User’s Manual FreeZone® Bulk Tray Dryers Models 78060 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.
Copyright © 2004, 2007, 2010, 2012, 2013 Labconco Corporation. All rights reserved. The information contained in this manual and the accompanying products are copyrighted and all rights reserved by Labconco Corporation. Labconco Corporation reserves the right to make periodic design changes without obligation to notify any person or entity of such change. Warranty Labconco provides a warranty on all parts and factory workmanship.
TABLE OF CONTENTS CHAPTER 1: INTRODUCTION Freeze Dry Process Freeze Dry Rates Freeze Dry Capacity Samples Containing Volatile Substances 1 1 2 3 4 CHAPTER 2: PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements 4 4 4 5 CHAPTER 3: GETTING STARTED Unpacking Your Bulk Tray Dryer Bulk Tray Dryer Components Setting Up Your Bulk Tray Dryer Installing the Tray Dryer on the Freeze Dry System Venting the Vacuum Pump Electrical Connection Chemical Resistance of Freeze Dryer Compone
CHAPTER 7: TROUBLESHOOTING Vacuum Pump Gaskets, Tubing, Connections, Sample Valves System Components & Collection Chamber Isolation Bulk Tray Dryer 23 23 24 25 29 APPENDIX A: BULK TRAY DRYER COMPONENTS 30 APPENDIX B: BULK TRAY DRYER DIMENSIONS 32 APPENDIX C: BULK TRAY DRYER SPECIFICATIONS Electrical Specifications Environmental Conditions 33 33 33 APPENDIX D: BULK TRAY DRYER ACCESSORIES 34 DECLARATION OF CONFORMITY 39
Chapter 1: Introduction Congratulations on your purchase of a Labconco FreeZone® Bulk Tray Dryer, which is designed for laboratory lyophilization procedures. The unit is easy to install and maintain. Proper care and maintenance of this product will result in many years of dependable service. Freeze Dry Process Freeze drying is an important process in sample preparation and for the preservation and storage of biologicals, pharmaceuticals and foods.
Chapter 1: Introduction SAFE TEMPERATURE AND DRYING TIMES FOR SELECTED MATERIALS Material 10mm Thick Safe Temp °C Collector Temp °C Hours (Approx.) Milk -5 -40 10 Urea -7 -40 10 Blood Plasma -10 to -25 -40 16 Serum -25 -40 18 Vaccinia -30 to -40 -50 22 Influenza Vaccine -30 -50 24 Human Tissue -30 to -40 -50 48 Vegetable Tissue -50 -80 60 *Total sample quantities are contingent on various freeze dryer capacities.
Chapter 1: Introduction Freeze Dry Capacity The volume of a sample that can be freeze dried at one time is related to factors discussed previously and the size and design of the freeze dry system. With any given instrument, the capacity is based on the surface area of the sample, the eutectic temperature and concentration of the sample and the rate and amount of heat transferred to the frozen sample.
Chapter 2: Prerequisites Before you install your Bulk Tray Dryer, you need to prepare your site for installation. The Bulk 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 Bulk 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 Vacuum Pump Requirements A vacuum pump must be provided by the user. A vacuum pump with a displacement of 144 liters per minute and 0.002 mBar ultimate pressure is adequate for most samples. The inlet fitting on the vacuum pump must be suitable for 3/4" ID vacuum hose, which is provided with the FreeZone Freeze Dry System. It is recommended that the vacuum pump is equipped with an exhaust filter to minimize oil mist exhausting from the vacuum pump.
Chapter 3: Getting Started Now that the site for your Bulk Tray Dryer is properly prepared, you are ready to unpack, inspect, install and test your Bulk Tray Dryer. Read this chapter to learn how to: • • • • Unpack and move your Bulk Tray Dryer. Set up your Bulk Tray Dryer. Connect the electrical supply source to your Bulk Tray Dryer. Safely use solvents with your Bulk Tray Dryer. The Bulk Tray Dryer weighs over 202 lbs. (92 Kg). The carton allows for lifting with a mechanical lift truck or hand truck.
Chapter 3: Getting Started Bulk Tray Dryer Components Locate the model of Bulk Tray Dryer you received in the following table. Verify that the components listed are present and undamaged.
Chapter 3: Getting Started Lift the Bulk Tray Dryer into place on your Freeze Dry System while centering the vacuum coupling over the vacuum connection port. Align the four mounting holes in the Bulk Tray Dryer support stand with the four holes in the top of the Freeze Dry System. NOTE: Do not lift the Bulk Tray Dryer by the door or disturb it. Install the four bolts, nuts, and washers provided. Loosen the clamps and slide the lower hose down over the vacuum connection port.
