Labconco FreeZone 6 User Manual
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Labconco FreeZone 6 User Manual

Freeze dry systems
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User's Manual
FreeZone® 6, 12 and 18 Liter
Freeze Dry Systems
Models
7753000
7753500
7753001
7753501
7753003
7753503
7753010
7753510
7753011
7753511
7753013
7753513
Register your product online at
www.labconco.com/productreg.html
or return the attached card and
7754000
7754500
7754001
7754501
7754003
7754503
7754010
7754510
7754011
7754511
7754013
7754513
receive FREE LabbyWear
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
7755000
7755500
7755001
7755501
7755003
7755503
7755010
7755510
7755011
7755511
7755013
7755513
™
!
Labconco's Mascot,
Labby the LABster

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Summary of Contents for Labconco FreeZone 6

  • Page 1 7755513 Register your product online at www.labconco.com/productreg.html or return the attached card and receive FREE LabbyWear ™ Labconco’s Mascot, Labby the LABster 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...
  • Page 2 Product designs are subject to change without notice © 2002 Labconco Corporation Printed in U.S.A.
  • Page 3 The warranty for all Labconco products will expire one year from date of installation or two years from date of shipment from Labconco, whichever is sooner, except the following: •...

  • Page 5: 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 CHAPTER 2: PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements Chamber or Manifold Requirements Space Requirements Your Next Step CHAPTER 3: GETTING STARTED Unpacking Your Freeze Dryer...
  • Page 6 Adding Sample Alarms & Informational Messages Shut Down Defrosting Shell Freezer CHAPTER 5: MAINTAINING YOUR FREEZE DRYER CHAPTER 6: USING THE RECORDER JACK Recorder Jack Pin Configuration Computer Connection CHAPTER 7: TROUBLESHOOTING Vacuum Pump Gaskets, Tubing, Connections, Sample Valves System Components & Collection Chamber Isolation Refrigeration Module Operation APPENDIX A: FREEZE DRYER COMPONENTS APPENDIX B: FREEZE DRYER DIMENSIONS...

  • Page 7: Chapter 1: Introduction

    PTFE coated collector chamber, purge valve, and shell freezer are optional on all models. The Labconco Console Freeze Dry System is designed for laboratory lyophilization procedures. It is CFC-free so it will not endanger the environment. The unit is easy to install and maintain.

  • Page 8: Freeze Dry Rates

    Chapter 1: Introduction Freeze drying is a process whereby water is removed from frozen materials by converting the frozen water directly into its vapor without the intermediate formation of liquid water. The basis for this sublimation process involves the absorption of heat by the frozen sample in order to vaporize the ice;...
  • Page 9 Chapter 1: Introduction Up to the point of overloading the system, the greater the surface area of the sample, the faster the rate of freeze drying. By contrast, for a given surface area, the thicker the sample the slower the rate of freeze drying. This is based on the fact that the heat of sublimation is usually absorbed on one side of the frozen sample and must travel through the frozen layer to vaporize water...

  • Page 10: Freeze Dry Capacity

    Chapter 1: Introduction concentration of sodium chloride, the vapor pressure of the water would decrease as the concentration of sodium chloride increased. This is due to the fact that as the solute concentration increases, less of the surface area of the frozen sample is occupied by water. In general, most solutions or biological samples will have a eutectic temperature of –10 to –25°C.

  • Page 11: Samples Containing Volatile Substances

    Chapter 1: Introduction cascade type refrigeration so that the collector temperature can be cooled to below –75°C, or a dry ice/solvent trap can be used between the collector and the vacuum pump. Samples Containing Volatile Substances In certain cases the solvent in a sample to be freeze dried may contain volatile components such as acetic acid, formic acid or pyridine.
  • Page 12 Chapter 1: Introduction 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.

  • Page 13: Typographical Conventions

    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.
  • Page 14 Chapter 1: Introduction Refer to Chapter 7: Troubleshooting if you are experiencing problems with your Freeze Dryer. Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 15 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 16: Chapter 2: Prerequisites

    Chapter 2: Prerequisites Electrical Requirements The Freeze Dryer requires a dedicated electrical outlet. This outlet requires a 20 Amp circuit breaker or fuse for models rated at 115V (60 Hz). An outlet equipped with a 15 Amp circuit breaker or fuse is required for models rated at 230V (50/60 Hz).

  • Page 17: Chamber Or Manifold Requirements

    230V models). This will allow the vacuum pump to be plugged into the receptacle on the junction box inside the console cabinet. See Appendix D: Freeze Dryer Accessories for vacuum pumps available from Labconco. Chamber or Manifold Requirements A freeze drying chamber or manifold is not included and must be purchased separately.
  • Page 18 Chapter 2: Prerequisites Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 19 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 • unpack and move your Freeze Dryer. • set up your Freeze Dryer. •...

