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User's Manual
®
FreeZone
Plus
Freeze Dry Systems
Models
7386020
7386021
7386030
7386031
7386040
7386041
Please read the User's Manual before operating the equipment.
4.5 Liter Cascade
™
7387020
7387021
7387030
7387031
7387040
7387041
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complete your product registration card
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Labconco Corporation
8811 Prospect Avenue
Kansas City, MO 64132-2696
800-821-5525, 816-333-8811
FAX 816-363-0130
E-MAIL
labconco@labconco.com
HOME PAGE www.labconco.com
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Related Manuals for Labconco FreeZone Plus
Summary of Contents for Labconco FreeZone Plus
- Page 1 7387030 7386031 7387031 7386040 7387040 7386041 7387041 To receive important product updates, complete your product registration card online at register.labconco.com 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.
- Page 2 The warranty for all Labconco products will expire one year from date of installation or two years from date of shipment from Labconco, whichever is sooner, except the following;...
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Page 3: Table Of Contents
CHAPTER 1: INTRODUCTION Freeze Dry Process Freeze Dry Rates Freeze Dry Capacity Samples Containing Volatile Substances Safety Symbols CHAPTER 2: PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements Chamber or Manifold Requirements CHAPTER 3: GETTING STARTED Unpacking Your Freeze Dryer Freeze Dryer Components Setting Up Your Freeze Dryer Vacuum Pump Connection... - Page 4 Alarms Power Failure Line Voltage Out of Range Temperature Out of Range Service Vacuum Pump Moisture in Collector CHAPTER 5: MAINTAINING YOUR FREEZE DRYER CHAPTER 6: USING THE RS232 RECEPTACLE Computer Connection for Computer Interface CHAPTER 7: TROUBLESHOOTING Vacuum Pump Gaskets, Tubing, Connections, Sample Valves System Components &...
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Page 5: Chapter 1: Introduction
Congratulations on your purchase of a Labconco FreeZone® Freeze Dry System, which is designed for laboratory lyophilization procedures. The refrigerant used in the refrigeration system is CFC-free so it will not endanger the environment. The unit is easy to install and maintain. Proper care and maintenance of this product will result in many years of dependable service. -
Page 6: Freeze Dry Rates
Chapter 1: Introduction Freeze Dry Rates The efficiency of the freeze drying process is dependent upon the surface area and the thickness of the sample, the collector temperature and vacuum obtained, the eutectic point and solute concentration of the sample. It is important to remember these factors when trying to obtain efficient utilization of your freeze dry system. -
Page 7: Freeze Dry Capacity
Chapter 1: Introduction In order for lyophilization to occur, ice must be removed from the frozen sample via sublimation. This is accomplished by the collector and the vacuum pump. The collector, which should be at least 15 to 20°C colder than the eutectic temperature (melting temperature) of the sample, traps vapor as ice. -
Page 8: Samples Containing Volatile Substances
Chapter 1: Introduction If there is a problem with a particular type of sample melting when placed on the freeze dry system, dilution of the sample with more water or providing some insulation around the flask to decrease the rate of heat absorption by the sample may help. - Page 9 Chapter 1: Introduction Throughout this manual potentially hazardous conditions are identified using the following words and symbols. It is important that you understand the warnings listed throughout this manual before you operate the freeze dry system. Product Service 816-333-8811 or 1-800-522-7658...
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Page 10: 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: •... -
Page 11: Vacuum Pump Requirements
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. -
Page 12: 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. •... -
Page 13: Unpacking Your Freeze Dryer
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. -
Page 14: Setting Up Your Freeze Dryer
Drying Chamber with 12 valves 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. -
Page 15: Electrical Connection
Chapter 3: Getting Started 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. -
Page 16: Solvent Safety Precautions
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. - Page 17 Chapter 3: Getting Started 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.
