Labconco FreeZone Plus Manual
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Labconco FreeZone Plus Manual

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Summary of Contents for Labconco FreeZone Plus

  • Page 1: 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 2 Adding Sample Alarms & Informational Messages Shut Down Defrosting CHAPTER 5: MAINTAINING YOUR FREEZE DRYER CHAPTER 6: MODIFYING YOUR FREEZE DRYER Recorder Jack Computer Connection CHAPTER 7: TROUBLESHOOTING Vacuum Leak Detection Refrigeration Module Operation APPENDIX A: FREEZE DRYER COMPONENTS APPENDIX B: FREEZE DRYER DIMENSIONS APPENDIX C: FREEZE DRYER SPECIFICATIONS Wiring Diagram (115V) Wiring Diagram (230V)

  • Page 3: Chapter 1: Introduction

    Congratulations on your purchase of a Labconco Freeze Dry System. Models are available for operation on 115V or 230V. The Labconco FreeZone® Plus 2.5 Liter Freeze Dry System is designed for laboratory lyophilization procedures. It is CFC free so it will not endanger the environment.

  • Page 4: 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 water;...
  • Page 5 Chapter 1: Introduction Up to the point of overloading the system, the greater the surface area of the sample, the greater 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 6: 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 7: 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 8 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 9: 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 10 Chapter 1: Introduction For information on making modifications to the configuration of your Freeze Dryer go to Chapter 6: Modifying Your Freeze Dryer. 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 11 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: 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). A 10 Amp circuit breaker or fuse is required for models rated at 230V (50 Hz).

  • Page 13: Chamber Or Manifold Requirements

    Freeze Dryer. See Appendix D: Freeze Dryer Accessories for vacuum pumps available from Labconco. Chamber or Manifold Requirements A freeze drying chamber or manifold must be purchased separately.
  • Page 14 Chapter 2: Prerequisites Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 15 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 16: Chapter 3: Getting Started

    (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 17: Setting Up Your Freeze Dryer

    19676-00 Clamp (2) If you do 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 18: 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. Plug the power cord from the vacuum pump into the receptacle on the back of the Freeze Dryer.

  • Page 19: Your Next Step

    Chapter 3: Getting Started spilled. If a sample is spilled in the collector chamber it must immediately be cleaned up. Several components of the Freeze Dryer, which are located inside the chamber, are made of stainless steel which can be attacked by acids. Use of acids can result in degradation of the product and the vacuum pump.
  • Page 20 Chapter 3: Getting Started Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 21 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 22: Chapter 4: Using Your Freeze Dryer

    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 (Not Shown) – Turns the unit on or off. This switch is located on the right side of the unit near the front.

  • Page 23: Operation Checklist

    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 24: Operating The Freeze Dryer

    Chapter 4: Using Your Freeze Dryer 1. Wipe the interior of the collector chamber with a soft cloth or paper towel to remove any accumulated moisture. 2. Check the collector chamber drain hose to insure that the hose is free of moisture and that the drain plug is securely installed.

  • Page 25: Manual Start-Up

    Chapter 4: Using Your Freeze Dryer indicate “HI.” At 2000 x 10 mBar and below, the display will show the actual vacuum. When the system vacuum is between 450 and 133 x 10 mBar, the lower green vacuum graph LED will flash.
  • Page 26 Chapter 4: Using Your Freeze Dryer Note location of taper on knob in vacuum position. 3. Before adding another sample, allow system vacuum to return to 133 x 10-3 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 27: Alarms & Informational Messages

    Chapter 4: Using Your Freeze Dryer Note location of taper on knob in vent position. 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 28: Shut Down

    Chapter 4: Using Your Freeze Dryer other alarms if they have occurred. The alarm indicator can be cancelled by turning the REFRIGERATION off. 2. Power Line Voltage Out of Range – If the voltage to the freeze dryer drops or raises beyond a safe level, the alarm indicator will FLASH.

  • Page 29: Defrosting

    Chapter 4: Using Your Freeze Dryer collected frozen solvent will obstruct the flow of vapor to the collector chamber. At this point the unit should be defrosted. First, release system vacuum by turning the plastic knob on a valve to the “vacuum”/open position or by pulling the collector chamber drain hose plug.
  • Page 30 Chapter 4: Using Your Freeze Dryer Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 31 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 32: 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 33: Chapter 6: Modifying Your Freeze Dryer

    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 The system vacuum and collector temperature can be recorded during operation by connecting an appropriate...

