SP INDUSTRIES, INC.
Copyright © 2009 SP Industries, Inc. All marks herein are used under license. All brand or product names mentioned may be trademarks or registered trademarks of their respective companies. Part Number 414258 Revision 004, 12/09 SP Industries Inc.
Important Symbols Warning! Injury or even death may result if a recommendation marked with this symbol is not heeded. Crush Hazard. Keep hands clear when operating door. Electric Shock Danger! Use appropriate caution to avoid injury or death. Corrosive Chemical. Wear suitable gloves, safety glasses, and protective clothing. Burn Danger! Potentially hot surface. Use appropriate caution. Property Caution! To prevent damage to chamber equipment and/or load, adhere to procedures marked by this symbol.
Warranty Information VirTis BenchTop 2K, 4K and 6K are warranted by SP Industries to be free of defects in material and workmanship when operated under normal conditions as specified in the instructions provided in this manual. Please take this opportunity to locate the serial tag on your new VirTis BenchTop 2K, 4K and 6K and record the information below for future reference. SP Industries also recommends that you complete and return your unit’s warranty registration card.
iv Revision 004, 12/09 © SP Industries, Inc.
Contents Important Symbols ............................................................................................................................................... ii Freeze Dryer Safety Warnings............................................................................................................................. ii Warranty Information .......................................................................................................................................... iii Introduction....
Contents VirTis BenchTop 2K, 4K and 6K Relay Test .....................................................................................................................................................15 Vacuum Pump Maintenance .........................................................................................................................15 Alarms Menu.....................................................................................................................................................
VirTis BenchTop 2K, 4K and 6K Contents Appendix D: Spare Parts List ............................................................................................................. 45 Revision 004, 12/09 © SP Industries, Inc.
Chapter Introduction 1 VirTis BenchTop 2K, 4K and 6K freeze dryers offer a low-cost solution for laboratories with space constraints. Featuring condenser temperatures of -55 °C to -105 °C, BenchTop freeze dryers can handle a wide range of processing requirements. Key Features • Extremely compact design. • Direct chamber, flask and/or shelf drying capabilities. • Versatile Sentry 2.0 control panel. • Three- to nine-liter condenser capacity. • Variety of refrigeration system options.
Introduction VirTis BenchTop 2K, 4K and 6K Available Configurations Freeze-drying in the condenser Flask drying on drum manifold Shelf unit in drum manifold Flask drying on drum manifold with stoppered shelves Vertical manifold Fitted for cold trap application From Freeze Dryer to Condenser Module When using your BenchTop as a condenser module, the vacuum cover plate is replaced with either a ¾-inch stainless steel port for the manifold plate or a plain cover plate, which must be purchased separate
Chapter Installation and Setup 2 Initial Inspection Upon receiving your BenchTop series freeze dryer, inspect all contents of your shipment for damage. Check packing material for small accessory items. Remove all packing material carefully and inspect the unit for shipping damage. In the event that shipping damage has occurred, retain all packing material and contact your freight carrier immediately.
Installation and Setup VirTis BenchTop 2K, 4K and 6K Vacuum Pump Installation A remotely mounted vacuum pump is required for operation of your BenchTop freeze dryer. The vacuum pump must be a two-stage, high-vacuum pump that does not exceed the maximum allowable amperage listed on the unit’s serial tag and back panel label.
VirTis BenchTop 2K, 4K and 6K Installation and Setup 10. Plug the vacuum pump into the receptacle marked VACUUM PUMP on the back of the unit. The receptacle is an IEC universal outlet. This allows you to control the pump using the Sentry 2.0. The voltage, phase and frequency of the vacuum pump must match the voltage, phase and frequency specified on the rear panel of the freeze dryer.
Installation and Setup VirTis BenchTop 2K, 4K and 6K Freeze Dryer Setup To set up your BenchTop unit: Note: Refer to Basic Operation for complete equipment operation instructions. 1. Install a condenser gasket (black rubber ring with a slit in it) on the top of the unit. It should have a light film of vacuum grease on the outer surface. 2. Prepare the unit for your intended use. a.
