User’s Manual FreeZone 4.5 Liter Freeze Dry Systems Models 77500 Series 77510 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 1 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
Shut Down Defrosting Alarms Power Failure Line Voltage Out of Range Temperature Out of Range Service Vacuum Pump Moisture in Collector 21 21 22 22 22 23 23 23 CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 24 CHAPTER 6: USING THE RS232 RECEPTACLE Computer Connection for Computer Interface 26 26 CHAPTER 7: TROUBLESHOOTING Vacuum Pump Gaskets, Tubing, Connections, Sample Valves System Components & Collection Chamber Isolation Refrigeration Module Operation 30 30 31 33 33 CHAPTER 8: MODIFYING YOUR FREEZE DRY
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 A listing of selected materials and their approximate drying times are shown in Table 1 for your reference. Table 1 SAFE TEMPERATURE AND DRYING TIMES FOR SELECTED MATERIALS Material Safe Collector Hours 10mm Thick Temperature Temperature (Approx.
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 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 A: Freeze Dryer Components contains labeled diagrams of the components of the Freeze Dryer. 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 BE 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: 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.
Chapter 3: Getting Started DO NOT DISCARD THE CARTON OR PACKING MATERIAL FOR YOUR FREEZE DRYER UNTIL YOU HAVE CHECKED ALL OF THE COMPONENTS AND INSTALLED AND TESTED THE FREEZE DRYER. Freeze Dryer Components Locate the model of Freeze Dryer you received in the following table. Verify that the components listed are present and undamaged. 7751020 7751021 7751030 7751031 7751040 7751041 7751060 7751061 7751070 7751071 4.5L Console Freeze Dryer 4.5L Console Freeze Dryer 4.5L Console Freeze Dryer 4.
Chapter 3: Getting Started Plus the following: Part # 7416600 1291000 7373450 1488800 7730700 7688500 7445100 Component Description User’s Manual Plug (230V models only) Vacuum Hose Hose Clamps (2) Chamber Lid Lid Gasket Freeze Dry Valve Wrench 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.
Chapter 3: Getting Started Vacuum Pump Connection A vacuum pump as described in Chapter 2: Prerequisites is required to operate your Freeze Dry System properly. The Freeze Dryer is equipped with a 3/4" ID, heavy wall, vacuum hose for connecting the collector chamber to the vacuum pump. ! Make certain that the oil in the vacuum pump is at the proper level. Place the vacuum pump near the benchtop Freeze Dryer models.
Chapter 3: Getting Started Chamber & Fittings Pyridine D Methyl t-Butyl Ether (BTBE) 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 C * An access
Chapter 3: Getting Started Rubber and plastic components that have been exposed to damaging compounds should be removed and flushed with water. The oil in the vacuum pump should be checked often. It must be changed if it is cloudy, shows particles or is discolored. The useful life of vacuum pump oil can be extended if the vacuum pump is operated for an extended period of time after a freeze dry run. This allows contaminants to be purged from the hot oil.
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. ! 14 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 5 2 10 7 11 9 8 12 4 6 3 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 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. If “0” is selected, the vacuum control is disabled and the vacuum level in the Freeze Dry System will be determined by the capabilities of the vacuum pump. Press MENU.
Chapter 4: Using Your Freeze Dryer VACUUM TOTAL HOUR: XXXX SERVICE HOUR: XXXX To reset the SERVICE HOUR to 0, press SELECT. The display will show: VACUUM TOTAL HOUR: XXXX RESET SERVICE HOUR: ? If you want to reset the service hours to 0, continue to hold SELECT five seconds until hours are reset. Press SELECT. The display will show the RS-232 data transmission rate. RS-232 TRANSMISSION RATE 10 SECONDS To change the rate press SELECT until the desired time interval is shown.
Chapter 4: Using Your Freeze Dryer will show the actual temperature of the collector. When the vacuum in the system is above 5 mBar the vacuum display will indicate “HI.” At 5 mBar and below, the display will show the actual vacuum. When the system vacuum is between 0.450 and 0.133 mBar, the lower green vacuum graph LED will flash. When the system vacuum level is <0.133 mBar, the green LED will be lit steadily indicating that samples may be added.
Chapter 4: Using Your Freeze Dryer containers or larger). The temperature required for pre-freezing is dependent on the characteristics of the sample. Pre-freezing temperature typically is at least 10° to 20°C below the eutectic or collapse temperature of the sample. 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.
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, the Freeze Dryer should be defrosted.
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 will flash and the beeper will sound. The beeper will automatically mute itself after one minute. The specific alarm can be identified by pressing MENU. Pressing MENU multiple times will display multiple alarms if they have occurred.
Chapter 4: Using Your Freeze Dryer Temperature Out of Range An alarm will be activated if the collector temperature rises above –40°C. If this occurs, the display will show: COLLECTOR TEMPERATURE HOLD SELECT TO CLEAR IT Press and hold SELECT for five seconds until the error message is cleared from the display. Service Vacuum Pump The vacuum pump normally plugs into the vacuum pump electrical receptacle on the back of the Freeze Dryer.
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 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 The following test is used to check the collection chamber integrity and connections. The figure below points out potential areas to locate a leak. Fill the collection chamber with approximately 2 inches of water, enough to cover all fittings. Remove one wire from the moisture sensor. Replace the collection chamber lid and turn on the vacuum pump. Allow the vacuum pump to run for approximately 5 to 10 seconds.
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 Moisture Sensor Alarm The moisture sensor alarm may be disabled. It is shipped enabled as the factory default setting. Modifying the Display To enter an offset or to configure the alarms, perform the following steps: Press and hold MENU button (approximately 10 seconds) until the display shows: PRODUCTION MENU MASTER RESET? It is recommended that you do NOT perform a Master Reset because all offsets and configurations that have been entered will be lost.
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 Item Part No.
Appendix A: Freeze Dryer Components Product Service 1-800-522-7658 41
APPENDIX B FREEZE DRYER DIMENSIONS Model 77500xx 42 Product Service 1-800-522-7658
Appendix B: Freeze Dryer Dimensions Model 77510xx Product Service 1-800-522-7658 43
APPENDIX C FREEZE DRYER SPECIFICATIONS This Appendix contains technical information about the Freeze Dryer including electrical specifications and environmental operating 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). Main supply voltage fluctuations not to exceed ±10% of the nominal voltage. Transient over voltages according to Installation Categories II (Over voltage Categories per IEC 1010).
APPENDIX D FREEZE DRYER ACCESSORIES The following accessories are available for the Freeze Dryer. 46 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 PART # 1472200 DESCRIPTION Pump Inlet Filter Disposable filter that prevents oil back streaming and protects vacuum pump from sub micron 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 # 7522800 DESCRIPTION 12 Port Drying Chamber 9 ¾" high x 7 7/8" diameter, 304 stainless steel with 12 freeze dry valves. Requires 7762800 attachment port lid. 7522900 16 Port Drying Chamber 13" high x 138" diameter, 304 stainless steel with 16 freeze dry valves. Requires 7762800 attachment port lid. 7443500 Clear Drying Chamber with 8 Valves For bulk drying or drying in flasks. Requires 7762800 attachment port lid.
Appendix D: Freeze Dryer Accessories Fast-Freeze® Flasks Product Service 1-800-522-7658 49
Appendix D: Freeze Dryer Accessories Lyph-Lock® Flasks 50 Product Service 1-800-522-7658
Appendix D: Freeze Dryer Accessories Serum Bottles & Vials Product Service 1-800-522-7658 51
Appendix D: Freeze Dryer Accessories Ampules 52 Product Service 1-800-522-7658