  • Page 20: Unpacking Your Freeze Dryer

    (15) days of delivery. DO NOT RETURN GOODS WITHOUT THE PRIOR AUTHORIZATION OF LABCONCO. UNAUTHORIZED RETURNS WILL NOT BE ACCEPTED. IF YOUR FREEZE DRYER WAS DAMAGED IN TRANSIT, YOU MUST FILE A CLAIM DIRECTLY WITH THE FREIGHT CARRIER.
  • Page 21 Plug (230V 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. Product Service: Domestic 1-800-522-7658, International 816-333-8811...

  • Page 22: Setting Up Your Freeze Dryer

    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. Component Orientation The refrigeration system in the Freeze Dryer exhausts air through the rear of the cabinet.

  • Page 23: Electrical Connection

    Chapter 3: Getting Started Electrical Connection Plug the power cord into the receptacle on the back of the Freeze Dryer and plug the other end into a suitable power receptacle. Drying Chamber or Drying Manifold Installation The drying chamber or drying manifold, purchased separately, may be positioned directly above the 3-inch port on the top of the Freeze Dryer.

  • Page 24: Your Next Step

    Chapter 3: Getting Started Use care when using aggressive liquids which can damage the Freeze Dryer and thoroughly clean the Freeze Dryer after each use. Instructions for cleaning are in Chapter 5: Maintaining Your Freeze Dryer. WARNING: The disposal of substances used in connection with this equipment may be governed by various Federal, State or local...

  • Page 25: 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...

  • Page 26: Freeze Dryer Controls

    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. Main Power Switch – Turns the unit on or off. 2. LCD Display – Displays system parameters and alarm messages.
  • Page 27 Chapter 4: Using Your Freeze Dryer 5. 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.

  • Page 28: Operation Checklist

    Chapter 4: Using Your Freeze Dryer Operation Checklist The following checklist should be followed prior to each use of your Freeze Dryer: 1. Wipe the interior of the collector chamber with a soft cloth or paper towel to remove any accumulated moisture.

  • Page 29: Purge Valve

    Chapter 4: Using Your Freeze Dryer Purge Valve The optional purge valves are installed between the Freeze Dryer collection chamber and the vacuum pump. When the green LED above the PURGE switch is illuminated, the purge valves are closed and the vacuum pump is isolated from the Freeze Dryer collection chamber.

  • Page 30: Operating The Freeze Dryer

    Chapter 4: Using Your Freeze Dryer Operating the Freeze Dryer Automatic Start-Up Turn the MAIN POWER switch ON and the LCD display will illuminate. If the unit is equipped with the optional purge valve, the green annunciator above the PURGE switch will illuminate indicating that the purge valves are closed.

  • Page 31: Manual Start-Up

    Chapter 4: Using Your Freeze Dryer Manual Start-Up Turn the MAIN POWER switch ON and the LCD display will illuminate. If the unit is equipped with the optional purge valve, the green annunciator above the PURGE switch will illuminate indicating that the purge valves are closed.

  • Page 32: Adding Sample

    Chapter 4: Using Your Freeze Dryer Adding Sample The following procedure should be followed when freeze drying: 1. Pre-freeze 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 is a freezer.
  • Page 33 Chapter 4: Using Your Freeze Dryer 3. Before adding another sample, allow system vacuum to return to 133 x 10 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.

  • Page 34: Alarms & Informational Messages

    Chapter 4: Using Your Freeze Dryer 6. 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.

  • Page 35: Shut Down

    Chapter 4: Using Your Freeze Dryer 4. Service Vacuum Pump – The vacuum pump normally plugs into the vacuum pump 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.

  • Page 36: Defrosting

    Chapter 4: Using Your Freeze Dryer Defrosting The following procedure should be followed when defrosting the collector coil: 1. Pull the collector chamber drain hose out from the front panel of the unit and remove the drain plug. Place the drain hose in a suitable container to collect the condensate that will be defrosted off the collector coil.

  • Page 37: Shell Freezer

    Chapter 4: Using Your Freeze Dryer Shell Freezer Follow the steps below each time you use the optional shell freezer to obtain optimum performance: 1. Check that the solvent bath drain plug is securely installed in the drain hose. 2. Remove bath compartment cover and add solvent to bath compartment.
  • Page 38 Chapter 4: Using Your Freeze Dryer Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 39 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.

  • Page 40: Chapter 5: Maintaining Your Freeze Dryer

    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.

