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 Please read the User’s Manual before operating the equipment.
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TABLE OF CONTENTS CHAPTER 1: INTRODUCTION Freeze Dry Process Freeze Dry Rates Freeze Dry Capacity Samples Containing Volatile Substances About This Manual Typographical Conventions 1 1 2 3 4 4 5 CHAPTER 2: PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements 6 6 7 7 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 Venting the Vacuum Pump
Sample Freezing Freeze Drying Stoppering Vacuum Break/Backfilling Alarms System Temperature Variations Vacuum System Temperature Set Point Power Failure Temperature Probe 25 25 25 26 26 26 26 27 27 27 CHAPTER 5: MAINTAINING YOUR STOPPERING TRAY DRYER 28 CHAPTER 6: USING THE RS232 RECEPTACLE for Computer Interface Computer Connection 30 30 CHAPTER 7: TROUBLESHOOTING Vacuum Pump Gaskets, Tubing, Connections, Sample Valves System Components & Collection Chamber Isolation Stoppering Tray Dryer Refrigerati
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.
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. A listing of selected materials and their approximate drying times are shown in Table 1 for your reference.
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. 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.
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. Also, compared to water, they will require the absorption of less heat for sublimation to occur.
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. Appendix D: Stoppering Tray Dryer Accessories lists the part numbers and descriptions of all of the accessories available for your Stoppering Tray Dryer.
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. You must be certain that the area is level and of solid construction. An electrical source must be located near the installation site.
Chapter 2: Prerequisites Location Requirements The Freeze Dryer should be located in an area that provides an unobstructed flow of air around the cabinet. This air cools the refrigeration system. The refrigeration system draws air in through the front and exhausts it through the rear. A minimum of 3" must be allowed between the rear and both sides of the Freeze Dryer and adjacent wall surfaces. Restriction of airflow during operation could adversely affect performance.
CHAPTER 3 GETTING STARTED Now that the site for your Stoppering Tray Dryer is properly prepared, you are ready to unpack, inspect, install and test your Stoppering Tray Dryer. Read this chapter to learn how to: unpack and move your Stoppering Tray Dryer. set up your Stoppering Tray Dryer. connect the electrical supply source to your Stoppering Tray Dryer. safely use solvents with your Stoppering Tray Dryer. ! The Stoppering Tray Dryer weighs over 400 lbs. (181 Kg).
Chapter 3: Getting Started IF YOUR STOPPERING TRAY DRYER WAS DAMAGED IN TRANSIT, YOU MUST FILE A CLAIM DIRECTLY WITH THE FREIGHT CARRIER. LABCONCO CORPORATION AND ITS DEALERS ARE NOT RESPONSIBLE FOR SHIPPING DAMAGE. DO NOT DISCARD THE CARTON OR PACKING MATERIAL FOR YOUR STOPPERING TRAY DRYER UNTIL YOU HAVE CHECKED ALL OF THE COMPONENTS AND INSTALLED AND TESTED THE STOPPERING TRAY DRYER. Stoppering Tray Dryer Components Locate the model of Stoppering Tray Dryer you received in the following table.
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. If the Freeze Dry System has a flat gasket around the 3.0 inch vacuum port, remove it.
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” position and the Vac Release control is in the “CLOSED” position. Start the vacuum pump and monitor the vacuum gauge. The vacuum on the Freeze Dry System should reach 0.
Chapter 3: Getting Started Chamber & Fittings Pyridine D Methyl t-Butyl Ether (BTBE) D Dioxane C Cyclohexane D Carbon Tetrochloride Silicon Rubber Stainless Steel D Acetonittirle C D Solvents Acetone Neoprene D D Sodium Phosphate D Calcium Chloride C Buffers Trifluoroacetic Acid (TFA) Material Acetal Acrylic Formic Acid Component Valve Stem Collector* Lid & Door Hoses, Gaskets & Valve Bodies Flask Top Acetic Acid 20% Acids D D D D C C D D D C D D D D C D C * An
Chapter 3: Getting Started Another way to extend the life of the vacuum pump is to install an optional secondary trap in the line between the Freeze Dry System and the vacuum pump. Contact Labconco for ordering information. With prudent maintenance the FreeZone Freeze Dry System will provide years of service. Warranty on the affected parts will be voided if maintenance has been obviously neglected.
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. connect samples. ! 14 Do not use the Stoppering Tray Dryer in a manner not specified by the manufacturer (refer to Appendix C: Stoppering Tray Dryer Specifications).
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. 3 2 1 11 4 13 5 10 9 8 6 7 6 12 14 14 1. Display. Displays all necessary programming and operational data. Provides prompts to aid in programming. 2. Display Selector. Changes format of display from “monitor’ to “auto” to “manual” to “set up” screen. 3. Display Indicators.
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. 10. Run/Stop Switch. Initiates the start or stop of the lyophilization process. 11. Run/Stop Indicator. Amber lamp burns steadily while freeze drying is in progress and turns off if either the programmed cycle is completed or the process is terminated in mid cycle.
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.
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 (1) Turn the Power switch ON. The display will become active. (2) Push the DISPLAY button until the Manual LED lights. This will cause the manual display screen to be shown with the previously entered set point temperature.
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. Above 5.0 mBar the display will show “hi” vacuum. System temperature rather than probe temperature is the parameter that is regulated by the controller.
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. A typical 3 segment program is shown in Figure 5.
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. Turn the Power switch to the ON position. Press the DISPLAY button until the Auto LED lights. NOTE: Values shown in this example are for reference only.
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: P1 PRB 1=28 2=29 3=28 TMP=30 SEG=1R VAC=.
