User’s Manual 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 Please read the User’s Manual before operating the equipment.
Copyright © 2005, 2007, 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. Warranty Labconco provides a warranty on all parts and factory workmanship.
TABLE OF CONTENTS CHAPTER 1: INTRODUCTION Freeze Dry Process Freeze Dry Rates Freeze Dry Capacity Samples Containing Volatile Substances 1 1 2 3 3 CHAPTER 2: PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements 5 5 5 6 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 Chemical Resistance of Freeze Dryer Compon
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 Shelf Temperature Set Point Power Failure Platen Tilt 23 23 24 24 24 25 25 26 27 28 28 28 28 28 28 28 29 CHAPTER 5: MAINTAINING YOUR FREEZE DRY SYSTEM 30
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.
Chapter 1: Introduction Freeze Dry Rates The efficiency of the freeze drying process is dependent upon the surface area and the thickness of the sample, the collector temperature and vacuum obtained, the eutectic point and solute concentration of the sample. It is important to remember these factors when trying to obtain efficient utilization of your freeze dry system. A listing of selected materials and their approximate drying times are shown in Table 1 for your reference.
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.
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. Hence, samples that contain volatile substances will have a greater tendency to melt, particularly when placed in flasks or exposed to room temperature.
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. Location requirements. Vacuum pump requirements. Refer to Appendix C: Freeze Dry System Specifications for complete electrical and environmental conditions, specifications and requirements.
Chapter 2: Prerequisites Vacuum Pump Requirements The user must provide a vacuum pump. A vacuum pump with a displacement of 144 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 with the FreeZone Triad Freeze Dry System. It is recommended that the vacuum pump is equipped with an exhaust filter to minimize oil mist exhausting from the vacuum pump.
Chapter 3: Getting Started Now that the site for your Triad Freeze Dry System is properly prepared, you are ready to unpack, inspect, install and test your freeze dry system. Read this chapter to learn how to: Unpack and move your freeze dry system. Set up your freeze dry system. Safely use solvents with your freeze dry system. Unpacking Your Triad Freeze Dry System Carefully unpack your freeze dry system and inspect it for damage that may have occurred in transit.
Chapter 3: Getting Started Triad Freeze Dry System Components 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. 7400030 7400040 7400060 7400070 Plus the following: Part # 7373300 7373436 1488800 1291000 Qty.
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.
Chapter 3: Getting Started Some of the major components of the freeze dry system that are susceptible to degradation are as follows: C D D D D D C C D D D C D D D D C D Dioxane Sodium Phosphate Calcium Chloride D Pyridine D Methyl t-Butyl Ether (BTBE) D D Carbon Tetrochloride Cyclohexane C D D Acetonittirle Silicon Rubber Stainless Steel D Solvents Acetone Neoprene C Buffers Trifluoroacetic Acid (TFA) Material Acetal Acrylic Formic Acid Component Valve Stem Door Hoses,
Chapter 3: Getting Started With prudent maintenance the 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 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.
Chapter 4: Operating Instructions 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). The electrical protection may be impaired if used inappropriately.
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. Display Button: Changes format of display from “monitor” to “auto” to “manual” to “set up” screen. 3. Display Indicators: Green INDICATOR shows which display “screen” is shown. 4.
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. 14. Stoppering: Controls the stoppering platen up and down movement. The mechanism will function only while the chamber is under vacuum.
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. To configure your Triad Freeze Dry System, turn the main Power Switch ON. Press the DISPLAY button until the SET UP indicator is lit.
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. The display will show: REFRIGERATION TOTAL HOURS: XXXX: RESET SERVICE HOUR: ? X Press ENTER. The display will show: VACUUM TOTAL HOURS: XXXX: SERVICE HOUR: XXXX Press ENTER if you do not want to reset SERVICE HOURS.
Chapter 4: Operating Instructions The display will show: VACUUM UNITS: MBar Pa 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. Normally, the sublimation rate will increase if there is less vacuum (a higher pressure) in the Triad Freeze Dry System.
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. There is no shelf temperature control in this mode.
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. Above 5.0 mBar the display will show “HIGH” vacuum.