  • Page 41: Chapter 6: Using The Recorder Jack

    The operation of your Freeze Dryer can be monitored using either a recorder or a computer. Read this chapter to learn how to: • connect a recorder to the Freeze Dryer. • connect a computer to the Freeze Dryer. • interpret the data received. Recorder Jack Pin Configuration The system vacuum and collector temperature can be...

  • Page 42: Computer Connection

    Either of these cables can be purchased from Labconco as an accessory. The part numbers for these cables are listed with the following schematics and are also listed in Appendix D: Freeze Dryer Accessories.
  • Page 43 Chapter 6: Modifying Your Freeze Dryer Cable configuration for 9 pin male connector (Labconco accessory cable part number 7534000) View from back of computer View from front of Labconco Freeze Dryer 1-DCD (Data Carrier Detect) 1-TXD (Transmit Data) 2-RX (Receive Data)
  • Page 44 Chapter 6: Modifying Your Freeze Dryer There are several commercially available software packages which can read RS232 data and enter the data into a computer program such as a word processor (to create a text file) or spreadsheet (to tabulate and plot the data).
  • Page 45 Chapter 6: Modifying Your Freeze Dryer 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.” 5. The “Com X Properties” dialogue box will open. Enter the appropriate data properties and press “OK.”...
  • Page 46 Chapter 6: Modifying Your Freeze Dryer 6. When the Freeze Dryer main power switch is on. the data will be transmitted and updated every ten seconds. Product Service: Domestic 1-800-522-7658, International 816-333-8811...

  • Page 47: Chapter 7: Troubleshooting

    If the suggested corrective actions do not solve your problem, contact Labconco for additional assistance. Labconco Freeze Dry Systems should reach a vacuum of 133 x 10 mBar within 10 minutes and should achieve an ultimate vacuum of 33 x 10 mBar within 18 hours.

  • Page 48: Gaskets, Tubing, Connections, Sample Valves

    Chapter 7: Troubleshooting 2. Check the oil level in the pump. Ensure it is filled to the correct level. 3. Check vacuum hose connections from the pump to the Freeze Dryer and try running the unit. If vacuum problems continue, consider obtaining a second vacuum gauge capable of reading a vacuum of 10 x 10 mBar.
  • Page 49 Chapter 7: Troubleshooting 6. When checking the sample valves, pull as much vacuum as possible. If a vacuum indication is displayed, wiggle or rotate the valves and watch the gauge for any fluctuations. Fluctuations can indicate a potential vacuum leak. If the valve seems to be in good condition, remove the valve and apply vacuum grease and reinstall the valve.

  • Page 50: System Components & Collection Chamber Isolation

    Chapter 7: Troubleshooting 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 and cover the connection port. 3. Start the freeze dryer and observe the vacuum indication.
  • Page 51 Chapter 7: Troubleshooting The next test allows you to check the pump and the connections from the pump to the vacuum tube. 1. Remove the screw from the center of the vacuum tube cover and slide the cover off. 2. Take a 3 or 4 inch piece of vacuum hose and place it over the vacuum tube.
  • Page 52 Chapter 7: Troubleshooting The next test is used to check the collection chamber integrity. The figure below points out potential areas to locate a leak. Areas for potential leaks 1. Remove the vacuum hose from the vacuum tube and place a freeze dry flask over the connection port.
  • Page 53 Chapter 7: Troubleshooting Do not fill above the collector coil Vacuum Port Bulkhead Fittings Fill the chamber with approximately 2 inches of water Vacuum Drain Sensor Hose location connection 4. If bubbling is observed around the bulkhead fittings, access the bottom of the chamber and remove the insulation.

  • Page 54: 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 55: 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. Product Service Domestic 1-800-522-7658, International 816-333-8811...
  • Page 56 Appendix A: Freeze Dryer Components Item Model Part No. Description 6 Liter 7945500 Condensing Module 115V, 60 Hz 7945501 Condensing Module 220/240V, 50 Hz 6 Liter Condensing Module 115V/ 60 Hz, PTFE-coated 6 Liter 7945502 12 Liter 7951600 Condensing Module 208/230V, 60 Hz Condensing Module 208/230V, 60 Hz, PTFE-coated 12 Liter 7951601...
  • Page 57 Appendix A: Freeze Dryer Components Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 58 Appendix A: Freeze Dryer Components Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 59 Product Service Domestic 1-800-522-7658, International 816-333-8811...

  • Page 60: Appendix B: Freeze Dryer Dimensions

    Appendix B: Freeze Dryer Dimensions Product Service: Domestic 1-800-522-7658, International 816-333-8811...

