Labconco FreeZone 7750000 User Manual
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Labconco FreeZone 7750000 User Manual

Benchtop and console freeze dry systems
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User's Manual
FreeZone® Benchtop and Console
Freeze Dry Systems
Models
7750000
7750001
7750003
7750004
Register your product online at
www.labconco.com/productreg.html
or return the attached card and
7751000
7751001
7751003
7751004
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
™
!
Labconco's Mascot,
Labby the LABster

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  • Page 1 7751004 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 4: 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 Space Requirements Your Next Step CHAPTER 3: GETTING STARTED Unpacking Your Freeze Dryer Freeze Dryer Components Setting Up Your Freeze Dryer...
  • Page 5 Adding Sample Alarms & Informational Messages Shut Down Defrosting 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 6: Chapter 1: Introduction

    Congratulations on your purchase of a Labconco Freeze Dry System. Benchtop and console models are available for operation on 115V or 230V. The Labconco FreeZone® 4.5 Liter Freeze Dry System is designed for laboratory lyophilization procedures. It is CFC-free so it will not endanger the environment.

  • Page 7: Freeze Dry Rates

    Chapter 1: Introduction 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; the use of a vacuum pump to enhance the removal of water vapor from the surface of the sample;...
  • Page 8 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 ice at...

  • Page 9: 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 10: 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 11 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 12: 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 13 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 14 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 15: 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 10 Amp circuit breaker or fuse is required for models rated at 230V (50/60 Hz).

  • Page 16: Space Requirements

    Freeze Dryer. See Appendix D: Freeze Dryer Accessories for vacuum pumps available from Labconco. Space Requirements Refer to Appendix C: Freeze Dryer Specifications for dimensional drawings of the Freeze Dryer.
  • Page 17 Chapter 2: Prerequisites Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 18 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 19: 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 20: Setting Up Your Freeze Dryer

    Plug, 230V, IEC 320 (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. Setting Up Your Freeze...

  • Page 21: Vacuum Pump Connection

    Chapter 3: Getting Started Vacuum Pump Connection A vacuum pump with a rated capacity of 113 liters per minute is required to operate your Freeze Dry System properly. The unit is provided with a 3/4" ID, heavy wall, vacuum hose for connecting the vacuum pump to the collector chamber on the unit.
  • Page 22 Chapter 3: Getting Started When using flammable or hazardous solvents, the vacuum pump should 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.

  • Page 23: Your Next Step

    Chapter 3: Getting Started Your Next Step The installation and setup of your Freeze Dryer is now complete. To learn how to load and operate your Freeze Dryer, proceed to Chapter 4: Using Your Freeze Dryer. To perform additional diagnostics on your Freeze Dryer, proceed to Chapter 7: Troubleshooting.

  • Page 24: 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 25: 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 26 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 27: 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 28: Operating The Freeze Dryer

    Chapter 4: Using Your Freeze Dryer Operating the Freeze Dryer Automatic Start-Up To run the Auto Mode press the panel switch labeled REFRIGERATION AUTO. The green annunciator above the switch will illuminate. This will start the refrigeration system. When the collector reaches –40°C the vacuum pump will start.

  • Page 29: 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 in a freezer.
  • Page 30 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 31: 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 32: 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 33: 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 melt off the collector coil.
  • Page 34 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 35: 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 36: 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 37: 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 38 Chapter 6: Using the Recorder Jack 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 39 Chapter 6: Using the Recorder Jack 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 40 Chapter 6: Using the Recorder Jack 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 41 Chapter 6: Using the Recorder Jack 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 42: 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 43: Gaskets, Tubing, Connections, Sample Valves

    Chapter 7: Troubleshooting Drain the oil and refill with clean oil. Repeat as necessary. 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...
  • Page 44 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 45: System Components & Collection Chamber Isolation

    Chapter 7: Troubleshooting III. System Components and Collection Chamber Isolation 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.
  • Page 46 Chapter 7: Troubleshooting The next test is used to check the collection chamber integrity and connections. 1. Fill the collection chamber with approximately 2 inches of water, enough to cover all fittings in the bottom of the collection chamber. Replace the collection chamber lid and turn on the vacuum pump.

