Labconco FreeZone Plus 4.5 Liter User Manual

FreeZone
Plus™ 4.5 Liter Cascade
Freeze Dry Systems
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User’s Manual
Labconco Corporation 8811 Prospect Avenue Kansas City, MO 64132-2696 800-821-5525, 816-333-8811 FAX 816-363-0130 E-MAIL labconco@labconco.com HOME PAGE www.labconco.com
Please read the User’s Manual before operating the equipment.
Warranty
Labconco provides a warranty on all parts and factory workmanship. The warranty includes areas of defective material and workmanship, provided such defect results from normal and proper use of the equipment. Glassware is not warranted from breakage when dropped or mishandled.
The warranty for FreeZone® Freeze Dry Systems will expire one year from date of installation or two years from date of shipment from Labconco, whichever is sooner. Warranty is non-transferable and only applies to the owner (organization) of record.
This limited warranty covers parts and labor, but not transportation and insurance charges. In the event of a warranty claim, contact Labconco Corporation or the dealer who sold you the product. If the cause is determined to be a manufacturing fault, the dealer or Labconco Corporation will repair or replace all defective parts to restore the unit to operation. Under no circumstances shall Labconco Corporation be liable for indirect, consequential, or special damages of any kind. This statement may be altered by a specific published amendment. No individual has authorization to alter the provisions of this warranty policy or its amendments. Lamps and filters are not covered by this warranty. Damage due to corrosion or accidental breakage is not covered.
Copyright © 2008, 2009, 2012, 2013, 2014 Labconco Corporation. All rights reserved.
The information contained in this manual and the accompanying products are copyrighted and all rights reserved by Labconco Corporation. Labconco Corporation reserves the right to make periodic design changes without obligation to notify any person or entity of such change.
Returned or Damaged Goods
Do not return goods without the prior authorization from Labconco. Unauthorized returns will not be accepted. If your shipment was damaged in transit, you must file a claim directly with the freight carrier. Labconco Corporation and its dealers are not responsible for shipping damages.
The United States Interstate Commerce Commission rules require that claims be filed with the delivery carrier within fifteen (15) days of delivery.
Limitation of Liability
The disposal and/or emission of substances used in connection with this equipment may be governed by various federal, state, or local regulations. All users of this equipment are required to become familiar with
any regulations that apply in the user’s area concerning the dumping of waste materials in or upon water,
land, or air and to comply with such regulations. Labconco Corporation is held harmless with respect to user’s compliance with such regulations.
Contacting Labconco Corporation
If you have questions that are not addressed in this manual, or if you need technical assistance, contact Labconco’s Customer Service Department or Labconco’s Product Service Department at 1-800-821-5525 or 1-816-333-8811, between the hours of 7:00 a.m. and 6:00 p.m., Central Standard Time.
Part #7387900, Rev. D
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CHAPTER 1: INTRODUCTION 1
Freeze Dry Process 1 Freeze Dry Rates 2 Freeze Dry Capacity 3 Samples Containing Volatile Substances 4 Safety Symbols 4
CHAPTER 2: PREREQUISITES 6
Electrical Requirements 6 Location Requirements 6 Vacuum Pump Requirements 7 Chamber or Manifold Requirements 7
CHAPTER 3: GETTING STARTED 8
Unpacking Your Freeze Dryer 9 Freeze Dryer Components 9 Setting Up Your Freeze Dryer 11
Vacuum Pump Connection 11 Electrical Connection 11
Drying Chamber or Drying Manifold Installation 11 Chemical Resistance of Freeze Dryer Components 12 Solvent Safety Precautions 13
CHAPTER 4: USING YOUR FREEZE DRYER 14
Freeze Dryer Controls 15 Operation Checklist 16 Vacuum Pump Ballast Setting 16 Operating the Freeze Dryer 17
Set-Up 17
Automatic Start-Up 19
Manual Start-Up 19 Setting the Operating Vacuum Level 20 Pre-Freezing Samples 20 Adding Sample 21 Shut Down 22 Defrosting 22
Alarms 23
Power Failure 23 Line Voltage Out of Range 23 Temperature Out of Range 24 Service Vacuum Pump 24 Moisture in Collector 24
CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 25
CHAPTER 6: USING THE RS232 RECEPTACLE 27
Computer Connection for Computer Interface 27
CHAPTER 7: TROUBLESHOOTING 31
Vacuum Pump 31 Gaskets, Tubing, Connections, Sample Valves 32 System Components & Collection Chamber Isolation 34 Refrigeration Module Operation 36
CHAPTER 8: MODIFYING YOUR FREEZE DRYER DISPLAY 37
Temperature and Vacuum Display 37 Line Voltage Alarm Points 37 Moisture Sensor Alarm 38 Modifying the Display 38
APPENDIX A: FREEZE DRYER COMPONENTS 42
APPENDIX B: FREEZE DRYER DIMENSIONS 44
APPENDIX C: FREEZE DRYER SPECIFICATIONS 47
Electrical Specifications 47 Environmental Conditions 48
APPENDIX D: FREEZE DRYER ACCESSORIES 49
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Congratulations on your purchase of a Labconco FreeZone® Freeze Dry System, which is designed for laboratory lyophilization procedures. The refrigerant used in the refrigeration system is CFC-free so it will not endanger the environment. The unit is easy to install and maintain. Proper care and maintenance of this product will result in many years of dependable service.
Freeze Dry Process
Freeze drying is an important process in sample preparation and for the preservation and storage of biologicals, pharmaceuticals and foods. Of the various methods of dehydration, freeze drying (lyophilization) is especially suited for substances that are heat sensitive. Other than food processing (e.g., coffee, whole dinners), freeze drying has been extensively used in the development of pharmaceuticals (e.g., antibiotics) and preservation of biologicals (e.g., proteins, plasma, viruses and cell lines). The nondestructive nature of this process has been demonstrated by the retention of viability in freeze dried viruses and microorganisms.
Freeze drying is a process whereby water or other solvent is removed from frozen material by converting the frozen water directly into vapor without the intermediate formation of liquid water. The basis for this sublimation process involves the absorption of heat by the frozen sample in order to vaporize the ice; the use of a vacuum pump to enhance the removal of water vapor from the surface of the sample; the transfer of water vapor to a collector; and the removal of heat by the collector in order to condense the water vapor. In essence, the freeze dry process is a balance between the heat absorbed by the sample to vaporize the ice and the heat removed from the collector to convert the water vapor into ice.
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Chapter 1: Introduction
2
SAFE TEMPERATURE AND DRYING TIMES
FOR SELECTED MATERIALS
Material 10mm Thick
Safe Temperature °C
Collector Temperature °C
Hours (Approx.) Milk
-5
-40
10
Urea
-7
-40
10
Blood Plasma
-10 to -25
-40
16
Serum
-25
-40
18
Vaccinia
-30 to -40
-50
22
Influenza Vaccine
-30
-50
24
Human Tissue
-30 to -40
-50
48
Vegetable Tissue
-50
-80
60
Table 1
Freeze Dry Rates
The efficiency of the freeze drying process is dependent upon the surface area and the thickness of the sample, the collector temperature and vacuum obtained, the eutectic point and solute concentration of the sample. It is important to remember these factors when trying to obtain efficient utilization of your freeze dry system. A listing of selected materials and their approximate drying times are shown in Table 1 for your reference.
*Total sample quantities are contingent on various freeze dryer capacities.
Up to the point of overloading the system, the greater the surface area of the sample, the faster the rate of freeze drying. By contrast, for a given surface area, the thicker the sample the slower the rate of freeze drying. This is based on the fact that the heat of sublimation is usually absorbed on one side of the frozen sample and must travel through the frozen layer to vaporize water at the other surface. In addition, as the sample is freeze dried, the water vapor must travel through the layer of dried material. The thicker the sample, the greater the chance that the dried layer may collapse, which would cause an additional decrease in the rate of freeze drying.
The surface area and thickness of the sample can usually be ignored when each sample contains only a few milliliters. However, for larger volumes, the samples should be shell frozen to maximize the surface area and minimize the thickness of the sample. The volume of the freeze dry flask should be two to three times the volume of the sample.
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Chapter 1: Introduction
3
In order for lyophilization to occur, ice must be removed from the frozen sample via sublimation. This is accomplished by the collector and the vacuum pump. The collector, which should be at least 15 to 20°C colder than the eutectic temperature (melting temperature) of the sample, traps vapor as ice. Since the vapor pressure at the collector is lower than that of the sample, the flow of water vapor is from the sample to the collector. Since this vapor diffusion process occurs very slowly under normal atmospheric conditions, a good vacuum is essential to maintain an efficient rate. In many applications, the maintenance of a vacuum of 0.133 mBar or less is recommended.
The rate of freeze drying is directly proportional to the vapor pressure and the vapor pressure is dependent upon both eutectic temperature and solute concentration of the sample. For example, a solution of sodium chloride and water would freeze dry at a slower rate than pure water. The eutectic temperature of a sodium chloride solution is about –21°C and at this temperature the vapor pressure is about 1/16 that of water at 0°C. Although the eutectic temperature is not dependent upon the concentration of sodium chloride, the vapor pressure of the water would decrease as the concentration of sodium chloride increased. This is due to the fact that as the solute concentration increases, less of the surface area of the frozen sample is occupied by water. In general, most solutions or biological samples will have a eutectic temperature of –10 to –25°C. However, if the sample contains a simple sugar such as glucose or if the sample is animal or plant tissue, the eutectic temperature may be as low as –30° to –50°C.