VirTis BenchTop 2K, 4K and 6K Installation and Setup Vacuum Baffle Plate The BenchTop 2K and 4K models include a two-position vacuum baffle plate. • Baffle Plate on Chamber Bottom (Position 1). By raising the baffle plate handle, the plate can be dropped to the bottom of the chamber. This allows you to pre-freeze items on the baffle plate. In some cases, it may be more convenient to remove the baffle plate completely and freeze items directly on the bottom of the chamber.
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Chapter Freeze-Drying Concepts 3 The first step of lyophilization (freeze-drying) is typically to freeze the product to a minimum of -40 °C. After the product is frozen, moisture can be extracted through sublimation. The sublimation process takes a solid (i.e., ice) and converts it to a gas (i.e., vapor), bypassing the liquid stage. The moisture is converted to a gas, while maintaining the material’s crystalline structure. The second step involves the migration of moisture from the product.
Freeze-Drying Concepts VirTis BenchTop 2K, 4K and 6K Heat Carefully controlled heat input to the frozen product speeds the drying process. The BenchTop unit is designed to be used as either a manifold freeze dryer or a tray dryer. Exposing glassware containing frozen product to ambient room temperature helps drive the drying process by adding heat. This causes the frozen solvents in the product to sublimate and then migrate to the colder surface of the condenser wall.
Chapter Sentry 2.0 Controls 4 The Sentry 2.0 is the control center for the BenchTop K series. Driven by a powerful microprocessor, the Sentry 2.0 is extremely versatile while remaining intuitively easy to use. The controller allows custom programming, includes a detailed LCD display and offers a wealth of customizable features. The Sentry 2.0 front panel consists of the following: • An LED wave display, which allows you to assess the status of the system quickly and easily.
Sentry 2.0 Controls VirTis BenchTop 2K, 4K and 6K 2. Vacuum The LEDs on the top wave represent the following vacuum setpoints: LED Vacuum (mTorr) Color 1 2000 Red 2 1000 Red 3 500 Amber 4 200 Amber 5 100 Green 6 50 Green 7 ≤ 20 Green Button Functions Up/Down (+/-) Buttons The Up/Down (+/-) buttons allow you to navigate the menus and increase or decrease setpoint values displayed on the LCD display. MENU Button The MENU button performs a number of functions.
VirTis BenchTop 2K, 4K and 6K Sentry 2.0 Controls LCD Display Functions By default, the LCD display shows the system Synoptic screen. The Synoptic screen gives a visual representation of the current operation and status of the unit. Alarm messages, run time and system status are displayed. Note: The actual synoptic screen may vary slightly from the illustration above. Main Menu Pressing the MENU button while on the Synoptic screen displays the Main Menu.
Sentry 2.0 Controls VirTis BenchTop 2K, 4K and 6K The ∧ symbol, located in the upper left corner of the screen, returns you to the previous screen. The > symbol allows you to go to the next screen within a selected option. Vacuum Control The Vacuum Control field displays the current vacuum level control setpoint. To change the setpoint, use the Up/Down (+/-) buttons and navigate to the Vacuum Control field. Press and hold the MENU button. When prompted, use the Up/Down (+/-) buttons to adjust the value.
VirTis BenchTop 2K, 4K and 6K Sentry 2.0 Controls Temperature Units The Temperature Units field displays the current setting for indicating temperature values. Temperature can be displayed in either Fahrenheit (°F) or Celsius (°C). Vacuum Units The Vacuum Units field displays the current setting for indication of system pressure. System pressure can be displayed in millitorr (mTorr), microbar (μbar) or Pascal (Pa).
Sentry 2.0 Controls VirTis BenchTop 2K, 4K and 6K Alarms Menu The Alarms screen displays all active alarms. A shaded box appears in front of triggered, active alarms. You can also accept and clear triggered alarms from this screen. To clear an alarm, use the Up/Down (+/-) buttons to highlight the desired alarm and press the MENU button. Before the alarm will clear, the condition that caused the alarm must be resolved.
VirTis BenchTop 2K, 4K and 6K Sentry 2.0 Controls Maintenance Menu and Factory Options The Maintenance menus are used for system configuration, calibration and factory setup. Use caution when modifying factory settings. PROPERTY CAUTION! ENABLING FEATURES THAT ARE NOT INSTALLED MAY CAUSE SERIOUS SYSTEM DAMAGE AND VOID YOUR WARRANTY. ONLY A QUALIFIED SP INDUSTRIES TECHNICIAN SHOULD EDIT VALUES IN THE FACTORY OPTIONS AND INTERSTAGE CONTROL SCREENS.