Chapter 4: Using Your Stoppering Tray Dryer Changing the Program Parameters in the Middle of a Run (1) Press DISPLAY to obtain Monitor screen. Note current operating segment. (2) Press DISPLAY to obtain Auto screen. (3) Enter a segment number that will occur after the current segment that is running. The presently running segment cannot be modified while the system is running. (4) Modify as required. (5) Press ENTER. Stopping the Freeze Dry Cycle 1.
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. It is best to observe the shelf supporting mechanism and practice while reading these procedures.
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. Sample Freezing Before the freeze dry process can occur, the products to be dried must be in a frozen state.
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. The Stoppering control should be left in the “LOWER” position when not stoppering. Vacuum Break/Backfilling To open the chamber door, the vacuum must be released.
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.
CHAPTER 5 MAINTAINING YOUR STOPPERING TRAY DRYER Under normal operation, the Stoppering Tray Dryer requires little maintenance. The following maintenance schedule is recommended: As needed: 1. The user has the responsibility for carrying out appropriate decontamination if hazardous material is spilled on or inside the equipment. This may be done by wiping the contaminated surfaces with a soft cloth dampened with alcohol. Alcohol may craze the acrylic door.
Chapter 5: Maintaining Your Stoppering Tray Dryer 2. Using a soft cloth, sponge or chamois and a mild, non-abrasive soap or detergent, clean the acrylic door. 3. Using a soft cloth, sponge, or chamois and a mild, non-abrasive soap or detergent, clean the exterior surfaces of the unit. Liquid spray cleaners and polishes may be used on the exterior surfaces. Do not use solvents to remove stains from the exterior surfaces as they may damage the finish. Annually: 1.
CHAPTER 6 USING THE RS232 RECEPTACLE The operation of the Stoppering Tray Dryer and the FreeZone Freeze Dry System can be monitored using a computer when the Stoppering Tray Dryer is connected to the RS232 receptacle on the rear panel of the Freeze Dry System base unit. The computer cannot control the operation of the Freeze Dry System. Computer Connection for Computer Interface Check your computer to see which type of serial port is provided, then use a connecting cable below: 1.
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 10 SECONDS Press select until the desired time interval is shown.
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.
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.
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.
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 achieve an ultimate vacuum of 0.040 mBar within 18 hours when the refrigeration is operating.
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. Isolate the pump by disconnecting the vacuum hose from the Freeze Dry System. Deadhead the pump by inserting the vacuum sensor from a secondary vacuum gauge into the end of the vacuum hose and observe the vacuum reading obtained.
Chapter 7: Troubleshooting The illustration below shows how the sample valve installs on a manifold. Manifold Assembly Knob & Stem Assembly Valve Body Trim Ring 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. 1. Place a rubber stopper in the vacuum port in the left side of the collector chamber and another in the drain port in the bottom. 2. Restart the vacuum system and check your vacuum indication.
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. 2. Fill the collection chamber with approximately 2 inches of water, enough to cover all fittings.
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. Be careful not to damage the evaporator coils or the brazed joints to the refrigeration system. Once the fitting is tightened, perform the test again.
Chapter 7: Troubleshooting Stoppering Tray Dryer Inspect the door and door gasket. Inspect the coupling between the freeze dryer and the Stoppering Tray Dryer. Remove the top left hand cover panel and inspect the valve and hose connections to the chamber. Remove the top right hand cover and inspect the electrical pass through and gasket on the top of the chamber.
Chapter 7: Troubleshooting Shelf and Stoppering System Removal (1) The shelf and stoppering system may be removed from the chamber as an assembly for repairs if needed. (2) Remove the acrylic door by taking out the two hex socket head screws located on the right hand end of the cross bar. (3) Remove the door gasket. Carefully pull loose all of the plastic fasteners (located around the periphery of the chamber) from the chamber. Leave the spacer blocks behind the gasket attached to the gasket.
Chapter 7: Troubleshooting Filling the Fluid System 1. 2. 3. 4. Fluid Circulation Valve Fluid Reservoir and Cap Electrical Junction Block Flexible Tubing (1) Make sure the Power Switch is in the OFF position. (2) Remove the left cover. (3) Remove the insulation and both caps from the fluid circulation valve, which is located directly behind the fluid reservoir (Item 1). (4) Attach a flexible tube to the exposed port (service port). The port is 3/8" x 45° male flare (Item 4).
Chapter 7: Troubleshooting (7) 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. (8) 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. If it is installed, the RUN/STOP switch must be off.
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. If irritation persists, get medical attention. Skin Contact: Wash contaminated areas with soap and water. Remove contaminated clothing and footwear. Wash clothing before reuse.
CHAPTER 8 MODIFYING YOUR STOPPERING TRAY 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. Use an accurate traceable reference to compare the readings. Vacuum offset may be varied ±0.010 mBar in 0.
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.
APPENDIX A STOPPERING TRAY DRYER COMPONENTS 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.
Appendix A: Stoppering Tray Dryer Components Item Part No.
Appendix A: Stoppering Tray Dryer Components Product Service 1-800-522-7658 49
APPENDIX B STOPPERING TRAY DRYER DIMENSIONS 50 Product Service 1-800-522-7658
Appendix B: Stoppering Tray Dryer Dimensions Serum Bottle Capacity of the Stoppering Tray Dryer Size 2 ml 3 ml 5 ml 10 ml 20 ml 30 ml 50 ml 100 ml 125 ml Labconco No. Shelf Capacity No.
APPENDIX C STOPPERING TRAY DRYER SPECIFICATIONS This Appendix contains technical information about the Freeze Dryer including electrical specifications and environmental operating conditions.
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.
Appendix D: Stoppering Tray Dryer Accessories Serum Bottles and Vials Threaded Vials Stoppers and threaded vials with Screw Caps are supplied in packages of 200. Perfect for long term storage of freeze dried samples. Labconco Serum Bottles and Treaded 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.