Freeze Dry Capacity
The volume of a sample that can be freeze dried at one time is related to factors discussed previously and the size and design of the freeze dry system. With any given instrument, the capacity is based on the surface area of the sample; the eutectic temperature and concentration of the sample; and the rate and amount of heat transferred to the frozen sample. Of these factors, the eutectic temperature is the most important factor in determining the amount of sample that can be freeze dried at one time, particularly when flasks are used. This is because as the eutectic temperature decreases, the vapor pressure decreases but the rate of heat absorption by the sample does not change. This tends to promote melting of the sample, which leads to a marked increase in vapor pressure and ultimately overloads the collector and vacuum pump. Samples that have eutectic temperatures of –20°C or lower should be placed on the freeze dry system one flask at a time so that the vacuum in the system may recover before adding another sample to the system. If the vacuum does not recover, the capacity of the freeze dry system has been exceeded and the sample should be removed.
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Chapter 1: Introduction
4
If there is a problem with a particular type of sample melting when placed on the freeze dry system, dilution of the sample with more water or providing some insulation around the flask to decrease the rate of heat absorption by the sample may help. If the eutectic temperature of the sample is –40 to –60°C, the freeze dry system selected for use must be equipped with cascade type refrigeration so that the collector temperature can be cooled to below –75°C, or a dry ice/solvent trap may be used between the collector and the vacuum pump.
Samples Containing Volatile Substances
In certain cases the solvent in a sample to be freeze dried may contain volatile components such as acetonitrile, methanol, acetic acid, formic acid or pyridine. In addition to these substances having an effect on the eutectic temperature, they may increase the vapor pressure at the surface of the sample. Also, compared to water, they will require the absorption of less heat for sublimation to occur. Hence, samples that contain volatile substances will have a greater tendency to melt, particularly when placed in flasks or exposed to room temperature. If a sample containing a volatile substance tends to melt when placed on a freeze dry system, dilution of the sample with more water will help keep the sample frozen. For example, a 0.2M solution of acetic acid is much easier to freeze dry than a 0.5M solution.
Safety Symbols
Your freeze dry system was designed with safety in mind, however conditions may exist that could be hazardous.
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Chapter 1: Introduction
5
Throughout this manual potentially hazardous conditions are identified using the following words and symbols.
It is important that you understand the warnings listed throughout this manual before you operate the freeze dry system.
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Before you install your freeze dryer, you need to prepare your site for installation. Carefully examine the location where you intend to install your freeze dryer. You must be certain that the area is level and of solid construction. An electrical source must be located near the installation site.
Carefully read this chapter to learn:
the electrical supply requirements. the vacuum pump requirements.
Refer to Appendix C: Freeze Dryer Specifications for complete freeze dryer electrical and environmental conditions, specifications and requirements.
Electrical Requirements
The freeze dryer requires a dedicated electrical outlet. This outlet requires a 20 Amp circuit breaker or fuse for models rated at 115V (60 Hz). An outlet equipped with a 15 Amp circuit breaker or fuse is required for models rated at 230V (50/60 Hz). See Freeze Dryer Components in Chapter 3 for detail plug specifications. If the plug supplied with the Freeze Dryer does not match the available receptacle, remove this plug and replace it with an approved plug of the suitable style.
Location Requirements
The freeze dryer should be located in an area that provides an unobstructed flow of air around the cabinet. This air cools the refrigeration system. The refrigeration system draws air through the rear panel and exhausts it through the sides. A minimum of 3" must be allowed between the back and both sides of the freeze dryer and adjacent wall surfaces. Restriction of airflow during operation could adversely affect performance.
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Chapter 2: Prerequisites
7
Refer to Appendix C: Freeze Dryer Specifications for dimensional drawings of the Freeze Dryer. The space for benchtop models must be large enough to accommodate the vacuum pump, which will be used with the freeze dryer.
Vacuum Pump Requirements
A vacuum pump must be provided by the user. A vacuum pump with a displacement of 86 liters per minute and 0.002 mBar ultimate pressure is adequate for most samples. The inlet fitting on the vacuum pump must be suitable for 3/4" ID vacuum hose, which is provided. It is recommended that the vacuum pump is equipped with an exhaust filter to minimize oil mist exhausting from the vacuum pump. The operating vacuum level may be set on the freeze dryer. The higher the pressure is set, the more likely it is that oil mist will be exhausted.
Vacuum pumps used with 115V models should be equipped with a 115V, 15 Amp NEMA 5-15P plug. Vacuum pumps used with 230V models should be equipped with a reverse IEC plug. This plug is included with 230V models. This will allow the vacuum pump to be plugged into the receptacle on the back panel of the freeze dryer. See Appendix D: Freeze Dryer Accessories for vacuum pumps available from Labconco.
Chamber or Manifold Requirements
A 12-port drying chamber is included with the unit. This allows samples to be attached to the freeze dryer. See Appendix D: Freeze Dryer Accessories for available chambers and manifolds.
Product Service 816-333-8811 or 1-800-522-7658
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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.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
9
Power Cords
Catalog #
Description
Volts
Hz
PTFE
Coated
Chamber
1336400
1336500
1342100
1332601
1332701
7386020
4.5L Benchtop Cascade Freeze Dryer
115
60 X
7386021
4.5L Benchtop Cascade Freeze Dryer
115
60 X X
7386030
4.5L Benchtop Cascade Freeze Dryer
230
50 X
7386031
4.5L Benchtop Cascade Freeze Dryer
230
50 X X
7386040
4.5L Benchtop Cascade Freeze Dryer
230
60 X
7386041
4.5L Benchtop Cascade Freeze Dryer
230
60 X X
7386060
4.5L Benchtop Cascade Freeze Dryer
230
50 X
7386061
4.5L Benchtop Cascade Freeze Dryer
230
50 X X
7386070
4.5L Benchtop Cascade Freeze Dryer
230
50 X
7386071
4.5L Benchtop Cascade Freeze Dryer
230
50 X X
Unpacking Your Freeze Dryer
Carefully unpack your freeze dryer and inspect it for damage that may have occurred in transit. If your freeze dryer is damaged, notify the delivery carrier immediately and retain the entire shipment intact for inspection by the carrier.
The Benchtop FreeZone Plus Cascade 4.5 Liter Freeze Dry System weighs over 125 lbs. (57 Kg). The Console FreeZone Plus Cascade 4.5 Liter Freeze Dry System weighs over 176 lbs. (80 Kg). If you must lift the freeze dryer manually, use at least two (2) persons and follow safe lifting guidelines.
If your freeze dryer was damaged in transit, you must file a claim directly with the freight carrier. The United States Interstate Commerce Commission rules require that claims be filed with the delivery carrier within fifteen (15) days of delivery. Labconco Corporation and its dealers are not responsible for shipping damage.
Do not return goods without the prior authorization of Labconco. Unauthorized returns will not be accepted.
Do not discard the carton or packing material for your freeze dryer until you have checked all of the components and installed and tested the freeze dryer.
Freeze Dryer Components
Locate the model of FreeZone Plus Cascade 4.5 Liter Freeze Dry System you received in the following table. Verify that the components listed are present and undamaged.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
10
Power Cords
Catalog #
Description
Volts
Hz
PTFE
Coated
Chamber
1336400
1336500
1342100
1332601
1332701
7387020
4.5L Console Cascade Freeze Dryer
115
60 X
7387021
4.5L Console Cascade Freeze Dryer
115
60 X X
7387030
4.5L Console Cascade Freeze Dryer
230
50 X
7387031
4.5L Console Cascade Freeze Dryer
230
50 X X
7387040
4.5L Console Cascade Freeze Dryer
230
60 X
7387041
4.5L Console Cascade Freeze Dryer
230
60 X X
7387060
4.5L Console Cascade Freeze Dryer
230
50 X
7387061
4.5L Console Cascade Freeze Dryer
230
50 X X
7387070
4.5L Console Cascade Freeze Dryer
230
50 X
7387071
4.5L Console Cascade Freeze Dryer
230
50 X X
7382020
4.5L -105C Benchtop Freeze Dryer
115
60 X
7382021
4.5L -105C Benchtop Freeze Dryer
115
60 X X
7382030
4.5L -105C Benchtop Freeze Dryer
230
50 X
7382031
4.5L -105C Benchtop Freeze Dryer
230
50 X X
7382032
4.5L -105C Benchtop Freeze Dryer
230
50 X
7382033
4.5L -105C Benchtop Freeze Dryer
230
50 X X
7382034
4.5L -105C Benchtop Freeze Dryer
230
50 X
7382035
4.5L -105C Benchtop Freeze Dryer
230
50 X X
7382040
4.5L -105C Benchtop Freeze Dryer
230
60 X
7382041
4.5L -105C Benchtop Freeze Dryer
230
60 X X
Part #
Component Description
7387900
User’s Manual
7373450
Vacuum Hose
1488800
Hose Clamps (2)
7395801
Chamber Lid
7395800
Lid Gasket
7522800
Drying Chamber (12-port)
1291000
Plug
Plus the following:
If you did not receive one or more of the components listed for your freeze dryer, or if any of the components are damaged, contact Labconco Corporation immediately for further instructions.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
11
Setting Up Your Freeze Dryer
After you verify receipt of the proper components, move your freeze dryer to the location where you want to install it. Then, follow the steps listed below.
