Labconco FreeZone 79480 Series User Manual

Stoppering tray dryers

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79480 Series

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Stoppering Tray Dryers

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Kansas City, MO 64132-2696

800-821-5525, 816-333-8811

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Page 1 User’s Manual  FreeZone Stoppering Tray Dryers Models 79480 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...
Page 2: Warranty
This limited warranty covers parts and labor, but not transportation and insurance charges. In the event of a warranty claim, contact Labconco Corporation or the dealer who sold you the product. If the cause is determined to be a manufacturing fault, the dealer or Labconco Corporation will repair or replace all defective parts to restore the unit to operation.
Page 3: Table Of Contents
CHAPTER 1: INTRODUCTION 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 CHAPTER 3: GETTING STARTED Unpacking Your Stoppering Tray Dryer Stoppering Tray Dryer Components Setting Up Your Stoppering Tray Dryer Installing the Tray Dryer on the Freeze Dry System...
Page 4 Sample Freezing Freeze Drying Stoppering Vacuum Break/Backfilling Alarms System Temperature Variations Vacuum System Temperature Set Point Power Failure Temperature Probe CHAPTER 5: MAINTAINING YOUR STOPPERING TRAY DRYER CHAPTER 6: USING THE RS232 RECEPTACLE Computer Connection for Computer Interface CHAPTER 7: TROUBLESHOOTING Vacuum Pump Gaskets, Tubing, Connections, Sample Valves System Components &...
Page 5: Chapter 1: Introduction
Congratulations on your purchase of a Labconco FreeZone® Stoppering Tray Dryer, 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.
Page 6: Freeze Dry Rates
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 7: Freeze Dry Capacity
Chapter 1: Introduction vapor is from the sample to the collector. Since this vapor diffusion process occurs very slowly under normal atmospheric conditions, a good vacuum is essential to maintain an efficient rate. In many applications, the maintenance of a vacuum of 0.133 mBar or less is recommended.
Page 8: Samples Containing Volatile Substances
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 9: Typographical Conventions
Chapter 1: Introduction Appendix A: Stoppering Tray Dryer Components contains labeled diagrams of the components of the Stoppering Tray Dryer. Appendix B: Stoppering Tray Dryer Dimensions contains comprehensive diagrams showing the dimensions for the Stoppering Tray Dryer. Appendix C: Stoppering Tray Dryer Specifications contains product specifications.
Page 10: Chapter 2: Prerequisites
Before you install your Stoppering Tray Dryer, you need to prepare your site for installation. The Stoppering Tray Dryer will mount on top of a FreeZone 6, 12 or 18 liter Freeze Dry System. This could be either a benchtop or console model. Carefully examine the location where you intend to install your Stoppering Tray Dryer.
Page 11: Location Requirements
Freeze Dry System. Refer to the User’s Manual for the FreeZone Freeze Dry System for vacuum pumps available from Labconco. Product Service 1-800-522-7658...
Page 12: Chapter 3: Getting Started
Commission by the carrier. rules require that claims be filed with the DO NOT RETURN GOODS WITHOUT THE PRIOR  delivery carrier AUTHORIZATION OF LABCONCO. within fifteen (15) days of UNAUTHORIZED RETURNS WILL NOT BE ACCEPTED. delivery. Product Service 1-800-522-7658...
Page 13: Stoppering Tray Dryer Components
Cable RS 232 If you did not receive one or more of the components listed for your Stoppering Tray Dryer, or if any of the components are damaged, contact Labconco Corporation immediately for further instructions. Setting Up Your Stoppering Tray Dryer After you verify receipt of the proper components, move your Stoppering Tray Dryer to the location where you want to install it.
Page 14: Installing The Tray Dryer On The Freeze Dry System
Chapter 3: Getting Started Installing the Tray Dryer on the Freeze Dry System The following tools are required to install the Stoppering Tray Dryer onto a FreeZone Freeze Dry System base unit: Flat blade screwdriver or 5/16" socket and a 7/16" wrench or socket. Remove the four plastic hole plugs from the top of the Freeze Dry System on which the Stoppering Tray Dryer is to be mounted.
Page 15: Venting The Vacuum Pump