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. Figure 3 Programming The Triad Freeze Dry System will store up to five programs numbered 1 through 5.
Chapter 4: Operating Instructions The display will show the parameters that were last entered for this program. P1 SEG 1 HOLD –34°C RAMP 00.0°C/MN 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. The flashing parameter name shows the parameter that will be changed.
Chapter 4: Operating Instructions During the hold cycle of the active segment the display will alternate as follows: P1 SHLF SAMP P1 SHLF = -55 COL = -85 SAMP= -55°C SEG = 1H VAC = .030M COL SEG TR P1 SHLF = -55 COL = -85 SAMP= -55°C TR = 4.6 VAC = .030M VAC M P T Selected Program Shelf Temperature Sample Temperature (if probe is not installed, the display shows ---) Collector Temperature Shows what segment is active and holding (H) Shows time remaining segment. If time is 10.
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 “- - -”. The temperatures and vacuum are displayed in the units selected in Set Up. Above 5.0 mBar the display will show “hi” vacuum.
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. With the display set in manual, select “Set Point Temperature” = PreFreeze. 2. Set mode to MAN. 3. Place unfrozen samples on the shelf and close the door. The sample probe can be placed in the sample. 4.
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. Stoppering Vials The stoppering operation (when desired) is performed after the freeze dry process is complete and before breaking vacuum.
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. Once the collector temperature is less than –80°C and vacuum is less than 0.133 mBar, connect a pre-frozen sample to a sample valve on the left side of the cabinet using an adapter.
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. The sample container may now be removed. In the vent position the bevel on the valve knob should point away from the sample port. 6.
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.
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.
Chapter 5: Maintaining Your Freeze Dry System Under normal operation, the freeze dry system requires little maintenance. However, the following maintenance schedule is recommended: As needed: 1. The user has the responsibility for carrying out appropriate decontamination if hazardous material is spilled on or inside the equipment. This may be done by wiping the contaminated surfaces with a soft cloth dampened with alcohol. Alcohol may craze the acrylic door.
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. 2. Using a soft cloth, sponge or chamois and a mild, non-abrasive soap or detergent, clean the acrylic door. 3.
Chapter 6: Using the RS232 Receptacle The operation of the Triad Freeze Dry System can be monitored using a computer connected to the RS232 receptacle located on the rear panel of the freeze dryer. The computer cannot control the operation of the freeze dry system. Computer Connection for Computer Interface Check your computer to see which type of serial port is provided. Use one of the two connecting cables listed below: 1.
Chapter 6: Using the RS232 Receptacle Press or until the desired time interval is shown. Press ENTER.
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. Press “OK.” 5. The “Com X Properties” dialogue box will open. Enter the appropriate data properties and press “OK.” 6.
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 and should achieve an ultimate vacuum of 0.040 mBar within 18 hours when the refrigeration is operating.
Chapter 7: Troubleshooting If vacuum problems continue, consider obtaining a second vacuum gauge capable of reading a vacuum of 0.010 mBar. It is often useful in determining if the vacuum pump is operating properly and the vacuum sensor reading is accurate. 4. Isolate the pump by disconnecting the vacuum hose from the freeze dry system. 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.
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. With the unit Power Switch OFF, press the button and turn the Power Switch ON. The display will show: DIAGNOSTIC MODE Press .
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. The Lexsol pump turns on or press . The display will show: DEFROST The defrost valve opens or press . The display will show: VACUUM PUMP The refrigeration system turns off.
Chapter 7: Troubleshooting Refrigeration Module Operation In the Pre-freeze mode under a no-load condition and an ambient temperature of 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.
Chapter 7: Troubleshooting (1) Disconnect power cord from supply outlet. (2) Make sure the Power Switch is in the OFF position. (3) Remove the rear cover to expose the marked back foam insulation. Cut through the foam along the marked lines and remove center cutout. (4) Remove the insulation and both caps from the fluid circulation valve. (5) Attach a flexible tube to the exposed port (service port). The port is 3/8" x 45° male flare.
Chapter 7: Troubleshooting Heat Transfer Fluid Precautions The fluid’s name and manufacturer are: Name: Manufacturer: Lexol 542 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. Handling and Storage Precautions – Dirty Solvent: Store in accordance with all applicable regulations.