Vacuum Pump Connection
A vacuum pump as described in Chapter 2: Prerequisites is required to operate your freeze dry system properly. The freeze dryer is equipped with a 3/4" ID, heavy wall, vacuum hose for connecting the collector chamber to the vacuum pump.
Place the vacuum pump near the benchtop freeze dryer models. For console models, from the back of the unit, place the vacuum pump on the floor of the cabinet.
Connect the vacuum pump power cord to the receptacle on the back of the
cabinet labeled “vacuum pump.” If the vacuum pump has an off/on switch,
turn the switch on. The vacuum pump will be controlled by the freeze dryer. Connect the vacuum pump inlet port to the vacuum tube on the back of the cabinet with the vacuum hose and clamps provided. If necessary, cut the hose to proper length to allow for gentle bends without kinks.
Models rated for use on 230V have a reverse IEC connector for attaching the vacuum pump power cord. A plug is supplied that can be installed on the vacuum pump power cord if necessary. Make certain that the oil in the vacuum pump is at the proper level.
Electrical Connection
Plug the power cord into the receptacle on the back of the freeze dryer and plug the other end into a suitable power receptacle.
Drying Chamber or Drying Manifold Installation
Install the clear lid with 3.0 inch hole on top of the collector chamber.
The supplied drying chamber or drying manifold, which may be purchased separately, may be positioned directly above the 3-inch hole in the collector chamber lid. Center the rubber gasket that came with the chamber over the hole in the lid. Then place the chamber over the gasket. When vacuum is applied to the system, the chamber will be held securely in place.
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Chapter 3: Getting Started
12
Acids
Buffers Solvents
Component
Material
Acetic Acid 20%
Formic Acid
Trifluoroacetic Acid (TFA) Calcium Chloride
Sodium Phosphate Acetone
Acetonittirle
Carbon Tetrochloride
Cyclohexane
Dioxane
Methyl t-Butyl Ether (BTBE)
Pyridine
Valve Stem
Acetal
C D D D D Collector Lid
Acrylic
D D D D
Hoses, Gaskets & Valve Bodies
Neoprene
C D D C C D D D C
D
Flask Top
Silicon Rubber
C D D D D D C
D
Chamber & Fittings
Stainless Steel
C
Chemical Resistance of Freeze Dryer Components
The FreeZone Freeze Dry System is designed to be chemically resistant to most compounds that are commonly used in freeze drying processes. However, by necessity, the freeze dryer is comprised of a number of different materials, some of which may be attacked and degraded by certain chemicals. The degree of degradation is dependent on the concentration and exposure duration. Some of the major components of the FreeZone Freeze Dry System that are susceptible to degradation are as follows:
C – Moderate degradation; Limited use D – Severe degradation; infrequent use recommended; immediate thorough cleaning required.
Most common compounds used in freeze drying processes, if allowed to
enter the vacuum pump, will degrade the oil and cause damage to the vacuum pump.
Sugars and proteins typically will have minimal negative effect on any of
the materials of construction.
When using compounds in the freeze dryer that are hostile to the materials of construction, it is imperative the equipment is thoroughly cleaned after use.
Rubber and plastic components that have been exposed to damaging
compounds should be removed and flushed with water.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 3: Getting Started
13
The oil in the vacuum pump should be checked often. It must be changed
if it is cloudy, shows particles or is discolored. The useful life of vacuum pump oil can be extended if the vacuum pump is operated for an extended period of time after a freeze dry run. This allows contaminants to be purged from the hot oil. This must be done with the inlet to the pump blocked off to prevent air from free flowing through the pump. If the pump is operated at an elevated vacuum level (> 10mBar), oil may be expelled from the pump and damage could occur.
Another way to extend the life of the vacuum pump is to install an optional secondary trap in the line between the freeze dryer and the vacuum pump. Contact Labconco for ordering information.
With prudent maintenance the FreeZone Freeze Dry System will provide years of service. Warranty on the affected parts will be voided if maintenance has been obviously neglected. If you have questions about using specific compounds in the freeze dryer, contact Labconco Technical Service at 1-800-821-5525 or 816-333-8811 or e-mail:
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.
NOTE: The disposal of substances used in connection with this equipment may be governed by various Federal, State or local regulations. All users of this equipment are urged to become familiar
with any regulations that apply in the user’s area concerning the
dumping of waste materials in or upon water, land or air and to comply with such regulations.
Product Service 816-333-8811 or 1-800-522-7658
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After your Freeze Dryer has been installed as detailed in Chapter 3: Getting Started, you are ready to begin using your Freeze Dryer. Read this chapter to
learn how to:
operate the controls. understand the display. connect samples.
Do not use the freeze dryer in a manner not specified by the manufacturer (refer to Appendix C: Freeze Dryer Specifications). The electrical protection properties of the freeze dryer may be impaired if the freeze dryer is used inappropriately.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 4: Using Your Freeze Dryer
15
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Freeze Dryer Controls
The control panel for the freeze dryer is shown below with a description about its function.
1. LCD Display – Displays system operating parameters, set-up parameters and alarm messages.
2. Menu Switch – This switch is used to change the display from operating system parameters to set-up parameters.
3. Select Switch – Used to select set-up parameters.
4. Vacuum Switch – Used to start or stop the vacuum pump when operating in manual start-up mode.
5. Vacuum Indicator – This green LED indicates that power is being supplied to the vacuum pump receptacle on the back of the freeze dryer.
6. Manual Refrigeration Switch – Used to start only the refrigeration module.
7. Manual Operation Indicator – When lit, the green LED indicates the freeze dryer is being controlled manually by the operator. Each function must be started by the operator.
8. Auto Mode Switch – Used to start or stop the refrigeration and the Auto Mode process.
9. Auto Mode Indicator – When lit, the green LED indicates that the freeze dryer is in Auto Mode. In this mode, the vacuum pump will start when the collector temperature reaches –40°C.
10. Vacuum Graph Display – This display indicates the relative system vacuum level. The highest LED indicates that the vacuum level is above 2.0 mBar. The indicators will sequence down when the vacuum level reaches 2.0, 1.0, 0.8, 0.6,
0.45, 0.12 mBar. The lower green LED flashes when the system vacuum level is
0.45 to 0.12 mBar and illuminates steadily below 0.133 mBar.
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Chapter 4: Using Your Freeze Dryer
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11. Collector Temperature Graph Display – This display indicates the temperature of the collector. The highest LED indicates the collector temperature is warmer than 10°C. The indicators will sequence down when the temperature reaches 10, 0,
-10, -20, -30, -40°C (-10, -20, -30, -40, -50, -60 for Models 73820xx). When the collector temperature is –40°C (-60°C for Models 73820xx) or lower the green indicator will light.
12. Alarm Indicator – This red LED indicates that a system alarm has occurred. Press the Menu Switch to display the alarm message on the LCD display.
13. Main Power Switch – Turns the freeze dryer on or off. (Not shown, located on the left side of the cabinet).
Operation Checklist
The following checklist should be followed prior to each use of your freeze dryer:
1. Wipe the interior of the collector chamber with a soft cloth or paper towel to remove any accumulated moisture.
2. Check the collector chamber drain hose to ensure that the hose is free of moisture and that the drain plug is securely installed. The freeze dryer will not start if moisture is detected.
3. Using a soft, lint-free cloth or paper towel, wipe the collector chamber lid gasket to remove any dirt and contaminants that could cause a vacuum leak. Vacuum grease is not required on the lid gasket to obtain a proper vacuum seal.
4. Remove the drying chamber or accessory manifold from the connection port and using a soft, lint-free cloth or paper towel, wipe the port gasket and sealing surfaces of the drying chamber/manifold to remove any dirt and contaminants that could cause a vacuum leak. Reinstall the drying chamber or manifold on the port. Vacuum grease is not required on the port gasket to obtain a proper vacuum seal.
5. Check that each sample valve is closed or in the “vent” position.
Vacuum Pump Ballast Setting
Most vacuum pumps are equipped with a gas ballast mechanism. The freeze dry process requires high vacuum. Therefore, it is recommended that the gas ballast be closed during the operation of the freeze dry system. If the gas ballast is left open for extended periods of operation, the oil can be pumped out the exhaust, causing the pump to fail.
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Chapter 4: Using Your Freeze Dryer
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VACUUM UNITS
mBar Pa Torr
TEMPERATURE UNITS
°C °F
VACUUM SET POINT
XXXX YYY
Operating the Freeze Dryer
Set-Up
The freeze dryer may be configured to automatically start the vacuum pump when the collector temperature reaches –40°C. The display units for vacuum may be selected to be mBar, Pascal (Pa) or Torr and the temperature may be displayed as °F or °C. The run time of the refrigeration system and the vacuum pump may be monitored.
To configure your freeze dryer, turn the main power switch ON and press MENU. The display shows:
Press SELECT until the desired units are flashing. Press MENU. The display shows:
Where YYY is the units selected above.
Press SELECT until the desired vacuum operating level is displayed.
See “Setting the Operating Vacuum Level” for guidelines.
If “0” is selected, the vacuum control is disabled and the vacuum
level in the freeze dry system will be determined by the capabilities of the vacuum pump.
