User’s Manual FreeZone® 1 Liter Benchtop Freeze Dry Systems Models 77400 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 Your Next Step 1 1 2 3 4 4 6 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 Dryi
CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 24 CHAPTER 6: TROUBLESHOOTING Vacuum Pump Gaskets, Tubing, Connections, Sample Valves System Components & Collection Chamber Isolation Refrigeration Module Operation 26 26 27 29 31 CHAPTER 7: MODIFYING YOUR FREEZE DRYER DISPLAY Temperature and Vacuum Display Modifying the Display 32 32 32 APPENDIX A: FREEZE DRYER COMPONENTS 34 APPENDIX B: FREEZE DRYER DIMENSIONS 37 APPENDIX C: FREEZE DRYER SPECIFICATIONS Electrical Specifications Environmental Conditions 3
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 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. Since the vapor pressure at the collector is lower than that of the sample, the flow of water vapor is from the sample to the collector.
Chapter 1: Introduction 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. If there is a problem with a particular type of sample melting when placed on the freeze dry system, dilution of the sample with more water or providing some insulation around the flask to decrease the rate of heat absorption by the sample may help.
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 through the rear panel and exhausts it through the sides. A minimum of 3" must be allowed between the back 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 1 Liter Freeze Dry System weighs over 82 lbs. (37 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 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 Drying Chamber or Drying Manifold Installation The drying chamber or drying manifold, purchased separately, may be positioned directly above the 3-inch hole in the collector chamber lid. When vacuum is applied to the system, the chamber will be held securely in place. 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.
Chapter 3: Getting Started • • Most common compounds used in freeze drying processes, if allowed to enter the vacuum pump, will degrade the oil and cause damage to the vacuum pump. Sugars and proteins typically will have minimal negative effect on any of the materials of construction. When using compounds in the Freeze Dryer that are hostile to the materials of construction, it is imperative that the equipment is thoroughly cleaned after use.
Chapter 3: Getting Started When using flammable or hazardous solvents, the vacuum pump must be vented to or operated inside a fume hood. 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.
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 4 3 1. LCD Display – Displays system operating parameters and set-up parameters. 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 4. Remove the accessory drying chamber or manifold from the connection port and using a soft, lint-free cloth or paper towel, wipe the port gasket and sealing surfaces of the drying chamber/manifold to remove any dirt and contaminants that could cause a vacuum leak. Reinstall the drying chamber or manifold on the port. Vacuum grease is not required on the port gasket to obtain a proper vacuum seal. 5. Check that each sample valve is closed or in the “vent” position.
Chapter 4: Using Your Freeze Dryer VACUUM UNITS mBar • • • Pa Torr Press SELECT until the desired units are flashing. Press MENU. The display will show: COLLECT TEMP UNITS °C • • • °F Press SELECT until the desired units are flashing. Press MENU. The display will show: REFRIG TOTAL HOUR: XXXX SERVICE HOUR: XXXX • • 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.
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. Automatic Start-Up Turn the MAIN POWER switch ON.
Chapter 4: Using Your Freeze Dryer Manual Start-Up Turn the MAIN POWER switch ON. The refrigeration system will start and the LCD display will illuminate and read: If the Freeze Dryer was configured in the set up steps above to run MANUAL, the vacuum pump must be started manually by pressing the vacuum switch. MANU VAC HI mBar WAIT COLLECTOR: XXX When the collector temperature reaches –40°C the display will read: MANU VAC HI mBar READY COLLECTOR: -40°C Press the vacuum switch.
Chapter 4: Using Your Freeze Dryer Pre-Freezing Samples Appropriate containers for freeze drying include ampules, serum bottles, and wide mouth freeze drying flasks. Shell freezing of samples is recommended for wide mouth freeze drying flasks. Smaller samples in ampules and serum bottles may be frozen in a freezer. The sample container size should always be at least two to three times the sample size (i.e., 40 ml samples should be prepared in 80 ml containers or larger).
Chapter 4: Using Your Freeze Dryer 3. 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. 4. When all the frost has disappeared from the outer surface of the sample container and no cold spots can be detected by handling the container, the sample is nearly dry.
Chapter 4: Using Your Freeze Dryer 4. If rapid defrost is desired, pour warm water over the collector coil. Do not allow the liquid to enter the vacuum port on the upper rear of the chamber. 5. Reinstall the drain hose plug and slide drain hose back into the side of the cabinet. Dispose of the liquid appropriately. ! Utilization of acid requires immediate cleaning and neutralization after defrost or physical damage to the collector chamber and collector coil will result.
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 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 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 6: 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 6: Troubleshooting and stopper the hole with a rubber stopper. Continue checking the other valves. 7. Make sure that the sample valve bulkhead nuts are tight. ither 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.
Chapter 6: 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 6: 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. 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. If the leak is in the chamber, check the drain hose, hose connections and the drain plug.
Chapter 6: Troubleshooting Refrigeration Module Operation Under a no-load condition, the FreeZone Freeze Dry System can achieve a collector temperature of –50°C or lower when the vacuum pump is operating, depending on ambient temperature and humidity. If the collector temperature does not reach –50°C within 30 minutes, then the refrigeration module is not functioning properly. If any repairs are required on the refrigeration module, contact your local laboratory supply dealer.
CHAPTER 7 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. Adjustments may be necessary if the Freeze Dryer requires service. Temperature and Vacuum Display An offset may be added to the collector temperature or vacuum display. Use an accurate traceable reference to compare the readings.
Chapter 7: Modifying Your Freeze Dryer Display Vacuum pump total hours to 0 Refrigeration to operate in Manual Mode Temperature and Vacuum Offsets If you do not want to restore all factory settings but want to adjust offsets, press MENU and hold for approximately 10 seconds. The display will show TEMPERATURE OFFSET: 0 VACUUM OFFSET: 0 Press SELECT until the appropriate temperature offset is shown. Each number represents 1°C. Press VACUUM until the appropriate vacuum offset is shown.
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 1 2 3 4 9 10 8 7 5 11 6 36 Product Service: Domestic 1-800-522-7658, International 816-333-8811
APPENDIX B FREEZE DRYER DIMENSIONS Product Service Domestic 1-800-522-7658, International 816-333-8811 37
APPENDIX C FREEZE DRYER SPECIFICATIONS This Appendix contains technical information about the Freeze Dryer including electrical specifications and environmental operating conditions.
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 40 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 # 7772600 DESCRIPTION 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 9-3/4" high x 7-7/8" diameter, and 304 stainless steel with 3/4" vacuum connections. For use with dry ice & solvent. Cools to approximately –75°C 7522800 12 Port Drying Chamber 9 ¾" high x 7 7/8" diameter, 304 stainless steel with 12 freeze dry valves.
Appendix D: Freeze Dryer Accessories 42 PART # 7509600 DESCRIPTION Sample Valve Kit Includes neoprene valve body, knob and installation parts. 7522900 16 Port Chamber 13" high x 138" diameter, 304 stainless steel with 16 freeze dry valves.
Appendix D: Freeze Dryer Accessories Product Service: Domestic 1-800-522-7658, International 816-333-8811 43
Appendix D: Freeze Dryer Accessories 44 Product Service: Domestic 1-800-522-7658, International 816-333-8811
Appendix D: Freeze Dryer Accessories Product Service: Domestic 1-800-522-7658, International 816-333-8811 45
Appendix D: Freeze Dryer Accessories Ampules 46 Product Service: Domestic 1-800-522-7658, International 816-333-8811
Product Service Domestic 1-800-522-7658, International 816-333-8811 47
