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LABCONCO CORPORATION
8811 Prospect Avenue
Kansas City, MO 64132
(800) 821-5525, (816) 333-8811
(816) 363-0130 fax
labconco@labconco.com
User's Manual
FreeZone
Freeze Dryers
Models
70020**** 2.5L -50°C Series
71020**** 2.5L -84°C Series
70040**** 4.5L -50°C Series
71040**** 4.5L -84°C Series
72040**** 4.5L -105°C Series
70080****
8L -50°C Series
Benchtop
®
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Summary of Contents for Labconco FreeZone 70020 Series
- Page 1 LABCONCO CORPORATION 8811 Prospect Avenue Kansas City, MO 64132 (800) 821-5525, (816) 333-8811 (816) 363-0130 fax labconco@labconco.com User's Manual FreeZone Benchtop ® Freeze Dryers Models 70020**** 2.5L -50°C Series 71020**** 2.5L -84°C Series 70040**** 4.5L -50°C Series 71040**** 4.5L -84°C Series 72040**** 4.5L -105°C Series...
- Page 2 Warranty Labconco Corporation provides a warranty to the original buyer for the repair or replacement of parts and reasonable labor as a result of normal and proper use of the equipment with compatible chemicals. Broken glassware and maintenance items, such as filters, gaskets, light bulbs, finishes and lubrication are not warranted.
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Page 3: Table Of Contents
Original instructions ABLE ONTENTS CHAPTER 1: INTRODUCTION Intended Use Freeze Dry Process Freeze Dry Rates Freeze Dry Capacity Samples Containing Volatile Substances About This Manual Typographical Conventions CHAPTER 2: PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements Chamber or Manifold Requirements CHAPTER 3: GETTING STARTED Unpacking Your Freeze Dryer Freeze Dryer Components... - Page 4 Original instructions Operation Buttons (Auto, Collector, Vacuum) Programs screen Data Logging screen Settings screen Language Time & Date Units Security Alerts Configure Email Settings Maintenance Vacuum Pump Settings Refrigeration System Settings Freeze Dryer Line Voltage Offset Calibration Display Network Sensors screen Drying Accessory screen End Point Detection screen Help screen...
- Page 5 Original instructions Gaskets, Tubing, Connections, Sample Valves System Components & Collector Chamber Isolation Refrigeration Module Operation APPENDIX A: FREEZE DRYER COMPONENTS APPENDIX B: FREEZE DRYER DIMENSIONS APPENDIX C: FREEZE DRYER SPECIFICATIONS Electrical Specifications Environmental Conditions APPENDIX D: FREEZE DRYER ACCESSORIES...
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Page 6: Chapter 1: Introduction
The unit is easy to install and maintain. Proper care and maintenance of this product will result in many years of dependable service. Intended Use The Labconco Freeze Dryers described in this manual are intended for laboratory use to facilitate the lyophilization process. Freeze Dry Process Freeze drying is an important process in sample preparation and for the preservation and storage of biologicals, pharmaceuticals and foods. -
Page 7: Freeze Dry Rates
Original instructions 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. -
Page 8: Freeze Dry Capacity
Original instructions 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. -
Page 9: Samples Containing Volatile Substances
Original instructions 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. -
Page 10: Typographical Conventions
Appendix B: Freeze Dryer Dimensions contains diagrams showing the dimensions for the Freeze Dryer. Appendix C: Freeze Dryer Specifications contains product specifications. Appendix D: Freeze Dryer Accessories see www.labconco.com for a complete list of Freeze Dry accessories. Typographical Conventions Recognizing the following typographical conventions will help you understand and use this manual: ... -
Page 11: Chapter 2 Prerequisites
Original instructions HAPTER REREQUISITES 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. -
Page 12: Location Requirements
Vacuum pumps used with 115V models should be equipped with a 115V, 15 Amp NEMA 5-15P plug. Vacuum pumps used with 230V models should be equipped with a reverse IEC plug (included with 230V pumps purchased from Labconco). This will allow the vacuum pump to be plugged into the receptacle on the back panel of the freeze dryer. -
Page 13: Chapter 3: Getting Started
Commission rules require that claims be DO NOT RETURN GOODS WITHOUT THE PRIOR filed with the AUTHORIZATION OF LABCONCO. UNAUTHORIZED delivery carrier RETURNS WILL NOT BE ACCEPTED. within fifteen (15) days of delivery. Product Service 816-333-8811 or 1-800-522-7658... -
Page 14: Freeze Dryer Components
-84C & -105C Models Only 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. -
Page 15: Component Identification
