User’s Manual FreeZone® 6 Liter Benchtop Freeze Dry Systems Models 77520 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 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 1 1 2 3 4 4 6 CHAPTER 2: PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements Chamber or Manifold Requirements 7 7 8 8 8 CHAPTER 3: GETTING STARTED Unpacking Your Freeze Dryer Freeze Dryer Components Setting Up Your Freeze Dryer Vacuum Pump Connection Electrical Connection Drying Chamber or Dry
Defrosting Alarms Power Failure Line Voltage Out of Range Temperature Out of Range Service Vacuum Pump Moisture in Collector 24 25 25 26 26 26 27 CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 28 CHAPTER 6: USING THE RS232 RECEPTACLE Computer Connection for Computer Interface 30 30 CHAPTER 7: TROUBLESHOOTING Vacuum Pump Gaskets, Tubing, Connections, Sample Valves System Components & Collection Chamber Isolation Refrigeration Module Operation 35 35 36 38 41 CHAPTER 8: MODIFYING YOUR FREEZE DRYER DISPLAY Te
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 ice and the heat removed from the collector to convert the water vapor into ice. 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.
Chapter 1: Introduction sample. The volume of the freeze dry flask should be two to three times the volume of the sample. 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.
Chapter 1: Introduction pressure and ultimately overloads the collector and vacuum pump. Samples that have eutectic temperatures of –20°C or lower should be placed on the freeze dry system one flask at a time so that the vacuum in the system may recover before adding another sample to the system. If the vacuum does not recover, the capacity of the freeze dry system has been exceeded and the sample should be removed.
Chapter 1: Introduction Chapter 2: Prerequisites explains what you need to do to prepare your site before you install your Freeze Dryer. Electrical requirements are discussed. Chapter 3: Getting Started contains the information you need to properly unpack, inspect and install your Freeze Dryer. Chapter 4: Using Your Freeze Dryer discusses the basic operation of your Freeze Dryer. Information on how to attach samples and run the Freeze Dryer is included.
Chapter 1: Introduction Typographical Conventions Recognizing the following typographical conventions will help you understand and use this manual: • • • • ! ) • Book, chapter, and section titles are shown in italic type (e.g., Chapter 3: Getting Started). Steps required to perform a task are presented in a numbered format. Comments located in the margins provide suggestions, reminders, and references.
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 Location Requirements The Freeze Dryer should be located in an area that provides an unobstructed flow of air around the cabinet. This air cools the refrigeration system. The refrigeration system draws air in through the rear and exhausts it through the sides. A minimum of 3" must be allowed between the rear and both sides of the Freeze Dryer and adjacent wall surfaces. Restriction of airflow during operation could adversely affect performance.
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. ! The FreeZone 6 Liter Benchtop Freeze Dry System weighs over 135 lbs. 61 kg).
Chapter 3: Getting Started ) IF YOUR FREEZE DRYER WAS DAMAGED IN TRANSIT, YOU MUST FILE A CLAIM DIRECTLY WITH THE FREIGHT CARRIER. LABCONCO CORPORATION AND ITS DEALERS ARE NOT RESPONSIBLE FOR SHIPPING DAMAGE. ) 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.
Chapter 3: Getting Started 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. 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.
Chapter 3: Getting Started Chemical Resistance of Freeze Dryer Components The FreeZone Freeze Dry System is designed to be chemically resistant to most compounds that are commonly used in freeze drying processes. However, by necessity, the freeze dryer is comprised of a number of different materials, some of which may be attacked and degraded by certain chemicals. The degree of degradation is dependent on the concentration and exposure duration.
Chapter 3: Getting Started When using compounds in the Freeze Dryer that are hostile to the materials of construction, it is imperative the equipment is thoroughly cleaned after use. • • 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.
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. WARNING: The disposal of substances used in connection with this equipment may be governed by various Federal, State or local regulations.
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 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 9. Auto Mode Indicator – When lit, the green LED indicates that the Freeze Dryer is in Auto Mode. In this mode, the vacuum pump will start when the collector temperature reaches –40°C. 10. Vacuum Graph Display – This display indicates the relative system vacuum level. The highest LED indicates that the vacuum level is above 2.0 mBar. The indicators will sequence down when the vacuum level reaches 2.0, 1.0, 0.8, 0.6, 0.45, 0.12 mBar.
Chapter 4: Using Your Freeze Dryer 5. Inspect each sample valve on the accessory drying chamber or manifold and check for any visible damage and for improper installation that might cause a vacuum leak. Also check that each sample valve is closed or in the “vent” position. Vacuum Pump Ballast Setting Most vacuum pumps are equipped with a gas ballast mechanism. The freeze dry process requires high vacuum.
