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User's Manual
FreeZone
Triad
Models
74000 Series
Please read the User's Manual before operating the equipment.
Freeze Dry System
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Labconco Corporation
8811 Prospect Avenue
Kansas City, MO 64132-2696
800-821-5525, 816-333-8811
FAX 816-363-0130
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Table of Contents
Related Manuals for Labconco FreeZone Triad 74000 Series
Summary of Contents for Labconco FreeZone Triad 74000 Series
- Page 1 FreeZone Triad Freeze Dry System Models 74000 Series 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...
- Page 2 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.
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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 CHAPTER 2: PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements CHAPTER 3: GETTING STARTED Unpacking Your Triad Freeze Dry Triad Freeze Dry Components Setting Up Your Triad Freeze Dry System Component Orientation and Hose Connection Venting the Vacuum Pump Electrical Connection... - Page 4 Freeze Drying inside the Chamber Manual Mode with Pre Frozen Samples Manual Mode with Unfrozen Samples Auto Mode with Pre Frozen Samples Auto Mode with Unfrozen Samples Stoppering Vials Vacuum Break/Backfilling Freeze Drying using Manifold Valves Defrosting Alarms Shelf Temperature Variations Collector Temperature Variations Vacuum Vacuum Pump Service...
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Page 5: Chapter 1: Introduction
Congratulations on your purchase of a Labconco FreeZone® Triad 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 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. - Page 8 Chapter 1: Introduction 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.
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Page 9: Chapter 2: Prerequisites
Before you install your Triad Freeze Dry System, you must be certain that the area is level and of solid construction. An electrical source must be located near the installation site. Carefully read this chapter to learn: Electrical supply requirements. ... -
Page 10: Vacuum Pump Requirements
Vacuum pumps should be equipped with a reverse IEC plug. This will allow the vacuum pump to be plugged into the receptacle on the back panel of the Freeze Dry System. Refer to Appendix D: Triad Freeze Dry System Accessories for vacuum pumps available from Labconco. Product Service 816-333-8811 or 1-800-522-7658... -
Page 11: Unpacking Your Triad Freeze Dry
(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 dry system until you have checked all of the components, installed and tested the system. -
Page 12: Chapter 3: Getting Started
Locate the model of freeze dry system you received in the following table. Verify that the components listed are present and undamaged. If you did not receive one or more of the components listed, contact Labconco Corporation immediately for further instructions. Power Cords Description... -
Page 13: Venting The Vacuum Pump
Chapter 3: Getting Started Figure 1 Venting the Vacuum Pump If any materials will be placed in the freeze dry system that can liberate hazardous gases when heated, the vacuum pump exhaust must be vented to a fume hood or other ventilation device. Electrical Connection Connect the power cord into the receptacle on the back of the freeze dry system and connect the other end into a suitable power receptacle. - Page 14 Optional secondary traps are available to help extend the life of the vacuum pump. These traps are installed between the freeze dry system and the vacuum pump. Contact Labconco for assistance in determining which trap is right for your application.
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Page 15: 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 dry system, 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 dry system may be flammable or hazardous to your health. - Page 16 Read this chapter to learn how to: Understand the display. Operate the controls. Connect samples. Do not use the freeze dry system in a manner not specified by the manufacturer (refer to Appendix C: Freeze Dry System Specifications).
