User’s Manual FreeZone 2.5 Liter Freeze Dry Systems Models 74200 Series 76700 Series 76705 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 © 2004, 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 About This Manual Typographical Conventions Your Next Step 1 1 2 3 4 4 5 5 CHAPTER 2: PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements Chamber or Manifold Requirements 6 6 6 7 7 CHAPTER 3: GETTING STARTED Unpacking Your Freeze Dryer Freeze Dryer Components Setting Up Your Freeze Dryer Component Orientation Vacuum Pump Connection Elec
Pre-Freezing Samples Adding Sample Shut Down Defrosting Alarms Power Failure Line Voltage Out of Range Temperature Out of Range Service Vacuum Pump Moisture in Collector 21 21 22 23 23 23 24 24 25 25 CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 26 CHAPTER 6: USING THE RS232 RECEPTACLE Computer Connection for Computer Interface 28 28 CHAPTER 7: TROUBLESHOOTING Vacuum Pump Gaskets, Tubing, Connections, Sample Valves System Components & Collection Chamber Isolation Refrigeration Module Operation 32 32 33 35
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.
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 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.
Chapter 1: Introduction 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.
Chapter 1: Introduction Appendix B: Freeze Dryer Dimensions contains comprehensive diagrams showing the dimensions for the Freeze Dryer. Appendix C: Freeze Dryer Specifications contains product specifications. Appendix D: Freeze Dryer Accessories lists the part numbers and descriptions of all of the accessories available for your Freeze Dryer.
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: the electrical supply requirements. the vacuum pump requirements.
Chapter 2: Prerequisites IT IS RECOMMENDED THAT THE CONSOLE MODEL FREEZE DRYER IS SECURELY ATTACHED TO THE FLOOR AFTER IT IS LOCATED WHERE IT WILL BE USED. THIS WILL PREVENT ACCIDENTAL TIPPING AND POSSIBLE INJURY. SEE INSTRUCTIONS IN CHAPTER 3 GETTING STARTED. 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.
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: ! 8 unpack and move your Freeze Dryer. set up your Freeze Dryer. connect the electrical supply source to your Freeze Dryer. properly exhaust your Freeze Dryer. safely use solvents with your Freeze Dryer. The FreeZone 2.5 Liter Benchtop Freeze Dryer System weighs over 82 lbs. (37 kg).
Chapter 3: Getting Started Unpacking Your Freeze Dryer The United States Interstate Commerce Commission rules require that claims be filed with the delivery carrier within fifteen (15) days of delivery. Carefully unpack your Freeze Dryer and inspect it for damage that may have occurred in transit. If your Freeze Dryer is damaged, notify the delivery carrier immediately and retain the entire shipment intact for inspection by the carrier. DO NOT RETURN GOODS WITHOUT THE PRIOR AUTHORIZATION OF LABCONCO.
Chapter 3: Getting Started 7670020 7670021 7670030 7670031 7670040 7670041 7670060 7670061 7670070 2.5L Benchtop Cascade Freeze Dryer 2.5L Benchtop Cascade Freeze Dryer 2.5L Benchtop Cascade Freeze Dryer 2.5L Benchtop Cascade Freeze Dryer 2.5L Benchtop Cascade Freeze Dryer 2.5L Benchtop Cascade Freeze Dryer 2.5L Benchtop Cascade Freeze Dryer 2.5L Benchtop Cascade Freeze Dryer 2.5L Benchtop Cascade Freeze Dryer 115 115 230 230 230 230 230 230 230 60 60 50 50 60 60 50 50 50 7670071 2.
Chapter 3: Getting Started If you did not receive one or more of the components listed for your Freeze Dryer, or if any of the components are damaged, contact Labconco Corporation immediately for further instructions. Setting Up Your Freeze Dryer After you verify receipt of the proper components, move your Freeze Dryer to the location where you want to install it. Then, follow the steps listed below.
Chapter 3: Getting Started TO MAXIMIZE THE STABILITY OF THE CONSOLE FREEZE DRYER, POSITION THE VACUUM PUMP AS CLOSE TO THE CENTER OF THE CABINET FLOOR AS POSSIBLE. 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.