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Page 18: Chapter 4: Using Your Freeze Dryer
After your Freeze Dryer has been installed as detailed in Chapter 3: Getting Started, you are ready to begin using your Freeze Dryer. Read this chapter to learn how to: • operate the controls. • understand the display. • connect samples. Do not use the freeze dryer in a manner not specified by the manufacturer (refer to Appendix C: Freeze Dryer Specifications). -
Page 19: Freeze Dryer Controls
Chapter 4: Using Your Freeze Dryer Freeze Dryer Controls The control panel for the freeze dryer is shown below with a description about its function. 1. 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. -
Page 20: Operation Checklist
Chapter 4: Using Your Freeze Dryer 11. Collector Temperature Graph Display – This display indicates the temperature of the collector. The highest LED indicates the collector temperature is warmer than 10°C. The indicators will sequence down when the temperature reaches 10, 0, -10, -20, -30, -40°C. -
Page 21: Operating The Freeze Dryer
Chapter 4: Using Your Freeze Dryer Operating the Freeze Dryer Set-Up The freeze dryer may be configured to automatically start the vacuum pump when the collector temperature reaches –40°C. The display units for vacuum may be selected to be mBar, Pascal (Pa) or Torr and the temperature may be displayed as °F or °C. - Page 22 Chapter 4: Using Your Freeze Dryer • Press SELECT until the desired units are flashing. • Press MENU. • The display shows: REFRIG TOTAL HOUR: XXXX SERVICE HOUR: XXXX • To reset the SERVICE HOUR to 0 press SELECT. This allows you to keep track of the time the refrigeration system operated since it was serviced.
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Page 23: Automatic Start-Up
Chapter 4: Using Your Freeze Dryer • To change the rate press and hold SELECT until the desired time interval is shown. The time between data transmissions may be set to occur at 10, 30, 60, 300 or 600 second intervals. •... -
Page 24: Setting The Operating Vacuum Level
Chapter 4: Using Your Freeze Dryer Setting the Operating Vacuum Level The vacuum level may be set by the user to optimize the freeze dry process. Normally, the sublimation rate will increase if there is less vacuum (a higher pressure) in the freeze dryer. A good starting place is to set the vacuum so its level is equivalent to about 10°C colder than the eutectic or collapse temperature of the sample. -
Page 25: Adding Sample
Chapter 4: Using Your Freeze Dryer Adding Sample The following procedure should be followed when using sample valves in the freeze dry process: 1. Connect a pre-frozen sample to a sample valve on the drying chamber or manifold using an adapter. Turn the plastic valve knob to the “VACUUM” position to open the valve, which connects the attached sample to system vacuum. -
Page 26: Shut Down
Chapter 4: Using Your Freeze Dryer 5. Ampules may be flame sealed while connected to a valve by using a sealing torch. Care must be taken not to burn the valve. An insulation material placed between the valve and the torch is recommended. Shut Down At the end of a run or when a sufficient amount of condensate accumulates on the collector coil to obstruct the flow of vapor to the collector chamber,... -
Page 27: Alarms
Chapter 4: Using Your Freeze Dryer Alarms A number of unusual events may occur during a lyophilization procedure that can adversely effect the operation of the freeze dryer. If an event occurs, the alarm indicator flashes and the beeper sounds. The beeper automatically mutes itself after one minute. -
Page 28: Temperature Out Of Range
Chapter 4: Using Your Freeze Dryer Temperature Out of Range An alarm activates if the collector temperature rises above –40°C. If this occurs, the display shows: COLLECTOR TEMPERATURE HOLD SELECT TO CLEAR IT Press and hold SELECT for five seconds until the error message is cleared from the display. - Page 29 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.
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Page 30: Chapter 5: Maintaining Your Freeze Dryer
Chapter 5: Maintaining Your Freeze Dryer Monthly: 1. The rubber components on the freeze dryer may eventually deteriorate and require replacement. The effective life of rubber parts depends upon both their usage and the surrounding environment. Check all rubber hoses and gaskets and replace any that show signs of hardening, permanent set or deterioration. -
Page 31: Chapter 6: Using The Rs232 Receptacle
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. - Page 32 Chapter 6: Using the RS232 Receptacle The time between data transmissions may be varied by the user to occur at 10, 30, 60, 300 or 600 second intervals. Press the MENU button until the RS232 screen appears on the display. RS-232 TRANSMISSION RATE SECONDS Press select until the desired time interval is shown.