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Page 17: Chapter 4: Operating Instruction
Chapter 4: Operating Instructions Triad Freeze Dry System Controls The control panel for the Triad Freeze Dry System is shown with a description about its function. Figure 2 1. Display: Displays all necessary programming and operational data. Provides prompts to aid in programming. 2. -
Page 18: Operation Checklist
Chapter 4: Operating Instructions 12. Run/Stop Button: Initiates the start or stop of the lyophilization process. 13. Run/Stop Indicator: Green INDICATOR burns steadily while freeze drying is in progress and turns off when the Run/Stop button terminates a run. The green INDICATOR flashes if freeze drying is in progress and a power failure occurs. -
Page 19: Operating The Triad Freeze Dry System
Chapter 4: Operating Instructions Operating the Triad Freeze Dry System Set-Up Vacuum may be displayed in mBar, Pascal (Pa) or Torr and the temperature may be displayed as either °F or °C. The refrigeration system and vacuum pump operating time may be monitored and the operating vacuum level may be set. - Page 20 Chapter 4: Operating Instructions Press ENTER if you do not want to reset SERVICE HOURS. Press and hold for 5 seconds to reset the Service Hours to 0. This allows you to keep track of the time the refrigeration system operated since it was serviced.
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Page 21: Setting The Operating Vacuum Level
Chapter 4: Operating Instructions The display will show: VACUUM UNITS: MBar Torr At any time the DISPLAY button can be pressed to select a different function. Setting the Operating Vacuum Level The vacuum level may be manually set by the user to optimize the freeze dry process. -
Page 22: Manual Control Operation
Chapter 4: Operating Instructions Manual Control Operation The manual operation has three selectable modes: Pre-Freeze, In-Flask and controlled shelf temperature. The Pre-Freeze setting allows the shelf temperature to freeze samples below –55°C obtaining “Max Cold” temperature of approximately –75°C. The In-Flask setting is used to freeze dry pre-frozen samples when using only the sample valves on the left side of the unit. -
Page 23: Automatic Control Operation
Chapter 4: Operating Instructions The segment numbers will always show “M” while operating in the manual mode. Segment numbers are used only in the automatic mode to identify portions of the programmed cycle. Temperatures and vacuum are displayed in the units selected during the set up procedure. -
Page 24: Programming
Chapter 4: Operating Instructions When the desired temperature is achieved, the hold function will maintain that temperature for the programmed length of time. The microprocessor control has a built in memory of the last entered program to allow the identical protocol to be repeated by simply pushing the RUN button. A typical 3-segment program is shown in Figure 3. -
Page 25: Starting The Freeze Dry Cycle
Chapter 4: Operating Instructions The display will show the parameters that were last entered for this program. SEG 1 RAMP 00.0°C/MN HOLD –34°C TIME 00.0 If any of the parameters are changed, the ENTER button must be pressed for the new value to be stored. If ENTER is not pressed within 10 seconds after the last parameter adjustment, the value will return to the previously stored value. -
Page 26: Changing The Program Parameters In The Middle Of A Run
Chapter 4: Operating Instructions During the hold cycle of the active segment the display will alternate as follows: Selected Program SHLF Shelf Temperature SAMP Sample Temperature (if probe is not installed, the display shows ---) P1 SHLF = -55 SAMP= -55°C Collector Temperature COL = -85 SEG = 1H VAC = .030M... -
Page 27: Monitoring The System Operation
Chapter 4: Operating Instructions Monitoring the System Operation Press the DISPLAY button to obtain the Monitor Screen. The display will show the collector temperature, shelf temperature, system vacuum and sample temperatures. If the sample probe is not connected, the sample temperature display will show “- - -”. -
Page 28: Manual Mode With Unfrozen Samples
Chapter 4: Operating Instructions Note: The system will go from room temperature start up to –55°C in under 7 hours. 5. Shelf temperatures and vacuum set points can be changed at anytime during the manual Freeze Dry process. Manual Mode with Unfrozen Samples 1. -
Page 29: Stoppering Vials
Chapter 4: Operating Instructions compromised and damage could occur to the vacuum pump when turned on in segment 1. 2. Set mode to AUTO. 3. Place the unfrozen samples on the shelf and close the door. 4. Start the refrigeration system by pressing “RUN/STOP.” Note: The vacuum pump will run 10 seconds and then turn off automatically. -
Page 30: Freeze Drying Using Manifold Valves
Chapter 4: Operating Instructions Freeze Drying Using Manifold Valves The following procedure should be followed when using the sample valves for the freeze dry process: 1. Turn on the Triad Freeze Dry System. Select manual mode, change the set point temp to “IN-FLASK” and turn on the vacuum. 2. -
Page 31: Defrosting
Chapter 4: Operating Instructions 5. To remove a container after freeze 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. -
Page 32: Alarms
Chapter 4: Operating Instructions Alarms A number of events may occur during a lyophilization procedure that can adversely effect the operation of the Triad Freeze Dry System. If an event occurs, the alarm indicator will flash and beep. The beep will automatically mute itself after one minute. The specific alarm can be identified by observing the display. -
Page 33: Platen Tilt
Chapter 4: Operating Instructions Platen Tilt If the stoppering platen tilts more than 4° while stoppering, the platen will stop. The display will read “SHELF UNEVENLY LOADED.” Product Service 816-333-8811 or 1-800-522-7658... - Page 34 Before using any cleaning or decontamination method except those recommended by Labconco, users should check with Labconco to determine that the proposed method will not damage the equipment. 2. Clean up all spills; remove liquids from the chamber.