Chapter 3: Getting Started Chamber & Fittings Methyl t-Butyl Ether (BTBE) Pyridine D Dioxane C Cyclohexane D Carbon Tetrochloride Silicon Rubber Stainless Steel D Acetonittirle C D Solvents Acetone Neoprene D D Sodium Phosphate D Calcium Chloride C Buffers Trifluoroacetic Acid (TFA) Material Acetal Acrylic Formic Acid Component Valve Stem Collector Lid Hoses, Gaskets & Valve Bodies Flask Top Acetic Acid 20% Acids D D D D C C D D D C D D D D C D D C C – Moderate
Chapter 3: Getting Started 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.
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).
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 2 5 10 7 1 11 9 8 6 4 3 12 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.
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. When the collector temperature is –40°C or lower the green indicator will light. 12. Alarm Indicator – This red LED indicates that a system alarm has occurred.
Chapter 4: Using Your Freeze Dryer To configure your Freeze Dryer, turn the main power switch ON and press MENU. The display will show: VACUUM UNITS mBar Pa Torr Press SELECT until the desired units are flashing. Press MENU. The display will show: VACUUM SET POINT XXXX YYY 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.
Chapter 4: Using Your Freeze Dryer 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 will show the refrigeration system hours. REFRIG TOTAL HOUR: XXXX RESET SERVICE HOUR: ? 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 will show the vacuum pump hours.
Chapter 4: Using Your Freeze Dryer Baffle The cylindrical plastic component shipped with Cascade Freeze Dryers (Models 76700XX and 74200X) is a baffle, which is designed to evenly distribute collected ice over the entire collector coil. Proper positioning of the baffle is required to achieve maximum ice loading capabilities. The baffle installs into the collection chamber with the flat flange upward. The large boss on the flange should be positioned toward the rear of the chamber.
Chapter 4: Using Your Freeze Dryer 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 prefreezing temperatures and vacuum levels.
Chapter 4: Using Your Freeze Dryer Bevel in “vent” position Vent/Backfill Port Bevel in “vacuum” position Adapter 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.
Chapter 4: Using Your Freeze Dryer 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 left 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.
Chapter 4: Using Your Freeze Dryer 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 will flash and the alarm beeper will sound. When the MENU button is pressed the display will show: POWER FAIL HOLD SELECT TO CLEAR IT Press and hold SELECT for five seconds until the error message is cleared from the display.
Chapter 4: Using Your Freeze Dryer 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: CHANGE VACUUM OIL HOLD SELECT TO CLEAR IT Press and hold SELECT for five seconds until the error message is cleared from the display. This will reset the 1000 hour timer.
CHAPTER 5 MAINTAINING YOUR FREEZE DRYER 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, nonabrasive soap or detergent. 3. Check oil level of the vacuum pump. It should be between MIN and MAX. If the oil level is less than an inch (25.4 mm) above MIN, add oil to proper level. 4.
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. 2. Using a soft cloth, sponge or chamois and a mild, non-abrasive soap or detergent, clean the acrylic chamber lid. 3.
CHAPTER 6 USING THE RS232 RECEPTACLE 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.
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 10 SECONDS Press select until the desired time interval is shown.
Chapter 6: Using the RS232 Receptacle The first time Hyper Terminal™ is opened a dialogue box requesting an area code and phone number will appear. Enter the appropriate numbers and continue. 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.
Chapter 6: Using the RS232 Receptacle 5. The “Com X Properties” dialogue box will open. Enter the appropriate data properties and press “OK.” 6. When the Freeze Dryer main power switch is on, the data will be transmitted and updated at the time intervals selected by the user.
CHAPTER 7 TROUBLESHOOTING Refer to the following if your Freeze Dryer fails to operate properly. If the suggested corrective actions do not solve your problem, contact Labconco for additional assistance. Labconco Freeze Dry Systems that are clean, dry and without samples attached should reach a vacuum of 0.133 mBar within 10 minutes and should achieve an ultimate vacuum of 0.040 mBar within 18 hours when the refrigeration is operating.
Chapter 7: Troubleshooting 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.
Chapter 7: Troubleshooting The illustrations below show how the sample valve installs on a chamber and a manifold.
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. 3. Start the Freeze Dryer and observe the vacuum indication.
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. 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.
Chapter 7: Troubleshooting Refrigeration Module Operation Under a no-load condition, the FreeZone Single Stage Freeze Dry System can achieve a collector temperature of -50°C or lower within 30 minutes when the vacuum pump is operating, depending on ambient temperature and humidity. FreeZone Cascade Freeze Dry Systems should achieve a collector temperature of -84°C or lower when the vacuum pump is operating.