Chapter 4: Using Your Freeze Dryer • Press SELECT until the desired vacuum operating level is displayed. See “Setting the Operating Vacuum Level” for guidelines • If “O” 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. The display will show: • • TEMPERATURE UNITS °C • • • °F Press SELECT until the desired units are flashing. Press MENU.
Chapter 4: Using Your Freeze Dryer • • 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 and hold SELECT until the desired time interval is shown.
Chapter 4: Using Your Freeze Dryer Manual Start-Up To manually run the freeze dry process, press the REFRIGERATION MAN switch. This will start the refrigeration system. The green LED above the switch will illuminate. When the collector temperature reaches –40°C, the vacuum pump may be started by pressing the VACUUM switch. The Temperature and Vacuum Graphs will indicate collector temperature and system vacuum. The LCD display will show the actual temperature of the collector.
Chapter 4: Using Your Freeze Dryer Some guidelines for setting the Freeze Dryer are shown below. These show pre-freezing temperatures and vacuum levels. Exact protocols must be determined by the user for the specific samples that are being freeze dried.
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 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. First, release system vacuum by turning the plastic knob on a valve to the open position or by pulling the collector chamber drain plug out of the drain hose. Now press the Vacuum Switch on the control panel to turn the vacuum pump OFF.
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 Line Voltage Out of Range If the voltage supplied to the Freeze Dryer varies beyond allowable limits, the alarm will be activated. When an alarm occurs, press MENU and the display will show: LINE VOLTAGE ERROR The alarm will self-cancel when the proper voltage is restored. The high and low alarm points are preset at the factory to correspond to the normal allowable voltage variations based on the nominal voltage specified for the freeze dryer.
Chapter 4: Using Your Freeze Dryer Moisture in Collector If there is liquid in the collector chamber and either a REFRIGERATION button or the VACUUM button is pressed, neither function will start and an alarm will be activated. When MENU is pressed, the display will show: MOISTURE IN COLLECTOR When the collector is drained, the alarm will self-cancel. This feature prevents the inadvertent start of the vacuum pump when liquid is in the collector and thereby can extend the life of the vacuum pump.
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, non-abrasive 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 RapidVap 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.
Chapter 6: Using the RS232 Receptacle 1. 2. 3. 4. 5. Data Rate 2400 Baud 8 Bit word length 1 Start bit, 1 Stop bit No parity is transmitted Standard ASCII character set 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 following describes how to use an IBM compatible computer with Hyper Terminal™ software (included with Windows® 95, 98, XP or 2000 operating systems) to collect the RS232 data from your Freeze Dryer: 1. Make sure that the Freeze Dryer is properly connected to the communication port on the computer. 2. Open Hyper Terminal™ software. i)Windows® 95 or 98 use: START/PROGRAMS/ACCESSORIES.
Chapter 6: Using the RS232 Receptacle 5. The “Com X Properties” dialogue box will open. Enter the appropriate data properties and press “OK.
Chapter 6: Using the RS232 Receptacle 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 0.033 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 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.
Chapter 7: Troubleshooting 7. Make sure that the sample valve bulkhead nuts are tight. Either tighten by hand or use the wrench supplied with chambers. To use the wrench, first remove the knob and stem assembly and also the valve body. The pins on the wrench fit into the round holes of the nut. The nut should be snug, but avoid over-tightening. Replace the valve body, knob and stem assembly. The illustrations below show how the sample valve installs on a chamber and a manifold.
Chapter 7: Troubleshooting Manifold Assembly Knob & Stem Assembly Valve Body Valve Assembly (Manifold) Valve Body Trim Ring Knob & Stem Assembly Bulkhead Nut Thrust Washer Gasket (No grease required) Bulkhead Fitting Valve Assembly (Stainless Steel Chamber) III. System Components and Collection Chamber Isolation 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.
Chapter 7: Troubleshooting The following test allows you to check the pump and the connections from the pump to the vacuum tube. 1. Place a rubber stopper in the vacuum port in the left side of the collector chamber and another in the drain port in the bottom. 2. Restart the vacuum system and check your vacuum indication. Insufficient vacuum indicates a bad pump or a leak in the connections from the pump to the side of the chamber.
Chapter 7: Troubleshooting The following test is used to check the collection chamber integrity. The figure below points out potential areas to locate a leak: 1. Remove the stopper from the side of the chamber and place a freeze dry flask over the connection port. 2. Fill the collection chamber with approximately 2 inches of water, enough to cover all fittings. Replace the collection chamber lid and turn on the vacuum pump. Allow the vacuum pump to run for approximately 5 to 10 seconds.
Chapter 7: Troubleshooting 4. If bubbling was observed on the chamber surface, the chamber must be replaced. This type of leak cannot be successfully repaired. The leading cause of a chamber surface leak is corrosive residue left in the chamber after use.