Press MENU. The display shows:
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Chapter 4: Using Your Freeze Dryer
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REFRIG TOTAL HOUR: XXXX SERVICE HOUR: XXXX
REFRIG TOTAL HOUR: XXXX RESET SERVICE HOUR: ?
VACUUM TOTAL HOUR: XXXX SERVICE HOUR: XXXX
RS-232 TRANSMISSION RATE
10 SECONDS
VACUUM TOTAL HOUR: XXXX RESET SERVICE HOUR: ?
Press SELECT until the desired units are flashing. Press MENU. The display shows:
To reset the SERVICE HOUR to 0 press SELECT. This allows you
to keep track of the time the refrigeration system operated since it was serviced.
The display shows the refrigeration system hours.
To reset the service hours to 0, continue to hold SELECT 5 seconds
until hours are reset.
TOTAL HOUR cannot be reset. Press SELECT. The display shows the vacuum pump hours.
To reset the SERVICE HOUR to 0, press SELECT. The display shows:
If you want to reset the service hours to 0, continue to hold SELECT five seconds until hours are reset.
Press SELECT. The display shows the RS-232 data transmission rate.
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Chapter 4: Using Your Freeze Dryer
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To change the rate press SELECT until the desired time interval is
shown. The time between data transmissions may be set to occur at 10, 30, 60, 300 or 600 second intervals.
Press MENU to return to display operating parameters or after a short
delay, the display will automatically switch to show operating parameters.
Automatic Start-Up
To run the Auto Mode, press the panel switch labeled REFRIGERATION AUTO. The green LED above the switch illuminates and the refrigeration system starts. When the collector reaches –40°C, the vacuum pump will start. The Temperature and Vacuum Graph indicate collector temperature and system vacuum. The LCD display shows the actual temperature of the collector. When the vacuum in the system is above 5 mBar the vacuum display indicates “HI.” At 5 mBar and below, the display shows the actual vacuum.
When the system vacuum is between 0.450 and 0.133 mBar, the lower green vacuum graph LED will flash. When the system vacuum level is <0.133 mBar, the green LED will be lit steadily indicating that most samples may be added.
Manual Start-Up
To manually run the freeze dry process press the REFRIGERATION MAN switch. This starts the refrigeration system. The green LED above the switch illuminates. When the collector temperature reaches –40°C, the vacuum pump may be started by pressing the VACUUM switch. The Temperature and Vacuum Graph indicate collector temperature and system vacuum. The LCD display shows the actual temperature of the collector. When the vacuum in the system is above 5 mBar the vacuum display indicates “HI.” At 5 mBar and below, the display will show the actual vacuum.
When the system vacuum is between 0.450 and 0.133 mBar, the lower green vacuum graph LED will flash. When the system vacuum level is <0.133 mBar, the green LED will be lit steadily indicating that samples may be added.
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Chapter 4: Using Your Freeze Dryer
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Material
Solidification/Eutectic
Temperature
Pre-Freeze
Temperatures
Vacuum Set Point
Bacteria,Virus
-40°C and Colder
-50°C & Colder
0.040 mBar & Lower
Milk
-5 to -13
-15 to -23
1.65 to 0.77
Fungi
-40 and Colder
-50 & Colder
0.04 and lower
Vegetable Tissue
-25 to -50
-35 to -60
0.22 to 0.01
Human Tissue
-30 to –40
-40 to –50
0.12 to 0.04
Blood Plasma
-10 to –25
-20 to –35
1.03 to 0.22
Vaccine
-30 to –40
-40 to –50
0.12 to 0.04
Setting the Operating Vacuum Level
The vacuum level may be set by the user to optimize the freeze dry process. Normally, the sublimation rate will increase if there is less vacuum (a higher pressure) in the freeze dryer. A good starting place is to set the vacuum so its level is equivalent to about 10°C colder than the eutectic or collapse temperature of the sample. Adjustments to the vacuum level must be made for various freeze drying conditions. Factors that must be considered are whether the sample is freeze dried on heated shelves or in glassware attached to manifold valves, the volatility of the sample itself, the size of the sample and the heat energy supplied to the sample.
Some guidelines for setting the freeze dryer are shown below. These show pre-freezing temperatures and vacuum levels. Exact protocols must be determined by the user for the specific samples that are being freeze dried.
When the vacuum control is set to operate at less vacuum, the ice holding capacity of the collector may be decreased.
Pre-Freezing Samples
Appropriate containers for freeze drying include ampules, serum bottles, and wide-mouth freeze drying flasks. Shell freezing of samples is recommended for wide-mouth freeze drying flasks. Smaller samples in ampules and serum bottles may be frozen in a freezer or in the center of the collector chamber. The sample container size should always be at least two to three times the sample size (i.e., 40 ml samples should be prepared in 80 ml containers or larger). The temperature required for pre-freezing is dependent on the characteristics of the sample. Pre-freezing temperature typically is at least 10° to 20°C below the eutectic or collapse temperature of the sample.
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Chapter 4: Using Your Freeze Dryer
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Vent/Backfill Port
Bevel in “vent” position
Bevel in “vacuum”
position
Adapter
Adding Sample
The following procedure should be followed when using sample valves in the freeze dry process:
1. Connect a pre-frozen sample to a sample valve on the drying chamber or
manifold using an adapter. Turn the plastic valve knob to the “VACUUM”
position to open the valve, which connects the attached sample to system vacuum. The bevel on the knob should be positioned toward the sample port to apply vacuum to the sample.
2. Before adding another sample, allow system vacuum to return to 0.133 mBar or lower. Any combination of valves and sample sizes may be utilized at one time provided that the system vacuum and collector temperature remain sufficiently low to prevent melting of the frozen sample.
3. When all the frost has disappeared from the outer surface of the sample container and no cold spots can be detected by handling the container, the sample is nearly dry. To be certain of low final moisture content, dry the sample for several hours past this point.
4. To remove a container after drying is complete, turn the plastic knob on
the valve to the “VENT” position, which closes the valve and vents the
container. Should backfilling with an inert gas be required, connect the gas supply line to the vent port on the valve before turning the plastic knob on the valve to vent position. The sample container may now be removed. In the vent position the bevel on the valve knob should point away from the sample port.
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Chapter 4: Using Your Freeze Dryer
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5. Ampules may be flame sealed while connected to a valve by using a sealing torch. Care must be taken not to burn the valve. An insulation material placed between the valve and the torch is recommended.
Shut Down
At the end of a run or when a sufficient amount of condensate accumulates on the collector coil to obstruct the flow of vapor to the collector chamber, the Freeze Dryer should be defrosted. First, release system vacuum by turning the plastic knob on a valve to the open position or by pulling the collector chamber drain plug out of the drain hose. Now press the Vacuum Switch on the control panel to turn the vacuum pump OFF. Press the Refrigeration Switch next to the illuminated LED to turn OFF the refrigeration system. Turn OFF the Main Power Switch on the right hand side of the cabinet.
Defrosting
The following procedure should be followed when defrosting the collector coil:
1. Pull the collector chamber drain hose out from the right hand side of the freeze dryer and remove the drain plug. Place the drain hose in a suitable container to collect the condensate that will melt off the collector coil.
2. Remove the collector chamber lid and allow ambient room air to melt the ice. Dispose of the liquid appropriately.
3. Flush the collector chamber with water and wipe chamber dry.
4. If rapid defrost is desired, pour warm water over the collector coil. Do not allow the liquid to enter the vacuum port on the upper rear of the chamber.
5. Reinstall the drain hose plug and slide drain hose back into the side of the cabinet. Dispose of the liquid appropriately.
Utilization of acid requires immediate cleaning and neutralization after defrost or physical damage to the collector chamber and collector coil will result.
Do not attempt to chip ice from the collector coil as damage may occur to the coil.
Never attempt to start the vacuum pump when there is liquid in the collector chamber. This could result in damage to the vacuum pump.
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Chapter 4: Using Your Freeze Dryer
23
POWER FAIL HOLD SELECT TO CLEAR IT
LINE VOLTAGE ERROR
Alarms
A number of unusual events may occur during a lyophilization procedure that can adversely effect the operation of the freeze dryer. If an event occurs, the alarm indicator flashes and the beeper sounds.
The beeper automatically mutes itself after one minute. The specific alarm can be identified by pressing MENU. Pressing MENU multiple times displays multiple alarms if they have occurred. The following “out of specification” conditions initiate an alarm:
Power Failure
If a power failure occurs during a freeze dry process, the vacuum control valve allows air to bleed into the freeze dryer system. If the failure is of a short duration and the collector does not warm up excessively, when power is restored the freeze dryer restarts and resume operation of the refrigeration and vacuum systems. If the power failure lasts for a longer duration and the collector warms above safe limits, when the power is restored, the freeze dryer will not automatically restart. This prevents melted sample from being drawn into the collector and prevents liquid from being sucked into the vacuum pump.
When power is restored, the alarm indicator flashes and the alarm beeper sounds. When the MENU button is pressed the display shows:
Press and hold SELECT for five seconds until the error message is cleared from the display.
Line Voltage Out of Range
If the voltage supplied to the freeze dryer varies beyond allowable limits, the alarm will be activated. When an alarm occurs, press MENU and the display shows:
The alarm self-cancels when the proper voltage is restored. The high and low alarm points are preset at the factory to correspond to the normal allowable voltage variations based on the nominal voltage specified for the freeze dryer. Some models may be operated outside the normal voltage limits. See Appendix C. If necessary, the high and low alarm points may be adjusted for these models. See Chapter 8.