Original instructions Chapter 3: Getting Started Component Identification On/Standby Button Collector Chamber & LED Indicator & Coil USB Port Touch Screen Display Quick-Connect drain coupling Quick-Connect drain fitting Vacuum Connection Ethernet Port Drying Accessory Serial Tag (& Electrical Rating) End Point Detection Vacuum Pump Outlet Power Inlet... -
Page 16: Vacuum Pump Connection
Original instructions Chapter 3: Getting Started Vacuum Pump Connection A vacuum pump (as described in Chapter 2: Prerequisites) is required to operate your Freeze Dryer properly. The Freeze Dryer is equipped with a 3/4" ID 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. -
Page 17: Electrical Connection
Original instructions Chapter 3: Getting Started 7. VERIFY THE VACUUM PUMP VOLTAGE SETTING AGREES WITH THE FREEZE DRYER VOLTAGE SHOWN ON THE SERIAL NUMBER LABEL. Reconfigure if necessary (see vacuum pump instructions). 8. Connect the vacuum pump power cord to the receptacle labeled “vacuum pump”... -
Page 18: Drying Chamber Or Manifold Installation
Original instructions Chapter 3: Getting Started Arrow pointing forward Drying Chamber or Drying Manifold Installation A drying chamber or drying manifold (purchased separately) may be positioned directly above the 3-inch hole in the collector chamber lid. 12 or 16 Port Drying Chamber Installation on Acrylic & Stainless Steel Lids DRYING CHAMBER LATCH SPACER(SSTL) -
Page 19: Chemical Resistance Of Freeze Dryer Components
Original instructions Chapter 3: Getting Started 4 or 8 Port Manifold Installation on Acrylic or Stainless Steel Lids MANIFOLD ACRYLIC LID GASKET ASSEMBLY SPACER(PLASTIC) GASKET STAINLESS STEEL GASKET LIP LID ASSEMBLY FACING DOWN SPACER(SSTL) LATCH GASKET LIP FACING DOWN Clear Drying chambers come with their own bottom adapter plate that will be used in place of the collector chamber lid supplied with the Freeze Dryer. - Page 20 Original instructions Chapter 3: Getting Started major components of the FreeZone Freeze Dry System that are susceptible to degradation are as follows: Acids Buffers Solvents Component Material Valve Stem Acetal Collector Acrylic Hoses, Neoprene Gaskets & Valve Bodies Flask Top Silicon Rubber Chamber &...
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Page 21: Solvent Safety Precautions
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 Dryer, 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 Dryer may be flammable or hazardous to your health. -
Page 22: Chapter 4: Lyo-Works ™ Operating System
Original instructions HAPTER ORKS™ PERATING YSTEM After your Freeze Dryer has been installed as detailed in Chapter 3: Getting Started, read this chapter to learn how to: Operate the controls. Understand the display. Do not use the Freeze Dryer in a manner not specified by the manufacturer (refer to Appendix C: Freeze Dryer Specifications). -
Page 23: Control Panel
Original instructions Chapter 4: Lyo-Works Operating System Control Panel The control panel for the Freeze Dryer is shown below with a description of its functions. 1. Touch Screen Display – Capacitive touch screen displays system operating parameters, set-up parameters and alarm messages. All user interface will take place via the touch screen. -
Page 24: Touch Screen Operation
Original instructions Chapter 4: Lyo-Works Operating System Touch Screen Operation Home Screen After initial power up, the Home screen will be displayed. Most of the general operation and system monitoring can be done from the Home screen. Menu Indicator Bar Line 1 Line 2 Operation... -
Page 25: System Parameters Display
Original instructions Chapter 4: Lyo-Works Operating System System Parameters Display Line 1 COLLECTOR & VACUUM HEADING – Describes the measurement that is displayed directly below the text. Line 2 COLLECTOR MEASUREMENT - Displays the temperature of the collector coil in °C or °F (as selected in Settings). The value displayed will be if the temperature is: >... -
Page 26: Operation Buttons (Auto, Collector, Vacuum)
Original instructions Chapter 4: Lyo-Works Operating System Operation Buttons Operation buttons are displayed across the bottom of the Home screen. AUTO – Use this button to initiate an auto start up sequence. When auto start is initiated the refrigeration system (collector) will be started immediately, and the vacuum pump will start when the collector temperature has cooled down to -40°... - Page 27 Original instructions Chapter 4: Lyo-Works Operating System Start/Stop – Use this button to start or stop a program. The wording on this button will change from “Start” to “Stop” depending on whether or not a program is currently running. A DRYING ACCESSORY MUST BE ATTACHED TO THE FREEZE ...