- Page 33 Chapter 6: Using the RS232 Receptacle 3. The “Connection Description” dialogue box opens. Type in a user defined name and select an icon for the new connection. Press “OK.” 4. The “Connect To” dialogue box opens. Using the down arrow selection button, select the communication port to which the cable has been connected.
- Page 34 Chapter 6: Using the RS232 Receptacle 5. The “Com X Properties” dialogue box opens. Enter the appropriate data properties and press “OK.” 6. When the freeze dryer main power switch is on, the data is transmitted and updated at the time intervals selected by the user. Product Service 816-333-8811 or 1-800-522-7658...
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Page 35: Chapter 7: Troubleshooting
Refer to the following if your freeze dryer fails to operate properly. If the suggested corrective actions do not solve your problem, contact Labconco for additional assistance. FreeZone Freeze Dry Systems that are clean, dry and without samples attached should reach a vacuum of 0.133 mBar within 10 minutes and should achieve an ultimate vacuum of 0.033 mBar within 18 hours when the... -
Page 36: Ii. Gaskets, Tubing, Connections, Sample Valves
Chapter 7: Troubleshooting If vacuum problems continue, consider obtaining a second vacuum gauge capable of reading a vacuum of 0.010 mBar. It is often useful in determining if the vacuum pump is operating properly and the vacuum sensor reading is accurate. - Page 37 Chapter 7: Troubleshooting The illustrations below show how the sample valve installs on a chamber and a manifold. Knob & Stem Assembly Valve Body Valve Assembly (Clear Chamber with Valves) Bulkhead Nut Valve Body Manifold Assembly Thrust Washer Valve Body Thrust Washer Gasket Knob &...
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Page 38: System Components & Collection Chamber Isolation
Chapter 7: Troubleshooting III. System Components and Collection Chamber Isolation This test determines if the source of a leak is in the drying chamber. 1. Remove the drying chamber or manifold. 2. Leave the gasket on and turn a large freeze dry flask upside down to cover the connection port. - Page 39 Chapter 7: Troubleshooting The following test determines if a vacuum leak is in the collection chamber. 1. Insert a rubber stopper in the small hole in the rear of the collector chamber and another in the drain port in the bottom. 2.
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Page 40: Refrigeration Module Operation
Chapter 7: Troubleshooting Refrigeration Module Operation Under a no-load condition, FreeZone Plus Cascade Freeze Dry Systems should achieve a collector temperature of –81°C or lower when the vacuum pump is operating. If the collector temperature does not reach the design temperature within 40 minutes, then the refrigeration module is not functioning properly. -
Page 41: Chapter 8: Modifying Your Freeze Dryer Display
Your freeze dryer has been carefully calibrated and tested before shipping, however under certain circumstances it may be necessary to adjust the calibration of the temperature and/or vacuum display or to modify alarm points. Adjustments may be necessary if the freeze dryer requires service or if it is operating on a line voltage outside the voltage range at which the alarm was preset. -
Page 42: Moisture Sensor Alarm
Chapter 8: Modifying Your Freeze Dryer Display High line limit may be raised in 5 increments of approximately 4 to 5V increments for 230V models or disabled. Moisture Sensor Alarm The moisture sensor alarm may be disabled. It is shipped enabled as the factory default setting. - Page 43 Chapter 8: Modifying Your Freeze Dryer Display Press MENU and if the drying chamber has been installed, the display shows: SDC TEMP. OFFSET: Press SELECT until the appropriate offset is shown. Each number represents 1°C. Press MENU and the display shows: VACUUM OFFSET: O uBar Press SELECT until the appropriate offset is shown.