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Chapter 4: Using Your Freeze Dryer
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COLLECTOR TEMPERATURE HOLD SELECT TO CLEAR IT
CHANGE VACUUM OIL HOLD SELECT TO CLEAR IT
MOISTURE IN COLLECTOR
Temperature Out of Range
An alarm activates if the collector temperature rises above –40°C (-60°C for Models 73820xx). If this occurs, the display shows:
Press and hold SELECT for five seconds until the error message is cleared from the display.
Service Vacuum Pump
The vacuum pump normally plugs into the vacuum pump electrical receptacle on the back of the freeze dryer. When the freeze dryer has accumulated a total of 1000 operating hours, the alarm indicator will flash. Press MENU to display the alarm:
Press and hold SELECT for five seconds until the error message is cleared from the display.
This resets the 1000 hour timer. It may be necessary to service the vacuum pump more frequently than every 1000 hours depending on the operation of the freeze dryer. The pump oil should be regularly monitored to verify that it is clean.
Moisture in Collector
If there is liquid in the collector chamber and either a REFRIGERATION button or the VACUUM button is pressed, neither function will start and an alarm will be activated. When MENU is pressed, the display shows:
When the collector is drained, the alarm self-cancels.
This feature prevents the inadvertent start of the vacuum pump when liquid is in the collector and thereby can extend the life of the vacuum pump.
A few drops of liquid may remain in the drain hose after draining. When the vacuum pump is started these drops may be sucked into the collector chamber. This is normal.
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Under normal operation, the freeze dryer requires little maintenance. The following maintenance schedule is recommended:
As needed:
1. Clean up all spills; remove liquids from the chamber.
2. Clean lid and gasket using soft cloth, sponge or chamois and a mild, non-
3. Check oil level of the vacuum pump. It should be between MIN and
4. If oil shows cloudiness, particles or discoloration, drain the pump and
5. Utilization of acids requires immediate cleaning and neutralization
6. Check the collection chamber for condensed or frozen solvents and
7. If sample valves leak or stems become difficult to turn, pull the stem out
abrasive soap or detergent.
MAX. If the oil level is less than an inch (25.4 mm) above MIN, add oil to proper level.
replace with fresh oil.
after a run or physical damage to the collector chamber and collector coil will result.
dispose of appropriately. Completely empty the collector chamber before the next run or before attempting to start the vacuum pump.
of the rubber valve body and apply a thin coat of vacuum grease to the stem. Reinsert the stem into the valve body.
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Chapter 5: Maintaining Your Freeze Dryer
26
Monthly:
1. The rubber components on the freeze dryer may eventually deteriorate and require replacement. The effective life of rubber parts depends upon both their usage and the surrounding environment. Check all rubber hoses and gaskets and replace any that show signs of hardening, permanent set or deterioration.
2. Using a soft cloth, sponge or chamois and a mild, non-abrasive soap or detergent, clean the acrylic chamber lid.
3. Using a soft cloth, sponge, or chamois and a mild, non-abrasive soap or detergent, clean the exterior surfaces of the freeze dryer. Liquid spray cleaners and polishes may be used on the exterior surfaces. Do not use solvents to remove stains from the exterior surfaces as they may damage the finish.
Annually:
1. Every 12 months, or more often if the freeze dryer is operated in a dusty environment, the refrigeration system condenser should be cleaned. Using a vacuum cleaner with brush attachment, clean the condenser to ensure proper airflow for peak performance.
Front Access Panel Removal (Console Models)
The front stainless steel panel can be removed by placing a flat blade screwdriver in the rectangular hole in the center of the kick panel. Pivot the handle downward to disengage the latch and simultaneously pull the bottom edge of the lower panel forward. The lower panel is installed by first sliding the top edge under the lip on the plastic control panel. Pivot the bottom inward and push until the latch is secure.
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The operation of the freeze dryer can be monitored using a computer when it is connected to the RS232 receptacle on the rear panel. The computer cannot control the operation of the freeze dryer. The monitored parameters are the collector temperature in °C and vacuum in microbars.
Computer Connection for Computer Interface
Check your computer to see which type of serial port is provided, then use a connecting cable below:
1. Computers with a 25 pin D-sub male serial connector should use Connect Cable, Labconco part number 7537801, to connect a computer to the freeze dryer.
2. Computers with a 9 pin D-sub male serial connector should use Connect Cable, Labconco part number 7537800, to connect a computer to the freeze dryer.
The purpose of the RS232 interface is to send data to a data logging computer to monitor the state and activity of the freeze dryer. This data is half duplex data. The data properties are as follows:
1. Data Rate 2400 Baud
2. 8 Bit word length
3. 1 Start bit, 1 Stop bit
4. No parity is transmitted
5. Standard ASCII character set
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Chapter 6: Using the RS232 Receptacle
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B
= Base Unit
T
= Collector Temperature
-48
= Collector Temperature in °Celsius
V
= Vacuum
18
= Vacuum Level in Micro Bars
SF
= Shell Freezer Temperature (not available on 4.5L models)
9
= Feature not installed or out of range
C
= Vacuum Chamber Temperature(not available on 4.5L models)
PG
= Purge (not available on 4.5L models)
RS-232 TRANSMISSION RATE
10 SECONDS
The time between data transmissions may be varied by the user to occur at 10, 30, 60, 300 or 600 second intervals. Press the MENU button until the RS232 screen appears on the display.
Press select until the desired time interval is shown.
The format of the transmitted message is as follows:
B<T= -48 V= 18 SF = 999 C=999 PG=9 >
Where:
There are several commercially available software packages, which can read RS232 data and enter the data into a computer program, such as a word processor (to create a text file) or spreadsheet (to tabulate and plot the data). Consult your laboratory supply dealer regarding the latest software available. The following describes how to use an IBM compatible computer with Hyper
Terminal™ software (included with Windows® 95, 98, XP or 2000 operating
systems) to collect the RS232 data from your freeze dryer:
1. Make sure that the freeze dryer is properly connected to the communication port on the computer.
2. Open Hyper Terminal™ software.
i)Windows® 95 or 98 use:
START/PROGRAMS/ACCESSORIES.
ii) Windows® 2000 use:
START/ROGRAMS/ACCESSORIES/COMMUNICATIONS
The first time Hyper Terminal™ is opened a dialogue box requesting an area
code and phone number appears. Enter the appropriate numbers and continue.
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Chapter 6: Using the RS232 Receptacle
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3. The “Connection Description” dialogue box opens. Type in a user defined name and select an icon for the new connection. Press “OK.”
4. The “Connect To” dialogue box opens. Using the down arrow selection button, select the communication port to which the cable has been connected. Press “OK.”
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Chapter 6: Using the RS232 Receptacle
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5. The “Com X Properties” dialogue box opens. Enter the appropriate data properties and press “OK.”
6. When the freeze dryer main power switch is on, the data is transmitted and updated at the time intervals selected by the user.
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Refer to the following if your freeze dryer fails to operate properly. If the suggested corrective actions do not solve your problem, contact Labconco for additional assistance.
FreeZone Freeze Dry Systems that are clean, dry and without samples attached should reach a vacuum of 0.133 mBar within 10 minutes and should achieve an ultimate vacuum of 0.040 mBar within 18 hours when the refrigeration is operating. If the freeze dryer does not obtain a satisfactory vacuum, perform the following maintenance tests.
I. Vacuum Pump
First make sure that the vacuum pump operates. If it fails to operate, check the electrical connections of the freeze dryer to the power source and then check the electrical connection of the vacuum pump to the freeze dryer. If the vacuum pump has a power switch, make sure that it is turned on. If the vacuum is not adequate when the vacuum pump is operating, proceed with the following steps:
1. Check the oil and ensure it is clear and clean. If the oil looks cloudy or has any particulates, replace the pump oil. Sometimes it may be necessary to flush the pump with clean oil several times. To flush the pump, run the pump 5 to 10 minutes to allow the oil to warm up. Drain the oil and refill with clean oil. Repeat as necessary.
2. Check the oil level in the pump. Ensure it is filled to the correct level.
3. Check vacuum hose connections from the pump to the freeze dryer and try running the unit.
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Chapter 7: Troubleshooting
32
If vacuum problems continue, consider obtaining a second vacuum gauge capable of reading a vacuum of 0.010 mBar. It is often useful in determining if the vacuum pump is operating properly and the vacuum sensor reading is accurate.
4. Isolate the pump by disconnecting the vacuum hose from the freeze dryer. Deadhead the pump by inserting the vacuum sensor from a secondary vacuum gauge into the end of the vacuum hose and observe the vacuum reading obtained. Confirm that the pump is capable of achieving an ultimate vacuum less than 0.010 mBar or approximately 10 microns. If an inadequate vacuum reading is obtained, the pump has most likely failed and may need to be replaced or rebuilt.
II. Gaskets, Tubing, Connections, Sample Valves
1. Check all sample valves on the drying chamber/manifold and ensure all valves are closed or in the vent position. Check to ensure all fittings are tight and sealed properly against the chamber. Inspect valves for cracks or cuts.
