosure with Purge & Chamber
Assembly 115V
X X X
7340303
Electrical Enclosure with Purge & Chamber
Assembly 230V
X
7340304
Electrical Enclosure with Purge & Shell
Freezer Assembly 115V
X
7340305
Electrical Enclosure with Purge & Shell
Freezer Assembly 230V
X
7340306
Electrical Enclosure Cascade with Purge
Assembly 115V
X X
7340307
Electrical Enclosure Cascade with Purge
Assembly 230V
X
7340308
Elec Enclosure Cascade with Purge & Drying
Chamber Assembly 115V
X X
7340309
Elec Enclosure Cascade with Purge & Drying
Chamber Assembly 230V
25
X X X X X
7515302
Temperature Sensor – Collector
(Not Shown)
X
7515302
Temperature Sensor – Shell Freezer
(Not Shown)
X X X X X
7515302
Temperature Sensor - Drying Chamber (Not
Shown)
26
X X X X X
1336400
Power Cord 115V 60Hz US (Not Shown)
X X X X X
1338002
Power Cord 230V 60Hz US (Not Shown)
X X X X X
1332601
Power Cord 230V 60Hz Saudi
(Not Shown)
X X X X X
1336500
Power Cord 230V 50Hz EU (Not Shown)
X X X X X
1332701
Power Cord 230V 50Hz China
(Not Shown)
X X X X X
1332601
Power Cord 230V 50Hz UK (Not Shown)
X X X X X
1345701
Power Cord 230V 50Hz India
(Not Shown)
27 X X X X X 7361101
Wire Harness, IOB Control (Not Shown)
28
X X X
7361700
Wire Harness, Power (Not Shown)
X X
7361701
Wire Harness, Power (Not Shown)
29
X
7303300
Purge Valve 115V
X X X X
7303301
Purge Valve 230 V
30 X X X X X 7814601
Valve Drying Chamber
31
X
7407300
Heater Drying Chamber 115 V
X X X X
7407301
Heater Drying Chamber 230 V
32
X
7213200
Baffle 6L (SSTL)
X
7213201
Baffle 6L (PTFE)
X
7213300
Baffle 12L (SSTL)
X
7213301
Baffle 12L (PTFE)
X
7390700
Baffle 18L (SSTL)
X
7390701
Baffle 18L (Polypro)
33 X X X X X 7205304
Drain Hose (Not Shown)
Appendix A: Freeze Dryer Components
Product Service 816-333-8811 or 1-800-522-7658
59
Original instructions
1
2
3
3
4
4
5
6
7
7
8
9
10
11
12
13
14
15
16
17
19
24
32
Appendix A: Freeze Dryer Components
Product Service 816-333-8811 or 1-800-522-7658
60
Original instructions
20
21
22
23
29
30
31
18
Product Service 1-800-522-7658
61
Original instructions
APPENDIX B
FREEZE DRYER DIMENSIONS
6L -50C Models (70061xxxx) 6L -84C Models (71061xxxx)
12L -50C Models (70121xxxx) 12L -84C Models (71121xxxx)
18L -50C Models (70181xxxx)
*Dimensions in inches & (centimeters)
36.6
93
31.8
80.7
29.6
75.1
Product Service 816-333-8811 or 1-800-522-7658
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Original instructions
APPENDIX C
FREEZE DRYER
SPECIFICATIONS
This Appendix contains technical information about the Freeze Dryer including
electrical specifications and operating conditions.
Electrical Specifications
Voltage
Frequency
Amps
Catalog #
Description
Nominal
Operating
Range
(Hz)
Max. with
Vacuum Pump
70061xxxx
6L -50C
115V
103-127
60
16
230V
187-253
60
8
230V
198-253
50
8
71061xxxx
6L -84C
115V
103-127
60
16
230V
187-253
60
10
230V
198-253
50
10
70121xxxx
12L -50C
230V
187-253
60
9
230V
198-253
50
9
71121xxxx
12L -84C
230V
187-253
60
9
230V
198-253
50
9
70181xxxx
18L -50C
230V
187-253
60
9
230V
198-253
50
9
Appendix C: Freeze Dryer Specifications
Product Service 816-333-8811 or 1-800-522-7658
63
Environmental Conditions
• Indoor use only.
• 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.
Product Service 816-333-8811 or 1-800-522-7658
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Original instructions
APPENDIX D
FREEZE DRYER ACCESSORIES
Labconco offers a full line of accessories to enhance your Freeze Dryer’s operation
and usability. For a complete list of these accessories, please consult our website
at www.labconco.com.
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