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.
Chapter 8: Modifying Your Freeze Dryer Display High line limit may be raised in 5 increments of approximately 2 to 3V increments for 115V models or disabled. 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.
Chapter 8: Modifying Your Freeze Dryer Display Press MENU and if the drying chamber has been installed, the display will show: SDC TEMP. OFFSET: OC Press SELECT until the appropriate offset is shown. Each number represents 1°C. Press MENU and the display will show: VACUUM OFFSET: O uBar Press SELECT until the appropriate offset is shown. Each number represents 0.001mBar. Press MENU and the display will show: LOW LINE OFFSET: 0 Press SELECT until the appropriate offset is shown.
Chapter 8: Modifying Your Freeze Dryer Display Press MENU and the display will show: PURGE VALVE: NOT INSTALLED Press and hold SELECT to change the status. Press MENU and the display will show: DEFROST HEATER: NOT INSTALLED Press and hold SELECT to change the status. Press MENU and the display will show: MOISTURE SENSOR: INSTALLED Press and hold SELECT if you want to disable the moisture sensor.
Chapter 8: Modifying Your Freeze Dryer Display In order to store offsets in memory, you Must Press and Hold MENU until display shows: PASSWORD: Wait approximately 10 seconds and the display will default to the main freeze dry display information. This can be done anytime throughout the Modifying the Display routine.
APPENDIX A FREEZE DRYER COMPONENTS The following pages list components that are available for your Freeze Dryer. The parts shown are the most common replacement parts. If other parts are required, contact Product Service.
Appendix A: Freeze Dryer Components Model 76705xx Item Part No.
Appendix A: Freeze Dryer Components Model 76705xx 1 2 17 14 3 18 9-10 8 4 5 7 11 Product Service 816-333-8811 or 1-800-522-7658 6 45
Appendix A: Freeze Dryer Components Models 76700xx and 74200xx Item 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 46 Part No.
Appendix A: Freeze Dryer Components Models 76700xx and 74200xx 1 2 17 14 5 3 18 4 9-10 8 5 7 6 Product Service 816-333-8811 or 1-800-522-7658 47
APPENDIX B FREEZE DRYER DIMENSIONS Model 76705xx 48 Product Service 1-800-522-7658
Appendix B: Freeze Dryer Dimensions Model 76700xx Product Service 816-333-8811 or 1-800-522-7658 49
Appendix B: Freeze Dryer Dimensions Model 74200xx 50 Product Service 816-333-8811 or 1-800-522-7658
APPENDIX C FREEZE DRYER SPECIFICATIONS This Appendix contains technical information about the Freeze Dryer including electrical specifications and operating conditions.
Appendix C: Freeze Dryer Specifications Catalog # 7420020 7420021 7420030 7420031 7420040 7420041 7420060 7420061 7420070 7420071 Voltage Nominal Operating Range 115V 100V 115V 100V 230V 230V 230V 230V 230V 230V 230V 230V 103-127 90-110 103-127 90-110 198-254 198-254 187-253 187-253 198-254 198-254 198-254 198-254 Frequency Phase 60 50 60 50 50 50 60 60 50 50 50 50 1 1 1 1 1 1 1 1 1 1 1 1 Amperage Nominal Max. with w/o Vacuum Vacuum Pump Pump 10.0 16 10.0 16 10.0 16 10.0 16 5.1 10 5.1 10 5.1 10 5.
APPENDIX D FREEZE DRYER ACCESSORIES The following accessories are available for the Freeze Dryer. PART # 1472100 DESCRIPTION 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.
Appendix D: Freeze Dryer Accessories 54 PART # 1472200 DESCRIPTION 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.
Appendix D: Freeze Dryer Accessories PART # 7772500 DESCRIPTION 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. 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.
Appendix D: Freeze Dryer Accessories 56 PART # 7868500 DESCRIPTION 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. 7419300 Baffle Mounts in the collector chamber to increase ice holding capacity when operating with the vacuum control.
Appendix D: Freeze Dryer Accessories Product Service 816-333-8811 or 1-800-522-7658 57
Appendix D: Freeze Dryer Accessories 58 Product Service 816-333-8811 or 1-800-522-7658
Appendix D: Freeze Dryer Accessories Product Service 816-333-8811 or 1-800-522-7658 59
Appendix D: Freeze Dryer Accessories Ampules 60 Product Service 816-333-8811 or 1-800-522-7658