2. Inspect gasket(s) for cracks or defects. Ensure the gasket is clean. Apply a thin coat of vacuum grease to the gasket. Keep in mind too much vacuum grease can actually cause leaks.
3. Check the drain line and ensure the drain plug is installed and the tube appears to be in good condition.
4. Check all rubber vacuum tubing for signs of deterioration or cracking.
5. Check all connections and make sure they are secure and leak tight.
6. When checking the sample valves, pull as much vacuum as possible. If a vacuum indication is displayed, wiggle or rotate the valves and watch the gauge for any fluctuations. Fluctuations can indicate a potential vacuum leak. If the valve seems to be in good condition, remove the valve and apply a thin coat of vacuum grease to the stem and the outside sealing surface of the valve body, and reinstall the valve. DO NOT APPLY VACUUM GREASE TO THE SAMPLE
VALVE GASKETS, WHICH SEAL TO THE WALL OF THE DRYING CHAMBER. If the valve still seems to be the source of
the problem, remove the valve and stopper the hole with a rubber stopper. Continue checking the other valves.
7. Make sure that the sample valve bulkhead nuts are tight. Either tighten by hand or use the wrench supplied with chambers. To use the wrench, first remove the knob and stem assembly and also the valve body. The pins on the wrench fit into the round holes of the nut. The nut should be snug but avoid over tightening. Replace the valve body and knob and stem assembly.
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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)
The illustrations below show how the sample valve installs on a chamber and a manifold.
Chapter 7: Troubleshooting
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Chapter 7: Troubleshooting
34
Isolating the freeze dryer from the accessory chamber/manifold
III. System Components and Collection Chamber Isolation
This test determines if the source of a leak is in the drying chamber.
1. Remove the drying chamber or manifold.
2. Leave the gasket on and turn a large freeze dry flask upside down to cover the connection port.
3. Start the freeze dryer and observe the vacuum indication. If the vacuum indication is good, then the problem is in the drying chamber or manifold and you should return to Section II, Gaskets, Tubing, Connections, Sample Valves.
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Chapter 7: Troubleshooting
35
Checking the connections to the pump and the vacuum tube
The following test determines if a vacuum leak is in the collection chamber.
1. Insert a rubber stopper in the small hole in the rear of the collector chamber and another in the drain port in the bottom.
2. Start the freeze dryer and observe the vacuum indication. If the vacuum is good, the problem is in the collection chamber. If it is bad, the problem is in the plumbing connections from the collection chamber to the vacuum pump.
3. If the leak is in the chamber, check the bulkhead fittings where the collection coil passes through the button of the chamber.
4. If the leak is in the plumbing connections, check all rubber parts, the drain hose, the drain plug, fittings and clamps.
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Chapter 7: Troubleshooting
36
Refrigeration Module Operation
Under a no-load condition, FreeZone Plus Cascade Freeze Dry Systems should achieve a collector temperature of –84°C (models 73860xx and 73870xx) or -105°C (models 73820xx) or lower when the vacuum pump is operating. If the collector temperature does not reach the design temperature within 30 minutes, then the refrigeration module is not functioning properly.
Cascade Systems consist of two vapor-compression refrigeration systems in series connected together via a heat exchanger. Each system has a compressor, condenser, capillary tube metering device and an evaporator.
During the operation the evaporator of the “high stage” system refrigerates the condenser of the “low stage” system. This takes place in the heat
exchanger. The low stage and high stage systems are balanced by design, however, sometimes that balance can be disrupted during operation and the unit will not function properly. If the unit is overloaded, or if the unit is defrosted and restarted in a short time interval, system unbalance is possible. If system unbalance occurs, turn the freeze dryer off and allow the unit to stabilize at ambient temperature for 2 to 4 hours.
If any repairs are required on the refrigeration module, contact your local laboratory supply dealer. If your laboratory supply dealer is unable to provide assistance, please call Labconco. Repairs should only be undertaken by a refrigeration technician or through an authorized Labconco service agency.
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Your freeze dryer has been carefully calibrated and tested before shipping, however under certain circumstances it may be necessary to adjust the calibration of the temperature and/or vacuum display or to modify alarm points. Adjustments may be necessary if the freeze dryer requires service or if it is operating on a line voltage outside the voltage range at which the alarm was preset. This DOES NOT mean that the freeze dryer may be operated at a voltage outside the ranges shown in Appendix C.
Temperature and Vacuum Display
An offset may be added to the collector temperature or vacuum display. Use an accurate traceable known reference to compare the readings.
Temperature offset may be varied ±5°C in 1°C increments. Vacuum offset may be varied ±0.020 mBar in 0.001 mBar increments.
Line Voltage Alarm Points
The freeze dryer is designed to alarm if the line voltage varies more than ±10% from nominal line voltage. Models rated to operate on 115V are preset to alarm if the voltage drops below approximately 103V or rises above approximately 127V. Models rated to operate on 230V will alarm if the voltage drops below approximately 206V or rises above approximately 254V. Some models are designed to operate below these ranges (see Appendix C). In these cases it is permissible to lower the low voltage alarm point to prevent nuisance alarms from occurring.
Low line limit may be lowered in 5 increments of approximately 2 to 3V increments for 115V models or disabled.
Low line limit may be lowered in 5 increments of approximately 4 to 5V increments for 230V models or disabled.
High line limit may be raised in 5 increments of approximately 2 to 3V increments for 115V models or disabled.
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Chapter 8: Modifying Your Freeze Dryer Display
38
PRODUCTION MENU MASTER RESET?
COLLECTOR TEMP OFFSET: O C
High line limit may be raised in 5 increments of approximately 4 to 5V increments for 230V models or disabled.
Moisture Sensor Alarm
The moisture sensor alarm may be disabled. It is shipped enabled as the factory default setting.
Modifying the Display
To enter an offset or to configure the alarms, perform the following steps:
Press and hold MENU button (approximately 10 seconds) until the display shows:
It is recommended that you do NOT perform a Master Reset because all offsets and configurations that have been entered will be lost. If you must perform a Master Reset, hold SELECT approximately 5 seconds.
This will reset:
Vacuum units to mBar Vacuum set point to 0 mBar Temperature units to °C Refrigeration total hours to 0 Vacuum pump total hours to 0 RS232 transmission rate to 10 seconds Temperature offset to 0°C Vacuum offset to 0 mBar Low line voltage to 0 V offset High line voltage to 0 V offset Moisture sensor to enabled Refrigeration to operate in Manual Mode
The display will default to the main freeze dry display information. If you do not want to restore all factory settings, but want to adjust offsets, press MENU briefly and the display shows:
Press SELECT until the appropriate offset is shown. Each number represents 1°C
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Chapter 8: Modifying Your Freeze Dryer Display
39
SDC TEMP. OFFSET: O C
VACUUM OFFSET: O uBar
LOW LINE OFFSET: 0
HIGH LINE OFFSET: 0
Press MENU and if the drying chamber has been installed, the display shows:
Press SELECT until the appropriate offset is shown. Each number represents 1°C.
Press MENU and the display shows:
Press SELECT until the appropriate offset is shown. Each number represents 0.001mBar.
Press MENU and the display shows:
Press SELECT until the appropriate offset is shown. If the freeze dryer is operating on nominal 115V, each number represents 2V. If 3 is entered into the display, the low line alarm activates when the voltage drops to approximately 97V, for example 103-(2x3)=97V. If the Freeze Dryer is operating on nominal 230V each number represents 4V (if 3 is entered into the display, the low line alarm activates when the voltage drops to approximately 194V, for example 206-(4x3)=194V. There will be no alarm indicated if DISABLED is selected.
Press MENU and the display will show
Press SELECT until the appropriate offset is shown. If the freeze dryer is operating on nominal 115V, each number represents 2V. If 3 is entered into the display, the high line alarm activates when the voltage raises to approximately 133V, for example. 127+(2x3)=133V. If the Freeze Dryer is operating on nominal 230V each number represents 4V (if 3 is entered into the display, the low line alarm activates when the voltage drops to approximately 266V, for example. 254+(4x3)=266V. There will be no alarm indicated if DISABLED is selected.
Product Service 816-333-8811 or 1-800-522-7658
Chapter 8: Modifying Your Freeze Dryer Display
40
DEFROST HEATER: NOT INSTALLED
SHELL FREEZER: NOT INSTALLED
HOLD SELECT TO CLEAR ALL TOTAL HOURS?
DRYING CHAMBER: NOT INSTALLED
PURGE VALVE: NOT INSTALLED
MOISTURE SENSOR: INSTALLED
PRODUCTION MENU: MASTER RESET?
Press MENU and the display shows:
Press and hold SELECT to change the status.
Press MENU and the display shows:
Press and hold SELECT to change the status.
Press MENU and the display shows:
Press and hold SELECT to change the status.
Press MENU and the display shows:
Press and hold SELECT if you want to disable the moisture sensor.
Press MENU and the display shows:
Press and hold SELECT to change the status
Press MENU and the display shows:
If you want to reset Total Hours, press and hold SELECT until an audible beep is heard. The display defaults to the main freeze dry display information.
If you do not want to set Total Hours, press MENU and the display shows:
Product Service 816-333-8811 or 1-800-522-7658
Chapter 8: Modifying Your Freeze Dryer Display
41
PASSWORD:
The routine repeats by pressing MENU or wait approximately 10 seconds for the display to default to the main freeze dry information display information.