Chapter 3: Getting Started The Stoppering Tray Dryer is now installed and must be tested to make certain the system is free of leaks. To test, turn on the Freeze Dry System refrigeration and allow the temperature to reach –40° or lower. Close the door of the Tray Dryer and make sure the Stoppering Control is in the “LOWER”...
Page 16 Chapter 3: Getting Started Acids Buffers Solvents Component Material Valve Stem Acetal Collector* Acrylic Lid & Door Hoses, Neoprene Gaskets & Valve Bodies Flask Top Silicon Rubber Chamber & Stainless Fittings Steel * An accessory glass lid is available for the Freeze Dry Systems. C –...
Page 17: 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 Dry System, 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 Stoppering Tray Dryer may be flammable or hazardous to your health.
Page 18: Chapter 4: Using Your Stoppering Tray Dryer
After your Stoppering Tray Dryer has been installed as detailed in Chapter 3: Getting Started, you are ready to begin using your Stoppering Tray Dryer. Read this chapter to learn how to:  operate the controls.  understand the display. ...
Page 19: Stoppering Tray Dryer Controls
Chapter 4: Using Your Stoppering Tray Dryer Stoppering Tray Dryer Controls The control panel for the Stoppering Tray Dryer is shown with a description about its function. 1. Display. Displays all necessary programming and operational data. Provides prompts to aid in programming. 2.
Page 20: Operation Checklist
Chapter 4: Using Your Stoppering Tray Dryer 8. Mode Indicator. Amber lamp indicates whether the control is set to operate either in the automatic or manual mode. 9. Mode Selector Switch. Selects the mode of operation – either manual or automatic.
Page 21: Operating The Stoppering Tray Dryer
Chapter 4: Using Your Stoppering Tray Dryer 4. Using a soft, lint-free cloth or paper towel, wipe the Freeze Dry System collector chamber lid gasket and the Stoppering Tray Dryer door gasket to remove any dirt and contaminants that could cause a vacuum leak. Vacuum grease is not required on the door gasket or collector lid gasket to obtain a proper vacuum seal.
Page 22: Manual Control Operation
Chapter 4: Using Your Stoppering Tray Dryer  Hold  for 5 seconds.  Press ENTER.  At any time the DISPLAY button can be pressed to select a different display screen. Manual Control Operation Turn the Power switch ON. The display will become active. Push the DISPLAY button until the Manual LED lights.
Page 23: Automatic Control Operation
Chapter 4: Using Your Stoppering Tray Dryer The segment number will always indicate “M” while operating in the manual mode. Segment numbers are used only in the automatic mode to identify portions of the programmed cycle. Temperatures and vacuum are displayed in the units selected during the set up procedure.
Page 24: Automatic Start-Up Of Freeze Dryer Vacuum
Chapter 4: Using Your Stoppering Tray Dryer When the desired temperature is achieved, the hold function will maintain that temperature for the programmed length of time. The microprocessor control has a built in memory of the last entered program to allow the identical protocol to be repeated by simply pushing the RUN button.
Page 25: Programming
Chapter 4: Using Your Stoppering Tray Dryer Programming The Tray Dryer will store up to five programs numbered 1 through 5. The five programs, once programmed, will be retained in memory. To program a run, select the program number that you want to use and enter the parameters as follows.
Page 26 Chapter 4: Using Your Stoppering Tray Dryer Status Display will change and the Display will change to MONITOR mode. During the RAMP cycle of the active segment, the Status Display will be as follows: -indicates what program is PRB 1=28 2=29 3=28 selected...
Page 27: Changing The Program Parameters In The Middle Of A Run
Chapter 4: Using Your Stoppering Tray Dryer Changing the Program Parameters in the Middle of a Run Press DISPLAY to obtain Monitor screen. Note current operating segment. Press DISPLAY to obtain Auto screen. Enter a segment number that will occur after the current segment that is running.
Page 28: Shelf Spacing Adjustment
Chapter 4: Using Your Stoppering Tray Dryer If the temperature is warmer than +50°C, the display will show “HI”. If the temperature is cooler than –50°C, the display will say “LO”. Shelf Spacing Adjustment Prior to loading the shelves with the product to be freeze dried, adjust the shelves to the 3-shelf, 2-shelf or 1-shelf position.
Page 29: Sample Freezing