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Page 35: Chapter 5: Maintaining Your Freeze Dry System
Chapter 5: Maintaining Your Freeze Dry System Monthly: 1. The rubber components on the freeze dry system 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 36: 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 Labconco Freeze Dry System. 2. Computers with a 9-pin D-sub male serial connector should use Connect Cable, Labconco part number 7537800, to connect a computer to the Labconco Freeze Dry System. - Page 37 Chapter 6: Using the RS232 Receptacle Press or until the desired time interval is shown. Press ENTER. The format of the transmitted message with typical values is as follows: PROG = 1 SEG = 2R TRM = 17 COL = -85 SHLF = -55 SAMP = -55 VAC = 180 Where: PROG Program...
- Page 38 Chapter 6: Using the RS232 Receptacle 3. The “Connection Description” dialogue box will open. Type in a user defined name and select an icon for the new connection. Press “OK.” 4. The “Connect To” dialogue box will open. Using the down arrow selection button, select the communication port to which the cable has been connected.
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Page 39: Chapter 7: Troubleshooting
Refer to the following if your freeze dry system fails to operate properly. If the suggested corrective actions do not solve your problem, contact Labconco for additional assistance. Vacuum System FreeZone Triad Freeze Dry Systems that are clean and dry and without samples attached should reach a vacuum of 0.133 mBar within 30 minutes... -
Page 40: 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 41: Diagnostic Mode
Chapter 7: Troubleshooting The illustration below shows how the sample valve installs on the chamber. Figure 5 Diagnostic Mode In the event that there is a problem with the Triad Freeze Dry System, a diagnostic mode is available. This mode can be used to diagnose problems by isolating individual system components to confirm their operation. - Page 42 Chapter 7: Troubleshooting The shelf valve opens and refrigeration system turns on or press . The display will show: REFRIGERATION -- COLL The collector valve opens. The (shelf valve closes) refrigeration system remains on or press . The display will show: REF + LEX PUMP The refrigeration system remains on.
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Page 43: Refrigeration Module Operation
20°C, the freeze dry system refrigeration system can achieve a shelf temperature of –75°C or lower within 4 hours. If any repairs are required on the refrigeration module, please call Labconco. Repairs should only be undertaken by a competent refrigeration technician or through an authorized Labconco service agency. - Page 44 Chapter 7: Troubleshooting Disconnect power cord from supply outlet. Make sure the Power Switch is in the OFF position. Remove the rear cover to expose the marked back foam insulation. Cut through the foam along the marked lines and remove center cutout.