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 Low line limit may be lowered in 5 increments of approximately 2 to 3V increments for 115V models or disabled. Low line limit may be lowered in 5 increments of approximately 4 to 5V increments for 230V models or disabled. 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.
Chapter 8: Modifying Your Freeze Dryer Display The display will default to the main freeze dry display information. If you do not want to restore all factory settings, but want to adjust offsets, press MENU briefly and the display will show: COLLECTOR TEMP OFFSET OC Press SELECT until the appropriate offset is shown. Each number represents 1°C 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.
Chapter 8: Modifying Your Freeze Dryer Display Press SELECT until the appropriate offset is shown. If the Freeze Dryer is operating on nominal 115V, each number represents 2V. If 3 is entered into the display, the high line alarm will alarm when the voltage raises to approximately 133V, for example. 127+(2x3)=133V.
Chapter 8: Modifying Your Freeze Dryer Display Press MENU and the display will show HOLD SELECT TO CLEAR ALL TOTAL HOURS? If you want to reset Total Hours, press and hold SELECT until an audible beep is heard. The display will default to the main freeze dry display information. If you do not want to set Total Hours, press MENU and the display will show.
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: Domestic 1-800-522-7658, International 816-333-8811 49
APPENDIX B FREEZE DRYER DIMENSIONS 50 Product Service Domestic 1-800-522-7658, International 816-333-8811
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 • • • • • • • 52 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. PART # 1467700 7739403 1472100 7739402 7584000 7584002 1472200 DESCRIPTION Vacuum Pump Two stage direct drive pump, 195 liters/minute. 115 VAC, 50/60 Hz, single phase, 7.8 amps. Includes Pump Exhaust Filter 1473400. (Catalog #1473400) Vacuum Pump Two stage direct drive pump, 195 liters/minute. 230 VAC, 50/60 Hz, single phase, 4.0 amps. Includes Pump Exhaust Filter 1473400.
Appendix D: Freeze Dryer Accessories PART # 1473400 1473200 1473300 1988000 7772000 7772100 7584300 7772500 7772600 7538000 7522800 7522900 7443500 7444000 7442900 54 DESCRIPTION Pump Exhaust Filter Disposable filter that removes visible oil mist and odor from vacuum pump exhaust. Fits vacuum pumps 1467700 and 7739403. Replacement Element, Oil Mist, Pump Exhaust Filter Fits pump exhaust filter 1473400.
Appendix D: Freeze Dryer Accessories PART # 7867000 7509200 7509201 7442100 7441700 7522300 7522400 7522500 7868500 7509600 7439901 7439902 7509300 7509301 7509400 DESCRIPTION Clear Drying Chamber For Bulk Drying 12.0 Dia. Product Heater For use in chamber 7522800. Provides 3 heated shelves operating at 43°C (110°F). 115V Product Heater For use in chamber 7522800. Provides 3 heated shelves operating at 43°C (110°F). 230V Drying Rack- Unheated Provides three shelves.
Appendix D: Freeze Dryer Accessories PART # 7509401 7806020 7806021 7806022 7806023 7806030 7806031 7806032 7806033 7948020 7948030 7948040 7726500 56 DESCRIPTION Product Heater with Variable Heat For use in chamber 7522900, 7444000 and 7867000 Bulk Tray Dryer 115V, 60 Hz, three shelves, 630 square inches of area, provides heat control Bulk Tray Dryer 115V, 60 Hz, three shelves, 630 square inches of area, provides heat control with 6 port manifold Bulk Tray Dryer 115V, 60 Hz, three shelves, 630
Appendix D: Freeze Dryer Accessories PART # 7537800 7537801 7761500 7390702 DESCRIPTION Cable Connect the RS232 output from the Freeze Dryer (or Freeze Dryer/Tray Dryer combination) to an IBM compatible computer with a 9-pin serial data port. Cable Connects the RS232 output from the Freeze Dryer (or Freeze Dryer/Tray Dryer combination) to an IBM compatible computer with a 25-pin serial data port.
Appendix D: Freeze Dryer Accessories Fast-Freeze® Flasks 58 Product Service: Domestic 1-800-522-7658, International 816-333-8811
Appendix D: Freeze Dryer Accessories Lyph-Lock® Flasks Product Service: Domestic 1-800-522-7658, International 816-333-8811 59
Appendix D: Freeze Dryer Accessories Serum Bottles & Vials 60 Product Service: Domestic 1-800-522-7658, International 816-333-8811
Appendix D: Freeze Dryer Accessories Ampules Product Service: Domestic 1-800-522-7658, International 816-333-8811 61
62 Product Service Domestic 1-800-522-7658, International 816-333-8811