- Page 44 Chapter 8: Modifying Your Freeze Dryer Display Press MENU and the display shows: DRYING CHAMBER: NOT INSTALLED Press and hold SELECT to change the status. Press MENU and the display shows: PURGE VALVE: NOT INSTALLED Press and hold SELECT to change the status. Press MENU and the display shows: DEFROST HEATER: NOT INSTALLED...
- Page 45 Chapter 8: Modifying Your Freeze Dryer Display The routine repeats by pressing MENU or wait approximately 10 seconds for the display to default to the main freeze dry information display information. In order to store offsets in memory, you Must Press and Hold MENU until display shows, PASSWORD: Wait approximately 10 seconds and the display defaults to the main freeze...
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Page 46: Appendix A: Freeze Dryer Components
The following is a list of components that are available for your freeze dryer. The parts shown are the most common replacement parts. If other parts are required, contact Product Service. Models 73860xx and 73870xx Item Part No. Description 7395800 Lid Gasket 7395801 7388400... - Page 47 Appendix A: Freeze Dryer Components Models 73860xx and 73870xx Product Service 816-333-8811 or 1-800-522-7658...
- Page 48 Model 73860xx Product Service 816-333-8811 or 1-800-522-7658...
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Page 49: Appendix B: Freeze Dryer Dimensions
Appendix B: Freeze Dryer Dimensions Model 73870xx Product Service 816-333-8811 or 1-800-522-7658... -
Page 50: Appendix C: Freeze Dryer Specifications
This Appendix contains technical information about the freeze dryer including electrical specifications, environmental operating conditions and wiring diagrams. Electrical Specifications Catalog # Voltage Frequency Phase Amperage Nominal Max. with Operating Nominal Vacuum Range Vacuum Pump Pump 7386020 115V 103-127 100V 90-110 7386021 115V... -
Page 51: Environmental Conditions
Appendix C: Freeze Dryer Specifications 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). •... -
Page 52: Wiring Diagram (115V) And (230V)
Appendix C: Freeze Dryer Specifications Wiring Diagram, Catalog # 7386020, 7386021 and 7387020, 7387021 (115V, 60 Hz Models) Product Service 816-333-8811 or 1-800-522-7658... - Page 53 Appendix C: Freeze Dryer Specifications Wiring Diagram Catalog # 7386030, 7386031, 7386040, 7386041 and 7387030, 7387031, 7387040 and 7387041 (230V, 50 or 60 Hz Models) Product Service 816-333-8811 or 1-800-522-7658...
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Page 54: Appendix D: Freeze Dryer Accessories
The following accessories are available for the freeze dryer. 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. - Page 55 Appendix D: Freeze Dryer Accessories 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.
- Page 56 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 7772500 Carbon Solvent Trap Secondary trap that prevents migration of organic solvents into vacuum pump. 7772600 Replacement Activated Carbon Media for Carbon Solvent Trap 7538000 Secondary Vacuum Cold Trap Provides additional protection for the vacuum pump when processing low eutectic samples.
- Page 57 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 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"...
- Page 58 5 ml 7762300 7762200 10 ml 7762600 7762200 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.
- Page 59 *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...
- Page 60 187mm x 90.2mm *Valves on the freeze dry system, drying chambers and manifolds offered in this catalog fit adapters of both ½" and ¾" sizes. Size information is provided for selecting adapters for older Labconco models and other freeze dryers.
- Page 61 Connects to natural gas, butane or propane and oxygen with ¼" ID hose connectors. Shipping weight 3 lbs. (1.4 kg). Labconco Ampules are fabricated of highest quality borosilicate glass for strength and durability. They are available in five different configurations to provide...
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Page 62: Declaration Of Conformity
Directive(s) and Standard(s). See individual Declaration of Conformity which will be signed by the importer for your country. Place: _______________________________________ (Signature) Date: _______________________________________ (Full Name) _______________________________________ (Position) Labconco P/N 36960-02, Rev. F, ECO E652 Product Service 816-333-8811 or 1-800-522-7658...
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