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. Use an accurate traceable reference to compare the readings. Vacuum offset may be varied ±0.010 mBar in 0.
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. OFFSET: 0°C Press or until the appropriate offset is shown. Each number represents an offset of 1°C.
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.
Appendix A: Freeze Dry System Components Figure 7 Product Service 816-333-8811 or 1-800-522-7658 45
Appendix B: Freeze Dry System Dimensions Figure 8 Serum Bottle Capacity of the Triad Freeze Dry System Size 2 ml 3 ml 5 ml 10 ml 20 ml 30 ml 50 ml 100 ml 125 ml 46 Labconco No (100 pcs.).
Appendix C: Freeze Dry System Specifications This Appendix contains technical information about the freeze dry system’s electrical specifications and environmental operating conditions.
Appendix C: Freeze Dry System Specifications Performance Specifications Collector Minimum Temperature (°C) -85 Collector Capacity in 24 Hours (Liters) 1.84 Collector Total Capacity (Liters) 2.5 Shelf Minimum Temperature (°C) -75 Shelf Control Temperature Range (°C) -55 to +50 Shelf Size (Inches) 12.4 x 14.5 x 5.75 high Number of Shelves 1 Defrost Method Hot Gas Time to Defrost 2.0L (Hr) 1.
Appendix D: Freeze Dry System Accessories The following accessories are available for the Triad Freeze Dry System. PART # 7537800 7537801 7756100 7756200 7516200 7739403 7739402 7584002 DESCRIPTION Cable Connect the RS232 output from the Triad Freeze Dry System to an IBM compatible computer with a 9-pin serial data port. Cable Connects the RS232 output from the Triad Freeze Dry System to an IBM compatible computer with a 25-pin serial data port. Tray with Slide-Out Bottom 14" wide x 12" deep.
Appendix C: Freeze Dry System Specifications PART # 1472200 1473400 1473200 1473300 1988000 7584300 7772000 7772100 7772500 DESCRIPTION Pump Inlet Filter Disposable filter that prevents oil back streaming and protects vacuum pump from sub micron particles. Fits Vacuum Pump #7739403. Pump Exhaust Filter Disposable filter that removes visible oil mist and odor from vacuum pump exhaust. Fits Vacuum Pump #7739403. Replacement Element, Oil Mist, Pump Exhaust Filter Fits Pump Exhaust Filter #1473400.
Appendix A: Freeze Dry System Components Serum Bottles and Vials Threaded Vials Stoppers and threaded vials with Screw Caps are supplied in packages of 200. Perfect for long term storage of freeze dried samples. Labconco Serum Bottles and Treaded Vials are specifically designed for lyophilization applications. Their uniform thin wall construction ensures even freezing and drying. Bottles and vials are ideal containers for use in the FreeZone Stoppering Tray Dryer.
Appendix C: Freeze Dry System Specifications Fast-Freeze Flasks Fast-Freeze Flasks are specially designed to be easier to handle, faster to load and more convenient to use than other freeze dry glassware now in your laboratory. Compatible with all major brands of laboratory freeze dry equipment, Fast-Freeze Flasks eliminate the risk of contamination from vacuum grease, reduce spillage of valuable samples and require no washers, gaskets or retainers.
Appendix A: Freeze Dry System Components Lyph-Lock Flasks Lyph-Lock Flasks simplify your Lyophilization procedures because they have only three pieces per flask – a high strength borosilicate glass top and bottom with a silicone rubber ring seal. The unique wide-mouth design helps you load samples easily and lyophilize efficiently. How to select Lyph-Lock Flasks for your Freeze Dry System Select Lyph-Lock Flasks fast- based on your sample sizes.
Appendix C: Freeze Dry System Specifications Ampules Oxygen/Natural Gas Sealing Torch 7578500 Torch specifically designed for flame sealing freeze dry ampules. Seals all types of heat-resistant glass. Connects to natural gas, butane or propane and oxygen with ¼" ID hose connectors. Shipping weight 3 lbs. (1.4 kg). Labconco Ampules are fabricated of highest quality borosilicate glass for strength and durability.