  • Page 47: Refrigeration Module Operation

    If any repairs are required on the refrigeration module, contact you 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 48: 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 49 Appendix A: Freeze Dryer Components 77500 SERIES FREEZONE 4.5 LITER BENCHTOP Item Quantity Part No. Description 7525300 Condensing Module 115V, 60 Hz Condensing Module 115V, 60 Hz, PTFE-coated 7525301 7525302 Condensing Module 220/240V, 50 Hz 7525303 Condensing Module 208/230V, 60 Hz 7730700 7688500 Lid Gasket...
  • Page 50 Appendix A: Freeze Dryer Components Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 51 Appendix A: Freeze Dryer Components 77510 SERIES FREEZONE 4.5 LITER CONSOLE Item Quantity Part No. Description 7525300 Condensing Module 115V, 60 Hz Condensing Module 115V, 60 Hz, PTFE-coated 7525301 7525302 Condensing Module 220/240V, 50 Hz 7525303 Condensing Module 208/230V, 60 Hz 7730700 7688500 Lid Gasket...
  • Page 52 Appendix A: Freeze Dryer Components Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 53 Appendix A: Freeze Dryer Components Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 54 77500 SERIES FREEZONE 4.5 LITER BENCHTOP " " " Product Service Domestic 1-800-522-7658, International 816-333-8811...

  • Page 55: Appendix B: Freeze Dryer Dimensions

    Appendix B: Freeze Dryer Dimensions 77510 SERIES FREEZONE 4.5 LITER CONSOLE " " " Product Service: Domestic 1-800-522-7658, International 816-333-8811...

  • Page 56: Appendix C: Freeze Dryer Specifications

    This Appendix contains technical information about the Freeze Dryer including specifications, environmental operating conditions and wiring diagrams. Electrical Specifications • Nominal Voltage: Models 7750000, 7750003, 7751000, 7751003 – 115 Volt Models 7750001, 7751001 – 220/240 Volt Models 7750004, 7751004 – 208/230 Volt •...

  • Page 57: 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 58: 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 59: 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 60: 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. 7739403 Vacuum Pump Two stage direct drive pump, 195 liters/minute. 230 VAC, 50/60 Hz, single phase, 4.0 amps with reverse IEC plug.
  • Page 61 Disposable filter that prevents oil back streaming and protects vacuum pump from submicron particles. 1473400 Pump Exhaust Filter Disposable filter that removes visible oil mist and odor from vacuum pump exhaust. Included with Labconco direct drive rotary vane pumps. 1473200 Replacement Element, Oil Mist, Pump Exhaust Filter 1473300...
  • Page 62 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 7538200 Secondary Vacuum Trap 9 ¾" high x 7 7/8" diameter, 304 stainless steel with ½" vacuum connections. For use with dry ice and solvent. 7538400 Secondary Vacuum Trap 7 7/8" high x 6 5/8" diameter, 304 stainless steel with ½" vacuum connections.
  • Page 63 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 7509201* Product Heater For use in chamber 7522800. Provides 3 heated shelves operating at 43°C (110°F). 230V 7509300* Product Heater For use in chamber 7522900. Provides 3 heated shelves operating at 43°C (110°F). 115V 7509301* Product Heater For use in chamber 7522900.
  • Page 64 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 7750200 Wire Shelf Racks, Pair Racks easily attach without tools to the sides of the 4.5 Liter cabinet to provide additional support for glassware attached to the collection chamber. 7509600 Sample Valve Kit Includes Neoprene valve body, knob and installation parts.
  • Page 65 *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 66 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 67 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 Stoppering Tray Dryer.
  • Page 68 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 your specific lyophilization requirements, from tray drying to flame sealing applications.
  • Page 69 Appendix D: Freeze Dryer Accessories Product Service: Domestic 1-800-522-7658, International 816-333-8811...

  • Page 70: Declaration Of Conformity

    Product Service Domestic 1-800-522-7658, International 816-333-8811...
  • Page 71 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 72 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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