Chapter 4: Using Your Stoppering Tray Dryer The stoppering action should be monitored by looking through the chamber door. Cease stoppering when all bottles appear stoppered or if a problem occurs. Distributing the serum bottles evenly on the shelves also aids in consistent drying of all serum bottles on each shelf.
Page 30: Vacuum Break/Backfilling
Chapter 4: Using Your Stoppering Tray Dryer When all of the vials appear to be stoppered, move the Stoppering control to the “LOWER” position. This opens the diaphragm to the vacuum pump, which deflates the diaphragm. Opening the vacuum release control also deflates the stoppering diaphragm.
Page 31: System Temperature Set Point
Chapter 4: Using Your Stoppering Tray Dryer System Temperature Set Point If during a Ramp mode the system temperature stabilizes without reaching the set point temperature, the control will enter the next Hold mode. The Red Alarm indicator will flash and the program indicator “Px” on the display will flash. Pressing Run/Stop or turning off the power switch cancels the flashing warning.
Page 32 Alcohol may craze the acrylic door. Before using any cleaning or decontamination method except those recommended by Labconco, users should check with Labconco that the proposed method will not damage the equipment. 2. Clean up all spills; remove liquids from the chamber.
Page 33: Chapter 5: Maintaining Your Stoppering Tray Dryer
When freeze drying biological substances, it may be necessary to decontaminate the system. A surface decontaminant should be used to clean the accessible surfaces. The use of ethylene oxide is not recommended because of its hazardous and corrosive nature. Contact Labconco for additional information. Product Service 1-800-522-7658...
Page 34: Chapter 6: Using The Rs232 Receptacle
1. Computers with a 25-pin D-sub male serial connector should use Connect Cable, Labconco part number 7537801, to connect a computer to the Labconco Freeze Dry System. 2. Computers with a 9-pin D-sub male serial connector should use Connect Cable, Labconco part number 7537800, to connect a computer to the Labconco Freeze Dry System.
Page 35 Chapter 6: Using The RS232 Receptacle The time between data transmissions may be varied by the user to occur at 10, 30, 60, 300 or 600 second intervals. Press the MENU button on the Freeze Dryer base unit until the RS232 screen appears on the display. RS-232 TRANSMISSION RATE SECONDS Press select until the desired time interval is shown.
Page 36 Chapter 6: Using The RS232 Receptacle 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). Consult your laboratory supply dealer regarding the latest software available.
Page 37 Chapter 6: Using The RS232 Receptacle 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 38 Chapter 6: Using The RS232 Receptacle 6. When the Freeze Dryer main power switch is on, the data will be transmitted and updated at the time intervals selected by the user. Product Service 1-800-522-7658...
Page 39: Chapter 7: Troubleshooting
Refer to the following if your Freeze Dry System fails to operate properly. If the suggested corrective actions do not solve your problem, contact Labconco for additional assistance. FreeZone Freeze Dry Systems that are clean and dry and without samples attached should reach a vacuum of 0.133 mBar within 30 minutes and should...
Page 40: Gaskets, Tubing, Connections, Sample Valves
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 41: System Components & Collection Chamber Isolation
Chapter 7: Troubleshooting The illustration below shows how the sample valve installs on a manifold. Manifold Assembly Knob & Stem Valve Body Trim Ring Assembly System Components and Collection Chamber Isolation The following test allows you to check the pump and the connections from the pump to the vacuum tube.
Page 42 Chapter 7: Troubleshooting The following test is used to check the integrity at the Freeze Dry System collection chamber. The figure below points out potential areas to locate a leak: Collector Chamber Areas for Potential Leaks 1. Remove the stopper from the side of the chamber and place a flat gasket and a freeze dry flask over the connection port.
Page 43 Chapter 7: Troubleshooting 3. If bubbling is observed around the bulkhead fittings, access the bottom of the chamber and remove the insulation. Tighten the appropriate fitting by placing a wrench on the fitting inside the chamber and use a second wrench to turn the nut on the bottom of the chamber.
Page 44: Stoppering Tray Dryer
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 45: Shelf And Stoppering System Removal