  • Page 61: Appendix C: Freeze Dryer Specifications

    This Appendix contains technical information about the Freeze Dryer including electrical specifications, environmental operating conditions and wiring diagrams. Electrical Specifications Product Nominal Nominal Catalog # Frequency Phase Description Voltage Amperage 7753000 6 Liter Freeze Dryer 115V 10.0 Amps 60 Hz 7753001 6 Liter Freeze Dryer 220/240V...

  • Page 62: Environmental 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).

  • Page 63: Wiring Diagram (115V)

    Appendix C: Freeze Dryer Specifications Wiring Diagram (115V, 60 Hz Models) Product Service: Domestic 1-800-522-7658, International 816-333-8811...

  • Page 64: Wiring Diagram (230V)

    Appendix C: Freeze Dryer Specifications Wiring Diagram (230V, 50 or 60 Hz Models) Product Service: Domestic 1-800-522-7658, International 816-333-8811...

  • Page 65: Appendix D: Freeze Dryer Accessories

    The following accessories are available for the Freeze Dryer. PART # DESCRIPTION 1467700 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. 7739401 Vacuum Pump Two stage direct drive pump, 195 liters/minute. 230 VAC, 50/60 Hz, single phase, 4.0 amps.
  • Page 66 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 7806003 Bulk Tray Dryer (220V, 50 Hz) Three shelves, 630 square inches of area, provides temperature control, with 6 port manifold 7948000 Stoppering Tray Dryer (115V, 60 Hz) Three shelves, 600 square inches of area, provides temperature control and stoppering under vacuum.
  • Page 67 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 7772500 Carbon Solvent Trap Secondary trap that prevents migration of organic solvents into vacuum pump. 7772600 Replacement Activated Carbon Media for Charcoal Solvent Trap 7538000 Secondary Vacuum Trap 9 ¾" high x 7 7/8" diameter, 304 stainless steel with ¾" vacuum connections.
  • Page 68 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 7521001 Heated Drying Chamber 10 ½" high x 9" diameter type 304 stainless steel. The 3 shelf product heaters heat to 43°C (110°F). 230V 7509200 Product Heater For use in chamber 7522800. Provides 3 heated shelves operating at 43°C (110°F).
  • Page 69 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 7522400 10 Port Manifold 10” high x 29” wide x 11 3/8” deep. Type 304 stainless steel manifold with 10 freeze dry valves and support shelf. 7522500 20 Port Manifold 10” high x 29” wide x 19 5/8” deep. Type 304 stainless steel manifold with 20 freeze dry valves and 2 support shelves.
  • Page 70 *Valves on the freeze dry systems, drying chambers and manifolds offered in this catalog fit adapters 1000 (10 packages of 100). 1" diameter (28mm). Pore size 17 microns. of both 1/2” and 3/4" sizes. Size information is provided for selecting adapters for older Labconco mod- Shipping weight 0.5 lb.
  • Page 71 7557900 145 mm x 90.2 mm *Valves on the freeze dry systems, drying chambers and manifolds offered in this catalog fit adapters of both 1/2” and 3/4" sizes. Size information is provided for selecting adapters for older Labconco 1000 ml 7551000...
  • Page 72 7762200 Accessories Perfect for long term storage of freeze dried samples. Labconco Serum Bottles and Threaded Vials are specifically designed for lyophilization applications. Their uniform thin wall construction ensures even freezing and drying. Bottles and vials are ideal containers for use in the FreeZone Seal Crimper Stoppering Tray Dryer.
  • Page 73 1/4" ID hose connectors. Shipping weight 3 lbs. (1.4 kg). Labconco Ampules are fabricated of highest quality borosili- cate glass for strength and durability. They are available in five different configurations to provide the ideal ampule for...
  • Page 74 Appendix D: Freeze Dryer Accessories Product Service: Domestic 1-800-522-7658, International 816-333-8811...

  • Page 75: Declaration Of Conformity

    Product Service Domestic 1-800-522-7658, International 816-333-8811...
  • Page 76 How did you learn about the FreeZone Freeze Dry System? ❑ Dealer Sales Rep ❑ Dealer Catalog ❑ Colleague ❑ Advertisement ❑ Labconco Sales Rep ❑ Labconco Literature ❑ Trade Show ❑ Internet/WWW ❑ Other (please specify) ________________________ What factors most influenced your decision to purchase a FreeZone Freeze Dry System?
  • Page 77 LabbyWear is the official uniform ™ of LABsters everywhere! Be a LABster! As a token of our thanks for returning your Product Registration Card, we would like to send you the LabbyWear of your choice. Please select from one of the three items listed or collect Labby Bucks and redeem for other LabbyWear merchandise.

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