Chapter 3: Getting Started Venting the Vacuum Pump If any materials will be placed in the Bulk Tray Dryer that can liberate hazardous gases when heated, the vacuum pump exhaust must be vented to a fume hood or other ventilation device. Electrical Connection Plug the power cord into the receptacle on the back of the Bulk Tray Dryer and plug the other end into a suitable power receptacle. DO NOT ATTEMPT TO CONNECT THE BULK TRAY DRYER INTO THE FREEZONE FREEZE DRY SYSTEM.
Chapter 3: Getting Started • • Most common compounds used in freeze drying processes, if allowed to enter the vacuum pump, will degrade the oil and cause damage to the vacuum pump. Sugars and proteins typically will have minimal negative effect on any of the materials of construction. When using compounds in the Freeze Dryer that are hostile to the materials of construction, it is imperative the equipment is thoroughly cleaned after use.
Chapter 4: Using Your Bulk Tray Dryer After your Bulk Tray Dryer has been installed as detailed in Chapter 3: Getting Started, you are ready to begin using your Bulk Tray Dryer. Read this chapter to learn how to: • Operate the controls. • Understand the display. • Connect samples. Do not use the Bulk Tray Dryer in a manner not specified by the manufacturer (refer to Appendix C: Bulk Tray Dryer Specifications).
Chapter 4: Using Your Bulk Tray Dryer Bulk Tray Dryer Controls The control panel for the Bulk Tray Dryer is shown below with a description about its function. 4 2 3 3 5 1. Main Power Switch- (Not shown- Located on left side of cabinet) turns the unit on or off. 2. Run/Stop Switch- Initiates the Bulk Tray Dryer to control the temperature of the shelves at the set point temperature. An “R” or “S” will appear in the display at the left hand end to indicate the mode selected. 3.
Chapter 4: Using Your Bulk Tray Dryer 3. Check the collector chamber drain hose on the Freeze Dry System to ensure that the hose is free of moisture and that the drain plug is securely installed. 4. Using a soft, lint-free cloth or paper towel, wipe the Freeze Dry System collector chamber lid gasket and the Bulk 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 to obtain a proper vacuum seal. 5.
Chapter 4: Using Your Bulk Tray Dryer 3. Freeze the Sample - Before the freeze dry process can occur the product must be in a frozen state. This must be done in a freezer separate from the Bulk Tray Dryer. 4. Start the Freeze Dry System - Turn on the Freeze Dry System using the Manual Mode. (See Freeze Dry System User’s Manual) 5. Set the Bulk Tray Dryer Temperature - Turn the Bulk Tray Dryer on by pressing the Power Switch. Press either the Increase or Decrease button once.
Chapter 4: Using Your Bulk Tray Dryer Freeze Drying Using the Manifold Valves Some Bulk Tray Dryers are equipped with a manifold with six sample valves. The following procedure should be followed when freeze drying samples using the manifold. 1. Turn the power switch on the Bulk Tray Dryer to OFF and close the door. Set the vacuum control to CLOSE. 2. Pre-freeze samples; shell freezing of samples is recommended.
Chapter 4: Using Your Bulk Tray Dryer 6. When all the frost has disappeared from the outer surface of the sample container and no cold spots can be detected by handling the container, the sample is nearly dry. To be certain of low final moisture content, dry the sample for several hours past this point. 7. To remove a container after drying is complete, turn the plastic knob on the valve to the “VENT” position, which closes the valve and vents the container.
Chapter 5: Maintaining Your Bulk Tray Dryer Under normal operation, the Bulk 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 Bulk Tray Dryer Monthly: 1. The rubber components on the Bulk Tray 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. 2. Using a soft cloth, sponge or chamois and a mild, non-abrasive soap or detergent, clean the acrylic door. 3.
Chapter 6: Using the RS232 Receptacle The operation of the Bulk Tray Dryer can be monitored using a computer when the RS232 Receptacle is installed. The computer cannot control the operation of the Bulk Tray Dryer. The monitored parameters are the shelf set point temperature, actual temperature of each shelf, the run time and operating status. 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 data content of the RS232 message from the Bulk Tray Dryer is as follows: Sample output: RUN, T5 = 162, SP= -10, T1 = -9, T2 = -9, T3 = -9, T4 = *****, T5 = ***** Columns 1-4 Run, Stop, or Open Columns 7-11 Columns 14-19 Columns 22-29 T = 162 Running time in minutes Set Point = -10 T1 = -9 Columns 32-39 T2 = -9 Columns 42-49 T3 = -9 Columns 52-59 T4 = ***** Columns 62-69 T5 = ***** Tells overall operating status where “open” indicates door open Time in m
Chapter 6: Using the RS232 Receptacle The first time Hyper Terminal™ is opened a dialogue box requesting an area code and phone number will appear. Enter the appropriate numbers and continue. 3. The “Connection Description” dialogue box will open. Type in a user defined name and select an icon for the new connection. Press “OK.” 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.