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Page 28: Data Logging Screen
Original instructions Chapter 4: Lyo-Works Operating System Pressing the program name field will allow you to edit the program name. The Step numbers are listed in numerical order. Shelf Temp., Time, and Vacuum can be edited by pressing any of these cells. The “Add” button will add a new Step to the program. -
Page 29: Settings Screen
Original instructions Chapter 4: Lyo-Works Operating System If no data log file has been selected the “New” button will be the only active button along the bottom of the screen. A data log file can be selected from the list by pressing the data log file name. -
Page 30: Time & Date
Original instructions Chapter 4: Lyo-Works Operating System 2. Time/Date – Chose Clock Format (12 or 24 hour), Set Time, Set Date for manually setting the time and date. The Auto Update time & date feature can be used if a valid network connection has been established. With Auto Update the following settings need to be entered: ... -
Page 31: Alerts
Original instructions Chapter 4: Lyo-Works Operating System System – If the System security feature is selected (box checked), users will be required to enter the security code to gain access to the touch screen controls when the screen is reactivated from a screen timeout (sleep mode) or power failure (screen timeout described in the Settings/Display section). -
Page 32: Configure Email Settings
Edit – Use this button to edit an existing email address. Delete – Use this button to delete an existing email address. Device Name – The default name for this field will be “Labconco Freeze Dryer”. The name can be edited by pressing the name field. -
Page 33: Maintenance
Original instructions Chapter 4: Lyo-Works Operating System If all the SMTP fields entered are valid, but the network connection is not working (or Ethernet cable is not connected) the following message will appear after pressing the Save button: EMAIL SETTINGS ERROR – Network connection is not active ... -
Page 34: Refrigeration System Settings
Original instructions Chapter 4: Lyo-Works Operating System 7. Calibration – Some sensors in the Freeze Dryer can be calibrated. This process should be done by a qualified technician or metrologist with reference sensors that are known with certainty. An external reference sensor must be placed at the same measurement point (as close as physically possible) as the sensor being calibrated. -
Page 35: Display
Original instructions Chapter 4: Lyo-Works Operating System Current Reading (uncorrected) – This gives the raw sensor reading with no offset applied to the reading. Offset – This is the value that will be added to the Current Reading (uncorrected) to give the proper adjusted reading that matches the reference sensor being used for calibration. -
Page 36: Network
Original instructions Chapter 4: Lyo-Works Operating System Brightness Slider – Moving the slider to the right will increase the brightness level, moving to the left will decrease the brightness level of the display. Touch Sounds – With Touch Sounds turned ON, there will be an audible sound each time the display is touched. -
Page 37: Sensors Screen
Original instructions Chapter 4: Lyo-Works Operating System Sensors Screen This screen contains a list of all sensors currently installed on the Freeze Dryer and any attached accessory. The screen can be scrolled up and down if the list is too long to be viewed on a single page. -
Page 38: End Point Detection Screen
Original instructions Chapter 4: Lyo-Works Operating System Drying Accessory Sensor Table – The middle section of the screen displays a list of all the sensors that are available for the connected Drying Accessory. Sensors that are disconnected will have three dashes (---) for their value. Drying Accessory Status Box –... -
Page 39: Help Screen
Original instructions Chapter 4: Lyo-Works Operating System End Point Detection status – Shows the current status for each flask. The status will be one of the following: ON, OFF or COMPLETE. Touching the end point detection cell for any given flask will allow you to turn the end point detection ON/OFF. -
Page 40: Diagnostics
Original instructions Chapter 4: Lyo-Works Operating System Diagnostics – This screen will give information about the power supply to the Freeze Dryer (Voltage, Current & Frequency) and allow the user to run Manual or Auto Diagnostics on the unit. ... -
Page 41: Chapter 5: Using Your Freeze Dryer
Original instructions HAPTER SING REEZE RYER Operation Checklist The following checklist should be followed prior to each use of your Freeze Dryer: 1. Remove the accessory drying chamber or manifold from the collector chamber lid and using a soft, lint-free cloth or paper towel, wipe the port gasket(s) and sealing surfaces of the drying chamber/manifold and collector chamber lid to remove any dirt or contaminants that could cause a vacuum leak. -