  • Page 34: Computer Connection

    Pin 8 – Blank Computer Connection Connection diagrams for RS232 interface from Labconco equipment to a computer that supports either a 25 pin D-sub male connector or 9 pin D-sub male connector for serial communication. See Appendix D: Freeze Dryer Accessories for available connection cables.
  • Page 35 Chapter 6: Modifying Your Freeze Dryer Computer with a 9 pin male serial connector View from back of computer View from front of Labconco Freeze Dryer 1-DCD (Data Carrier Detect) 2-RX (Receive Data) 1-TXD (Transmit Data) 4-DTR (Data Terminal Ready)
  • Page 36 Chapter 6: Modifying Your Freeze Dryer Description COLLCTR=-86 – indicates the temperature of the collector in degrees Celsius. VAC=0018 – indicates the vacuum level of the collection system is mBAR x 10 RFG=ON – indicates the state of the refrigeration compressor.
  • Page 37 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. PROBLEM CAUSE CORRECTIVE ACTION Unit will not operate Unit not connected to Connect unit to proper electrical power...

  • Page 38: Chapter 7: Troubleshooting

    Chapter 7: Troubleshooting PROBLEM CAUSE CORRECTIVE ACTION Poor vacuum (greater Leaks in vacuum lines or Locate and repair than 500 x 10 mBar) connections (cont.) Foreign material on lid Clean gasket and lid gasket Damaged sample valve Locate and replace Vacuum Leak Detection The Freeze Dryer should achieve a vacuum of 133 x mBar within 10 minutes and should achieve an...

  • Page 39: Refrigeration Module Operation

    Labconco service agency. Refrigeration Module Operation Under a no-load condition, the FreeZone Plus 2.5 Liter Freeze Dryer can achieve a collector temperature of –84°C or lower, depending on ambient temperature and humidity. If the collector temperature does not reach –84°C within 40 minutes, then the refrigeration module...
  • Page 40 If any repairs are required on the refrigeration module, contact you local laboratory supply dealer. If satisfaction is not obtained through the dealer service network, please call Labconco. Repairs should only be undertaken by a competent refrigeration technician or through an authorized Labconco service agency.
  • Page 41 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 42: Appendix A: Freeze Dryer Components

    Appendix A: Freeze Dryer Components Item Quantity Part No. Description 7475600 Condensing Unit (115V) 7475601 Condensing Unit (230V) 1488200 Hose Clamp 7477300 Drain Tube 1643600 O-Ring 772800 Drain Plug 1967600 Hose Clamp 7474200 6 Min. Delay Timer (115V) 7474400 6 Min. Delay Timer (230V) 7646000 Vacuum Hose 1336400...
  • Page 43 Appendix A: Freeze Dryer Components Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 44 Appendix A: Freeze Dryer Components Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 45 Product Service Domestic 1-800-522-7658, International 816-333-8811...

  • Page 46: Appendix B: Freeze Dryer Dimensions

    Appendix B: Freeze Dryer Dimensions Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 47 This Appendix contains technical information about the Freeze Dryer including specifications, environmental operating conditions and wiring diagrams. Electrical Specifications • Nominal amperage for 115V Freeze Dry (model 76700-00) (excluding vacuum pump): 10.5A • Nominal amperage for 230V Freeze Dry (model 76700-01) (excluding vacuum pump): 5.3A •...

  • Page 48: Appendix C: Freeze Dryer Specifications

    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 49: Wiring Diagram (115V)

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

  • Page 50: Wiring Diagram (230V)

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

  • Page 51: Appendix D: Freeze Dryer Accessories

    The following accessories are available for the Freeze Dryer. PART # DESCRIPTION 14677-00 Vacuum Pump Two stage direct drive pump, 195 liters/minute. 115 VAC, 50/60 Hz, single phase, 7.8 amps. 77394-03 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 52 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 14723-00 Pump Exhaust Filter Disposable filter that removes visible oil mist from vacuum pump exhaust. 77720-00 Soda Acid Trap Secondary trap that prevents migration of corrosive chemicals into vacuum pump. 77721-00 Replacement Media for Soda Acid Trap 77725-00 Charcoal Solvent Trap Secondary trap that prevents migration of organic solvents into...
  • Page 53 Appendix D: Freeze Dryer Accessories PART # DESCRIPTION 75210-00 Heated Drying Chamber 10 ½" high x 9" diameter type 304 stainless steel. The 3 shelf product heaters heat to 43°C (110°F). 115V 75210-01 Heated Drying Chamber 10 ½" high x 9" diameter type 304 stainless steel. The 3 shelf product heaters heat to 43°C (110°F).
  • Page 54 Appendix D: Freeze Dryer Accessories ® Fast-Freeze Flasks Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 55 Appendix D: Freeze Dryer Accessories ® Lyph-Lock Flasks Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 56 Appendix D: Freeze Dryer Accessories Serum Bottles & Vials Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 57 Appendix D: Freeze Dryer Accessories Ampules Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 58 Appendix D: Freeze Dryer Accessories Product Service: Domestic 1-800-522-7658, International 816-333-8811...
  • Page 59 Product Service Domestic 1-800-522-7658, International 816-333-8811...

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