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Page 45: Heat Transfer Fluid Precautions
Chapter 7: Troubleshooting Heat Transfer Fluid Precautions The fluid’s name and manufacturer are: Name: Lexol 542 Manufacturer: Santa Barbara Chemical Co. 927 Indio Muerto Santa Barbara, CA 93140 805-963-7793 The fluid used for heat transfer in this system is combustible and hazardous. Leaks and spills should be attended to immediately or serious injury could occur. -
Page 46: Chapter 8: Modifying Your Freeze Dry System Display
Your Triad Freeze Dry System has been carefully calibrated and tested before shipping, however under certain circumstances it may be necessary to adjust the calibration of the vacuum display or to reset factory settings. These adjustments may be necessary if the freeze dry system requires service. An offset may be added to the vacuum display. - Page 47 Chapter 8: Modifying Your Freeze Dry System Display If you do not want to restore all factory settings, but want to adjust the vacuum offset, press DISPLAY briefly and the display will show: VACUUM OFFSET: 0 mBar Press or until the appropriate offset is shown. Each number represents an offset of 0.001 mBar Press DISPLAY and the display will show: COLLECTOR TEMP.
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Page 48: Appendix A: Freeze Dry System Components
The following pages list components that are available for your freeze dry system. The parts shown are the most common replacement parts. If other parts are required, contact Product Service. Item Part No. Description Compressor 230V – 50 Hz 7591806 Compressor 230V –... - Page 49 Appendix A: Freeze Dry System Components Figure 7 Product Service 816-333-8811 or 1-800-522-7658...
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Page 50: Appendix B: Freeze Dry System Dimensions
Figure 8 Serum Bottle Capacity of the Triad Freeze Dry System Size Labconco No (100 pcs.). Shelf Capacity 2 ml 7575010 3 ml 7575210 5 ml 7573010 10 ml 7573210 20 ml 7573410 30 ml 7573610 50 ml 7573810 100 ml... -
Page 51: Appendix C: Freeze Dry System Specifications
This Appendix contains technical information about the freeze dry system’s electrical specifications and environmental operating conditions. Electrical Specifications Voltage Catalog Operating Number Description Nominal Range Frequency Phase Amperage 7400030 Triad Freeze Dry System 198-254 7400040 Triad Freeze Dry System 187-253 7400060 Triad Freeze Dry System 198-254 7400070 Triad Freeze Dry System... -
Page 52: Performance Specifications
Appendix C: Freeze Dry System Specifications Performance Specifications Collector Minimum Temperature (°C) Collector Capacity in 24 Hours (Liters) 1.84 Collector Total Capacity (Liters) Shelf Minimum Temperature (°C) Shelf Control Temperature Range (°C) -55 to +50 Shelf Size (Inches) 12.4 x 14.5 x 5.75 high Number of Shelves Defrost Method Hot Gas... -
Page 53: Appendix D: Freeze Dry System Accessories
The following accessories are available for the Triad Freeze Dry System. PART # DESCRIPTION Cable 7537800 Connect the RS232 output from the Triad Freeze Dry System to an IBM compatible computer with a 9-pin serial data port. Cable 7537801 Connects the RS232 output from the Triad Freeze Dry System to an IBM compatible computer with a 25-pin serial data port. - Page 54 Appendix C: Freeze Dry System Specifications PART # DESCRIPTION Pump Inlet Filter 1472200 Disposable filter that prevents oil back streaming and protects vacuum pump from sub micron particles. Fits Vacuum Pump #7739403. Pump Exhaust Filter 1473400 Disposable filter that removes visible oil mist and odor from vacuum pump exhaust.
- Page 55 Stoppers and threaded vials with Screw Caps are supplied in packages of 200. Size Vials with Stoppers Perfect for long term storage of freeze Screw Caps dried samples. Labconco Serum 5 ml 7762300 7762200 10 ml 7762600 7762200 Bottles and Treaded Vials are specifically designed for lyophilization applications.
- Page 56 *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 (28mm). Pore size 17 micron. Shipping Labconco models and other freeze dryers. weight 0.5lb. Product Service 816-333-8811 or 1-800-522-7658...
- Page 57 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 58 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...
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