Page 42: Vacuum Pump Ballast Setting
Original instructions Chapter 5: Using Your Freeze Dryer 11. Attach a pre-frozen sample to sample valve on drying chamber or manifold. Note: If using a Clear Chamber, Tray Dryer or Heated Product Shelves, the vacuum chamber must be fully vented (to atmospheric pressure) in order to remove acrylic chamber or open door before loading sample into the drying chamber. -
Page 43: Pre-Freezing Samples
Original instructions Chapter 5: Using Your Freeze Dryer Vapor pressure above ice Temp. Pressure Temp. Pressure Temp. Pressure Temp. Pressure Temp. Pressure (°C) (mbar) (°C) (mbar) (°C) (mbar) (°C) (mbar) (°C) (mbar) 6.11 2.37 0.94 0.34 0.039 5.63 2.17 0.85 0.31 0.011 5.18... -
Page 44: Adding Sample
Original instructions Chapter 5: Using Your Freeze Dryer freezing temperature is typically 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 chambers or manifolds with sample valves in the freeze dry process: 1. -
Page 45: Starting A Program
Original instructions Chapter 5: 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. Starting a Program (for optional drying accessories) If one of the electronically controlled accessory drying chambers, suitable for your... -
Page 46: Alerts
Original instructions Chapter 5: Using Your Freeze Dryer 6. Disconnect the quick connect drain fitting from the quick connect drain coupling. DISCONNECT THE QUICK CONNECT DRAIN FITTING BEFORE STARTING THE VACUUM PUMP. FAILURE TO REMOVE THE FITTING WILL RESULT IN A LARGE VACUUM LEAK. - Page 47 Original instructions Chapter 5: Using Your Freeze Dryer operated outside the normal voltage limits (see Appendix C). If necessary, the high and low LINE VOLTAGE OFFSETS may be adjusted from the Settings / Maintenance screen. Collector Temp After the collector temperature has cooled to below -40°C, an alert will be activated if the collector temperature rises above –40°C for more than 5 minutes.
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Page 48: Copy (Export) A Data Log File
Original instructions Chapter 5: Using Your Freeze Dryer End Point Detection (optional accessory) An alert will be activated when the primary drying phase end point has been detected for any of the active flask sensors connected to the End-Zone end point detection accessory. -
Page 49: Copy A Program
Original instructions Chapter 5: Using Your Freeze Dryer 3. Write down the “IP Address” shown on the Settings>Network screen of the Freeze Dryer (this number will be used in Step 5) 4. Open an internet browser of your choice from a computer that is connected to your LAN. -
Page 50: Chapter 6: Maintaining Your Freeze Dryer
Original instructions HAPTER AINTAINING REEZE RYER Service Safety Precautions Always ensure that only authorized technicians service the refrigeration, vacuum and electrical systems. If performing any electrical maintenance, always disconnect the power at the main disconnect. If the refrigeration system must be operated with access panels removed (for diagnostic purposes only), stay clear of moving fan blade. - Page 51 Original instructions Chapter 5: Using Your Freeze Dryer 6. Check the collector chamber for condensed or frozen solvents and dispose of appropriately. Completely empty the collector chamber before the next run or before attempting to start the vacuum pump. 7. If sample valves leak or stems become difficult to turn, pull the stem out of the rubber valve body and apply a thin coat of vacuum grease to the stem.
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Page 52: Chapter 7: Troubleshooting
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. -
Page 53: Gaskets, Tubing, Connections, Sample Valves
Original instructions 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. - Page 54 Original instructions Chapter 7: Troubleshooting The illustrations below show how the sample valve installs on a chamber and a manifold. Knob & Stem Assembly Valve Body Valve Assembly (Clear Chamber with Valves) Bulkhead Nut Valve Body Manifold Assembly Thrust Washer Valve Body Thrust Washer Gasket...
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Page 55: System Components & Collector Chamber Isolation
Original instructions Chapter 7: Troubleshooting System Components and Collector Chamber Isolation This test determines if the source of a leak is in the drying chamber or manifold. 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. - Page 56 Original instructions Chapter 7: Troubleshooting The following test determines if a vacuum leak is in the collector 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 collector chamber.