In order to store offsets in memory, you Must Press and Hold MENU until display shows,
Wait approximately 10 seconds and the display defaults to the main freeze dry display information. This can be done anytime throughout the Modifying the Display routine.
Product Service 816-333-8811 or 1-800-522-7658
42
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Models
73860xx, 73870xx
Model
73820xx
Item
Part No.
Part No.
Description
1
7395800
7395800
Lid Gasket
2
7395801
7395801
Lid 3 7388400
7383600
Back Panel Assembly, 115V
7388401
7383601
Back Panel Assembly, 230V
4
7406600
7383500
Motor Fan, 115V
7406601
7383501
Motor Fan, 230V, 60 Hz
7406602
7383502
Motor Fan, 230V, 50 Hz
5
7591805
7382100
Compressor, 115V, 60 Hz Lo Stage
7591806
7382101
Compressor, 230V, 50 Hz Lo Stage
7591807
7382102
Compressor, 230V, 60 Hz Lo Stage
7591805
7382100
Compressor, 115V, 60 Hz Hi Stage
7591806
7382101
Compressor, 230V, 50 Hz Hi Stage
7591807
7382102
Compressor, 230V, 60 Hz Hi Stage
6
1302300
1302300
Switch 7 7426000
7426000
Control Panel Label
8
7445500
7445500
Printed Circuit Board
9
7728000
7728000
Drain Plug
10
1643600
1643600
O-Ring
11
7645900
7645900
Drain Hose
12
7373450
7373450
Vacuum Hose (Not Shown)
13
1336400
1336400
Power Cord, 115V (Not Shown) NEMA 5/20
1342100
1342100
Power Cord, 230V, 60 Hz (Not Shown) NEMA 6/20
1336500
1336500
Power Cord, 230V, 50 Hz (Not Shown) CEE 7/7
1332601
1332601
Power Cord, 230V, 50 Hz (Not Shown) BS 1363
1332701
1332701
Power Cord, 230V, 50 Hz (Not Shown) CH2-16P
14
7445400
7445400
Vacuum Sensor
15
7515300
7515300
Temperature Sensor, Collector (Not Shown)
16
7389402
7383300
Wire Harness, 115V (Not Shown)
7389403
7382301
Wire Harness, 230V (Not Shown)
17
7432700
7432700
Vacuum Control/Bleed Valve
18
7429700
7429700
Moisture Sensor
19
7389700
7389700
Wire Harness, Control, 115V & 230V (Not Shown)
The following is a list of components that are available for your freeze dryer. The parts shown are the most common replacement parts. If other parts are required, contact Product Service.
Product Service 816-333-8811 or 1-800-522-7658
Appendix A: Freeze Dryer Components
43
Models 73860xx and 73870xx
Product Service 816-333-8811 or 1-800-522-7658
44
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Model 73860xx
Product Service 816-333-8811 or 1-800-522-7658
Appendix B: Freeze Dryer Dimensions
45
Model 73870xx
Product Service 816-333-8811 or 1-800-522-7658
Appendix B: Freeze Dryer Dimensions
46
Model 73820xx
Product Service 816-333-8811 or 1-800-522-7658
47
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Catalog #
Voltage
Frequency
Phase
Amperage
Nominal
Operating
Range
Nominal
w/o
Vacuum
Pump
Max. with
Vacuum
Pump
7386020
115V
103-127
60 1 11
16
100V
90-110
50 1 11
16
7386021
115V
103-127
60 1 11
16
100V
90-110
50 1 11
16
7386030
230V
198-254
50 1 5.5
10
7386031
230V
198-254
50 1 5.5
10
7386040
230V
187-253
60 1 5.5
10
7386041
230V
187-253
60 1 5.5
10
7386060
230V
198-254
50 1 5.5
10
7386061
230V
198-254
50 1 5.5
10
7386070
230V
198-254
50 1 5.5
10
7386071
230V
198-254
50 1 5.5
10
7387020
115V
103-127
60 1 11
16
100V
90-110
50 1 11
16
7387021
115V
103-127
60 1 11
16
100V
90-110
50 1 11
16
7387030
230V
198-254
50 1 5.5
10
7387031
230V
198-254
50 1 5.5
10
7387040
230V
187-253
60 1 5.5
10
7387041
230V
187-253
60 1 5.5
10
7387060
230V
198-254
50 1 5.5
10
7387061
230V
198-254
50 1 5.5
10
7387070
230V
198-254
50 1 5.5
10
7387071
230V
198-254
50 1 5.5
10
This Appendix contains technical information about the freeze dryer including electrical specifications, environmental operating conditions and wiring diagrams.
Electrical Specifications
Product Service 816-333-8811 or 1-800-522-7658
Appendix C: Freeze Dryer Specifications
48
Catalog #
Voltage
Frequency
Phase
Amperage
Nominal
Operating
Range
Nominal
w/o
Vacuum
Pump
Max. with
Vacuum
Pump
7382020
115V
103-127
60 1 11.5
16
7382021
115V
103-127
60 1 11.5
16
7382030
230V
198-254
50 1 6.3
10
7382031
230V
198-254
50 1 6.3
10
7382032
230V
198-254
50 1 6.3
10
7382033
230V
198-254
50 1 6.3
10
7382034
230V
198-254
50 1 6.3
10
7382035
230V
198-254
50 1 6.3
10
7382040
230V
187-254
60 1 6.3
10
7382041
230V
187-254
60 1 6.3
10
Environmental Conditions
Indoor use only. Maximum altitude: 6562 feet (2000 meters). Ambient temperature range: 41° to 104°F (5° to 40°C). Maximum relative humidity: 80% for temperatures up to 88°F
(31°C), decreasing linearly to 50% relative humidity at 104°F (40°C).
Main supply voltage fluctuations not to exceed ±10% of the nominal
voltage.
Transient overvoltages according to Installation Categories II
(Overvoltage Categories per IEC 1010). Temporary voltage spikes on the AC input line that may be as high as 1500V for 115V models and 2500V for 230V models are allowed.
Used in an environment of Pollution degrees 2 (i.e., where normally
only non-conductive atmospheres are present). Occasionally, however, a temporary conductivity caused by condensation must be expected, in accordance with IEC 664.
Heat rejected from freeze dyer excluding the vacuum pump: Less
than 4320 BTU/HR.
Product Service 816-333-8811 or 1-800-522-7658
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PART #
DESCRIPTION
1472100
Vacuum Pump
Two stage direct drive pump, 117 liters/minute. 115 VAC, 50/60 Hz, single phase, 4.6 amps. Includes Pump Exhaust Filter
1473400. (Cat. # 1473400)
7739402
Vacuum Pump
Two stage direct drive pump, 117 liters/minute. 230 VAC, 50/60 Hz, single phase, 2.4 amps. Includes Pump Exhaust Filter
1473400. (Cat. # 1473400)
1467700
Vacuum Pump
Two stage direct drive pump, 195 liters/minute. 115 VAC, 50/60 Hz, single phase. Includes Pump Exhaust Filter. (Cat. # 1473400)
7739403
Vacuum Pump
Two stage direct drive pump, 195 liters/minute. 230 VAC, 50/60 Hz, single phase. Includes Pump Exhaust Filter. (Cat. # 1473400)
7584000
Vacuum Pump, Chemical-Resistant Hybrid
Combination two stage rotary vane pump and two stage chemistry diaphragm pump 98/115 liters/minute. 115 VAC, 50/60 Hz, single phase.
7584002
Vacuum Pump, Chemical-Resistant Hybrid
Combination two stage rotary vane pump and two stage chemistry diaphragm pump 98/115 liters/minute. 230 VAC, 50/60 Hz, single phase.
The following accessories are available for the freeze dryer.
Product Service 816-333-8811 or 1-800-522-7658
Appendix C: Freeze Dryer Specifications
50
PART #
DESCRIPTION
1472200
Pump Inlet Filter
Disposable filter that prevents oil back streaming and protects vacuum pump from submicron particles. Fits Vacuum Pumps 1472100 and 7739402.
1473400
Pump Exhaust Filter
Disposable filter that removes visible oil mist and odor from vacuum pump exhaust. Fits Vacuum Pumps 1472100 and
7739402.
1473200
Replacement Element, Oil Mist, Pump Exhaust Filter
Fits Pump Exhaust Filter 1473400.
1473300
Replacement Element, Odor, Pump Exhaust Filter, package of 5
Fits Pump Exhaust Filter 1473400 or Vacuum Pumps 1472100 and 7739402.
1988000
Vacuum Pump Oil, 1 Liter
A molecularly distilled hydrocarbon oil with low vapor pressure. For Vacuum Pumps 1472100 and 7739402.
7772000
Soda Acid Trap
Secondary trap that prevents migration of corrosive chemicals into vacuum pump.
7772100
Replacement Media for Soda Acid Trap
7772700
Vacuum Pump Oil, 1L
A mineral oil with low vapor pressure. For Vacuum Pumps 7438700, 7438800, 7769600, 7769800.
7670400
Replacement Filter Element
Disposable filter that removes oil mist from the vacuum pump exhaust. Fits Vacuum Pumps 7438700, 7438800, 7469600 and 7469800.
7584300
Vacuum Pump Oil
For Hybrid vacuum pumps 7584000, 7584002.
7772500
Carbon Solvent Trap
Secondary trap that prevents migration of organic solvents into vacuum pump.