Chapter 7: Troubleshooting Shelf and Stoppering System Removal The shelf and stoppering system may be removed from the chamber as an assembly for repairs if needed. Remove the acrylic door by taking out the two hex socket head screws located on the right hand end of the cross bar. Remove the door gasket.
Page 46: Filling The Fluid System
Chapter 7: Troubleshooting Filling the Fluid System 1. Fluid Circulation Valve 2. Fluid Reservoir and Cap 3. Electrical Junction Block 4. Flexible Tubing Make sure the Power Switch is in the OFF position. Remove the left cover. Remove the insulation and both caps from the fluid circulation valve, which is located directly behind the fluid reservoir (Item 1).
Page 47: Heat Transfer Fluid Precautions
Chapter 7: Troubleshooting Open the fluid circulation valve by completely “down-seating” (turn top valve stem completely clockwise) to direct fluid to by-pass through tubing to fluid reservoir. Attach the power wires to the power switch. Activate the pump by moving the Power switch to the ON position. The control panel does not need to be installed.
Page 48: Heat Transfer Fluid First Aid Procedures
Chapter 7: Troubleshooting Disposal of Non-Recyclable Solvents: Dispose of in accordance with all federal, state, and local health and pollution regulations. Follow same guidelines as used when disposing kerosene. Heat Transfer Fluid First Aid Procedures Eye Contact: Immediately flush eyes with fresh water for at least 15 minutes.
Page 49: Dryer Display
Your Stoppering Tray Dryer has been carefully calibrated and tested before shipping, however under certain circumstances it may be necessary to adjust the calibration of the vacuum display or to reset factory settings. These adjustments may be necessary if the Stoppering Tray Dryer requires service. An offset may be added to the vacuum display.
Page 50: Chapter 8: Modifying Your Stoppering Tray Dryer Display
Chapter 8: Modifying Your Stoppering Tray Dryer Display If you want to restore all factory settings hold ENTER approximately 5 seconds. This will reset: Vacuum units to mBar Temperature units to °C Refrigeration service hours to 0 Refrigeration total hours to 0 RS232 transmission rate to 10 seconds Vacuum offset to 0 mBar At the completion of Master Reset, the display will show operational parameters.
Page 51 The following pages list components that are available for your Stoppering Tray Dryer. The parts shown are the most common replacement parts. If other parts are required, contact Product Service. Product Service 1-800-522-7658...
Page 52 Appendix A: Stoppering Tray Dryer Components Item Part No. Description Compressor 115V – 60 Hz 7592002 Compressor 230V – 50 Hz 7592001 Compressor 230V – 60 Hz 7592000 7501900 Lexsol Pump 115V 7501901 Lexsol Pump 230V 7510900 Heater 115V 7510901 Heater 230V 7529500 Bulkhead Harness...
Page 53 Appendix A: Stoppering Tray Dryer Components Product Service 1-800-522-7658...
Page 54 Product Service 1-800-522-7658...
Page 55: Appendix B: Stoppering Tray Dryer Dimensions
Appendix B: Stoppering Tray Dryer Dimensions Serum Bottle Capacity of the Stoppering Tray Dryer Size Labconco No. Shelf Capacity No. of Shelves Total Capacity 2 ml 7575010 1290 3 ml 7575210 1449 5 ml 7573010 10 ml 7573210 20 ml...
Page 56: Appendix C: Stoppering Tray Dryer
This Appendix contains technical information about the Freeze Dryer including electrical specifications and environmental operating conditions. Electrical Specifications Voltage Catalog Operating Number Description Nominal Range Frequency Phase Amperage 7948020 Stoppering Tray Dryer 103-127 16.0 98-110 16.0 7948030 Stoppering Tray Dryer 208-254 7948040 Stoppering Tray Dryer...
Page 57: Appendix D: Stoppering Tray Dryer Accessories
The following accessories are available for the Freeze Dryer. PART # DESCRIPTION 7726500 6 Port Manifold for use with Stoppering Tray Dryer Mounts between the Stoppering Tray Dryer and the base unit and provides 6 freeze dry valves. 7537800 Cable Connect the RS232 output from the Freeze Dryer (or Freeze Dryer/Tray Dryer combination) to an IBM compatible computer with a 9-pin serial data port.
Page 58 Stoppers and threaded vials with Screw Caps are supplied in packages of 200. Size Vials with Stoppers Screw Caps Perfect for long term storage of freeze dried samples. Labconco Serum 5 ml 7762300 7762200 10 ml 7762600 7762200 Bottles and Treaded Vials are specifically designed for lyophilization applications.

This manual is also suitable for:

Freezone 7948030 Freezone 7948020 Freezone 7948040 Freezone 7948060 Freezone 7948070