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Page 57: Refrigeration Module Operation
If any repairs are required on the refrigeration module, contact your local laboratory supply dealer. If your laboratory supply dealer is unable to provide assistance, please call Labconco. Repairs should only be undertaken by a competent refrigeration technician or through an authorized Labconco service agency. -
Page 58: Appendix A: Freeze Dryer Components
Original instructions PPENDIX REEZE RYER OMPONENTS 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. Product Service 816-333-8811 or 1-800-522-7658... - Page 59 Original instructions Appendix A: Freeze Dryer Components 2.5L -50C Models (70020xxxx) 2.5L -84C Models (71020xxxx) Item -50C -84C Part No. Description 7395800 Lid Gasket 7395801 Lid (Acrylic) 7207500 Lid Assembly, Stainless Steel (includes lid gasket 7395800) 7953802 Motor Fan, 115V 7953803 Motor Fan, 230V 7591805...
- Page 60 Original instructions Appendix A: Freeze Dryer Components 2.5L -50C Models (70020xxxx) 2.5L -84C Models (71020xxxx) *2.5L -50C Model Shown Product Service 816-333-8811 or 1-800-522-7658...
- Page 61 Original instructions Appendix A: Freeze Dryer Components 4.5L -50C Models (70040xxxx) 4.5L -84C Models (71040xxxx) 4.5L -105C Models (72040xxxx) Item -50C -84C -105C Part No. Description 7690800 Lid Gasket 7329600 Lid (Acrylic) 7207400 Lid Assembly, Stainless Steel (includes lid gasket 7690800) 7953802 Motor, Fan, 9 Watt, 115V...
- Page 62 Original instructions Appendix A: Freeze Dryer Components 4.5L -50C Models (70040xxxx) 4.5L -84C Models (71040xxxx) 4.5L -105C Models (72040xxxx) *4.5L -84C Model Shown Product Service 816-333-8811 or 1-800-522-7658...
- Page 63 Original instructions Appendix A: Freeze Dryer Components 8L -50C Models (70080xxxx) Item -50C Part No. Description 7690800 Lid Gasket 7329600 Lid (Acrylic) 7953802 Motor, Fan, 9 Watt, 115V 7953803 Motor, Fan, 9 Watt, 230V 7750607 Compressor, 115V, 60Hz 7750606 Compressor, 230V, 50Hz 7750605 Compressor, 230V, 60Hz 7316600...
- Page 64 Original instructions Appendix A: Freeze Dryer Components 8L -50C Models (70080xxxx) Product Service 816-333-8811 or 1-800-522-7658...
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Page 65: Appendix B Freeze Dryer Dimensions
Original instructions PPENDIX REEZE RYER IMENSIONS 2.5L -50C Models (70020****) Product Service 1-800-522-7658... - Page 66 Original instructions Appendix B: Freeze Dryer Dimensions 2.5L -84C Models (71020****) 4.5L -50C Models (70040****) *Dimensions in inches & (centimeters) Product Service 816-333-8811 or 1-800-522-7658...
- Page 67 Original instructions Appendix B: Freeze Dryer Dimensions 4.5L -84C Models (71040****) 4.5L -105C Models (72040****) 8L -50C Models (70080****) *Dimensions in inches & (centimeters) Product Service 816-333-8811 or 1-800-522-7658...
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Page 68: Appendix C: Freeze Dryer Specifications
Original instructions PPENDIX REEZE RYER PECIFICATIONS This Appendix contains technical information about the Freeze Dryer including electrical specifications and operating conditions. Electrical Specifications Voltage Frequency Amps Operating Max. with Catalog # Description Nominal (Hz) Range Vacuum Pump 115V 103-127 70020xxxx 2.5L -50C 230V 187-253... -
Page 69: Environmental Conditions
Appendix C: Freeze Dryer Specifications Environmental Conditions Indoor use only. 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). ... -
Page 70: Appendix D Freeze Dryer Accessories
Original instructions PPENDIX REEZE RYER CCESSORIES Labconco offers a full line of accessories to enhance your Freeze Dryer’s operation and usability. For a complete list of these accessories, please consult our website at www.labconco.com. Product Service 816-333-8811 or 1-800-522-7658...
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