Chapter 6: Using the RS232 Receptacle 5. The “Com X Properties” dialogue box will open. Enter the appropriate data properties and press “OK.” 6. When the main power switch is on the Labconco unit is on, data will be transmitted and updated. See the previous paragraph of this chapter in this manual for details on exactly what RS232 data is transmitted and in what order.
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 0.033 mBar within 18 hours when the refrigeration is operating.
Chapter 7: Troubleshooting 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. Confirm that the pump is capable of achieving an ultimate vacuum less than 0.010 mBar or approximately 10 microns. If an inadequate vacuum reading is obtained, the pump has most likely failed and may need to be replaced or rebuilt. II.
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 of the Freeze Dry System collection chamber.
Chapter 7: Troubleshooting 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. Replace the collection chamber lid and turn on the vacuum pump. Allow the vacuum pump to run for approximately 5 to 10 seconds. (If the vacuum pump is left on, the water will begin to boil and the test will not be effective).
Chapter 7: Troubleshooting O Ring and Vacuum Grease Collector Coil Nut 4. If bubbling was observed on the chamber surface, the chamber must be replaced. This type of leak cannot be successfully repaired. The leading cause of a chamber surface leak is corrosive residue left in the chamber after use. This test verifies that the vacuum leak is in the Bulk Tray Dryer. 1. Remove the Bulk Tray Dryer. 2. Position a flat gasket over the 3.
Chapter 7: Troubleshooting IV. Bulk Tray Dryer • • • • Inspect the door and door gasket. Inspect the coupling between the freeze dryer and the Bulk Tray Dryer. Remove the top left hand cover panel and inspect the valve and hose connections to the chamber. Inspect the electrical pass through and gasket on the left side of the chamber.
Appendix A: Bulk Tray Dryer Components The following pages list components that are available for your Bulk Tray Dryer. The parts shown are the most common replacement parts. If other parts are required, contact Product Service. Item Qty Part No.
Appendix A: Bulk Tray Dryer Components Product Service 1-800-522-7658 31
Appendix B: Bulk Tray Dryer Dimensions 32 Product Service 1-800-522-7658
Appendix C: Bulk Tray Dryer Specifications This Appendix contains technical information about the Freeze Dryer including electrical specifications and environmental operating conditions. Electrical Specifications • Nominal amperage – Models 7806020 & 7806021: 8A • Nominal amperage – Models 7806030, 7806031, 7806040, 7806041, 7806060, 7806061, 7806070, & 7806071: 4A • Frequency: All Models 50/60 Hz • Phase: Single Environmental Conditions • Indoor use only. • Maximum altitude: 6562 feet (2000 meters).
Appendix D: Bulk Tray Dryer Accessories The following accessories are available for the Freeze Dryer. PART # DESCRIPTION 7756100 Tray with Slide-Out Bottom 14" wide x 12" deep. Stainless steel tray has separate bottom, which slides out allowing serum bottles and ampules direct contact with the shelf to facilitate the drying process. Bulk Tray 15" wide x 11-1/2" deep. Stainless steel tray will contain liquids for bulk drying. Support Grid 7" wide x 7" deep.
Appendix D: Bulk 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.
Appendix D: Bulk Tray Dryer Accessories Fast-Freeze® Flasks Fast-Freeze Flasks are specially designed to be easier to handle, faster to load and more convenient to use than other freeze dry glassware now in your laboratory. Compatible with all major brands of laboratory freeze dry equipment, Fast-Freeze Flasks eliminate the risk of contamination from vacuum grease, reduce spillage of valuable samples and require no washers, gaskets or retainers.
Appendix D: Bulk Tray Dryer Accessories Lyph-Lock® Flasks Lyph-Lock Flasks simplify your Lyophilization procedures because they have only three pieces per flask – a high strength borosilicate glass top and bottom with a silicone rubber ring seal. The unique wide-mouth design helps you load samples easily and lyophilize efficiently. How to select Lyph-Lock Flasks for your Freeze Dry System Select Lyph-Lock Flasks fast- based on your sample sizes.
Appendix D: Bulk Tray Dryer Accessories Ampules Oxygen/Natural Gas Sealing Torch Labconco Ampules are fabricated of highest quality borosilicate glass for strength and durability. They are available in four different configurations to provide the ideal ampule for your specific lyophilization requirements, from tray drying to flame sealing applications. 7578500 Torch specifically designed for flame sealing freeze dry ampules. Seals all types of heatresistant glass.
Product Service 816-333-8811 39