Product Service 816-333-8811 or 1-800-522-7658
Appendix C: Freeze Dryer Specifications
51
PART #
DESCRIPTION
7772600
Replacement Activated Carbon Media for Carbon Solvent Trap
7538000
Secondary Vacuum Cold Trap
Provides additional protection for the vacuum pump when processing low eutectic samples. 9 ¾" high x 7 7/8" diameter, 304 stainless steel with ¾" vacuum connections. For use with dry ice and solvent. Cools to approximately –75°C.
7509200
Product Heater, 115V
For use in chamber 7522800. Provides 3 heated shelves operating at 43°C (110°F).
7509201
Product Heater, 230V
For use in chamber 7522800. Provides 3 heated shelves operating at 43°C (110°F).
7443500
Clear Drying Chamber with 8 Valves
For bulk drying or drying in flasks.
7442100
Drying Rack- Unheated
Provides three shelves. For use in Chambers 7443500 and
7522800.
7442900
Clear Drying Chamber
For bulk drying.
7522300
20 Port Manifold
10" high x 27 ½" wide x 8 5/8" deep. Type 304 stainless steel manifold with 20 freeze dry valves.
7868500
48 Port Ampule Manifold
28 5/8" high x 5" wide x 5" deep. Type 304 stainless steel with 48 each ¼" tube stems.
7509600
Sample Valve Kit
Includes neoprene valve body, knob and installation parts.
7522900
16 Port Drying Chamber
13" high x 138" diameter, 304 stainless steel with 16 freeze dry valves.
Product Service 816-333-8811 or 1-800-522-7658
Appendix C: Freeze Dryer Specifications
52
Size
Vials with
Screw Caps
Stoppers
5 ml
7762300
7762200
10 ml
7762600
7762200
Size
20 mm
Corkage
13 mm
Corkage
Split
Stoppers
Aluminum
Seals
Sleeve-Type
Stoppers
2 ml 7575010
7576010
7577010
3 ml 7575210
7576010
7577010
5 ml
7573010
7576210
7577110
757710
10 ml
7573210
7576210
7577110
7577510
20 ml
7573410
7576210
7577110
7577510
30 ml
7573610
7576210
7577110
7577510
50 ml
7573810
7576210
7577110
7577510
100 ml
7574010
7576210
7577110
7577510
125 ml
7574210
7576210
7577110
7577510
Threaded Vials
Stoppers and threaded vials with Screw Caps are supplied in packages of 200.
Perfect for long term storage of freeze dried samples. Labconco Serum Bottles and Treaded Vials are specifically designed for lyophilization applications. Their uniform thin wall construction ensures even freezing and drying. Bottles and vials are ideal containers for use in the FreeZone Stoppering Tray Dryer. Serum bottles also connect to valve ports on drying chambers and manifolds.
Serum Bottles
Serum Bottles, Stoppers and seals are supplied in packages of 100.
Seal Crimper
Secures tear-away Aluminum Seals.
7578000 Seal Crimper for 13 mm corkage. Shipping weight 3 lbs. (1.4 kg) 7578100 Seal Crimper for 20 mm corkage. Shipping weight 3 lbs. (1.4 kg)
Serum Bottles and Vials
Product Service 816-333-8811 or 1-800-522-7658
53
Flask
Size
Complete
Flask
Flask
Bottom
Flask
Top
Flask Top
Adapter
Diameter*
Dimensions/
Flask Bottom
H x D
40 ml
7540000
7542000
7544000
½"
76mm 34mm
80 ml
7540200
7542200
7544000
½"
115mm x 34mm
120 ml
7540300
7542300
7544200
¾"
68mm x 59.2mm
150 ml
7540400
7542400
7544200
¾"
85mm x 59.2mm
300 ml
7540600
7542600
7544200
¾"
145mm x 59.2mm
600 ml
7540800
7542800
7544400
¾"
135mm x 90.2mm
750 ml
7541100
7542700
754400
¾"
162mm x 90.2mm
900 ml
7540900
7542900
7544400
¾"
190mm x 90.2mm
1200 ml
7541000
7543000
7544400
¾"
240mm x 90.2mm
2000 ml
7541200
7543200
7544400
¾"
380mm x 90.2mm
*Valves on the freeze dry system, drying chambers and manifolds offered in this catalog fit adapters of both ½" and ¾" sizes. Size information is provided for selecting adapters for older Labconco models and other freeze dryers.
Fast-Freeze Flasks are specially designed to be easier to handle, faster to load and more convenient to use than other freeze dry glassware now in your laboratory. Compatible with all major brands of laboratory freeze dry equipment, Fast-Freeze Flasks eliminate the risk of contamination from vacuum grease, reduce spillage of valuable samples and require no washers, gaskets or retainers.
How to select Fast-Freeze Flasks for your Freeze Dry System
Select fast-Freeze Flasks based on your sample sizes. Flasks should be filled no more than one­third of their volume so that maximum surface area is achieved and efficient lyophilization is assured. A complete Fast-Freeze Flask includes a rubber top, glass bottom and a supply of filter paper. Tops, bottoms and filter paper are available separately as replacement components. Adapters are required to attach flasks to freeze dry valve ports.
Adapters
Add the adapters for connecting the Fast-Freeze Flasks to the valve ports on your drying chamber or manifold. Choose borosilicate glass or stainless steel adapters in ½" and ¾" diameters.
7544810 Replacement Filter Paper
1000 (10 packages of 100). 1" diameter (28mm). Pore size 17 micron. Shipping weight 0.5lb.
Fast-Freeze Flasks
Appendix C: Freeze Dryer Specifications
Product Service 816-333-8811 or 1-800-522-7658
Appendix C: Freeze Dryer Specifications
54
Adapters
Add the adapters for connecting the Lyph-Lock Flasks to the valve ports on your drying chamber or manifold.
90° Bend Adapter
Description
7568000
Connects 19/38 STj Flask Top to ½" valve*
7568200
Connects 19/38 STj Flask Top to 3/4"valve*
7568400
Connects 24/40 STj Flask Top to ½" valve*
7568600
Connects 24/40 STj Flask Top to 3/4" valve*
Flask Size
Complete
Flask
19/38 STj
Complete
Flask
24/40 STj
Flask Top
19/38 STj
Flask Top
24/40 STj
Lyph-Lock
Seal
Flask
Bottom
Dimensions/
Flask Bottom
H x ID
25 ml
7550000
7550000
7552000
7556000
7559000
7557000
37mm x 34mm
50 ml
7550200
7554200
7552000
7556000
7559000
7557200
67mm x 34mm
100 ml
7550400
7554400
7552200
7556200
7559200
7557400
50mm x 59.2mm
250 ml
7550600
7554600
7552200
7556200
7559200
7557600
110mm x 59.2mm
500 ml
7550800
7554800
7552400
7556400
7559400
7557800
103mm x 90.2mm
750 ml
7550900
7554900
7552400
7556400
7559400
7557900
145mm x 90.2mm
1000 ml
7551000
7555000
7552400
7556400
7559400
7558000
187mm x 90.2mm
Lyph-Lock Flasks simplify your Lyophilization procedures because they have only three pieces per flask – a high strength borosilicate glass top and bottom with a silicone rubber ring seal. The unique wide-mouth design helps you load samples easily and lyophilize efficiently.
How to select Lyph-Lock Flasks for your Freeze Dry System
Select Lyph-Lock Flasks fast- based on your sample sizes. Flasks should be filled no more than one-third of their volume so that maximum surface area is achieved and efficient lyophilization is assured. A complete Lyph-Lock Flask includes a glass top and bottom and a rubber ring seal. Tops, bottoms and seals are available separately as replacement components. Adapters are required to attach flasks to freeze dry valve ports.
Lyph-Lock Flasks
*Valves on the freeze dry system, drying chambers and manifolds offered in this catalog fit adapters of both ½" and ¾" sizes. Size information is provided for selecting adapters for older Labconco models and other freeze dryers.
Product Service 816-333-8811 or 1-800-522-7658
55
Size
Straight
Pre-Scored
Flat Bottom
1 ml
7572710
7570610
2 ml 7570810
4 ml
5 ml 7571010
10 ml 7571210
25 ml
50 ml
Labconco Ampules are fabricated of highest quality borosilicate glass for strength and durability. They are available in five different configurations to provide the ideal ampule for your specific lyophilization requirements, from tray drying to flame sealing applications.
Ampules
Ampules are supplied in packages of 100.
Oxygen/Natural Gas Sealing Torch
7578500 Torch specifically designed for flame sealing freeze dry ampules. Seals all types of heat-resistant glass. Connects to natural gas, butane or propane and oxygen with ¼" ID hose connectors. Shipping weight 3 lbs. (1.4 kg).
Ampule Valve Adapters
7593401 Adapter connects ampules to valve ports or stainless steel stems. Ten per package. Shipping weight 0.5 lbs. (0.2 kg).
Trident Adapter
7762700 Three Way Adapter permits attachment of three ampules to a single valve port. Ampules are attached using Ampule Valve Adapters or 1/8" surgical tubing (not provided). Cavity in adapter body can be filled with cotton fiber media to help prevent contamination between samples. Shipping weight 3 oz. (0.1 kg).
Ampules
Appendix C: Freeze Dryer Specifications
Product Service 816-333-8811 or 1-800-522-7658
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