Sentry 2.0 Controls VirTis BenchTop 2K, 4K and 6K Interstage Control If your unit is equipped with a cascade refrigeration system, you can control the operation of the second compressor from the Interstage Control screen. A cascade system is a safety feature used to protect the refrigeration system from overloading. ∧ Interstage Control Interstage ON –12 ON DIFF 025 Current Temp 1.3 °C If the Interstage Control is set to ON, the COND or AUTO buttons will activate the high-stage compressor.
VirTis BenchTop 2K, 4K and 6K Sentry 2.0 Controls Vacuum Value To adjust the Vacuum value, open the condenser door and adjust the trim pot located on the main Sentry 2.0 module within the electrical box. Set the value to 760 Torr, or current atmospheric pressure. Turn the trim pot clockwise to increases the pressure or counter-clockwise to decrease the pressure. Once the rough vacuum has been set, connect a reference tube.
Sentry 2.0 Controls 20 VirTis BenchTop 2K, 4K and 6K Revision 004, 12/09 © SP Industries, Inc.
Chapter Basic Operation 5 Getting Started Prior to operating your freeze dryer, ensure that your condenser is clean and dry. If your unit is equipped with a shelf rack with stoppering, check that the stoppering mechanism is fully retracted before proceeding. Product Preparation: Flask / Manifold Drying BenchTop series units include Quickseal valves for processing samples using flasks or other glassware. To prepare samples for freeze-drying in glassware: 1. Fill flasks with your product.
Basic Operation VirTis BenchTop 2K, 4K and 6K Product Preparation: Chamber Drying BenchTop series freeze dryers can process product in vials or trays directly in the condenser chamber. To process samples in the chamber: 1. Fill tray(s) or vials with your product. 6 Do not exceed more than half of the container’s total capacity. 2. If using a BenchTop 2K or 4K, ensure that the vacuum baffle plate is in the desired position (i.e., position 1 for pre-freezing or position 2 for freezedrying). 3.
VirTis BenchTop 2K, 4K and 6K Basic Operation Operation Instructions 1. Ensure that the condenser is clean and dry before proceeding. Check the drain line for residual moisture, which can cause slow vacuum pump-down. Ensure that the plastic quick-connect drain fitting is not inserted into the drain fitting receptacle on the front of the unit. 2. Pre-freeze the product to a minimum of -40 °C. 3.
Basic Operation VirTis BenchTop 2K, 4K and 6K a. The condenser approaches its maximum low temperature. b. System vacuum approaches a constant low pressure reading. c. Product temperature is steady and close to shelf temperature (requires use of a product probe). d. Appearance of the product indicates the dryness (i.e., uniformly powdery or fluffy). e. The product probe reads near ambient temperature or the temperature of the heated rack (if equipped with that option). 10.
VirTis BenchTop 2K, 4K and 6K Basic Operation Preventing Glassware Breakage • Avoid cleaning glassware with a wire brush as metal-to-glass abrasion creates microscopic scratches which can cause breakage. • Never fill a flask to more than half of its total capacity (e.g., a 600 mL flask has a working capacity of 300 mL). • When pre-freezing samples in a storage freezer, tilt glassware at a 30° to 45° angle to increase surface area and reduce stress on the glass.
Basic Operation 26 VirTis BenchTop 2K, 4K and 6K Revision 004, 12/09 © SP Industries, Inc.
Chapter Cold Trap Condenser 6 Under conditions of high vacuum, vapor pressure of the solvent collecting on the condenser is much lower than that of the product. When vapor molecules leave the product in a vacuum concentrator, they migrate toward low-pressure areas in the condenser. Upon contact with the condenser, the vapors release their heat energy and condense. Whether or not ice forms is dependent on the chemical properties of the solvent.
Cold Trap Condenser VirTis BenchTop 2K, 4K and 6K Cold Trap Setup The following instructions will help you utilize your BenchTop as a cold trap to condense vapors from a gel dryer or vacuum concentrator: 1. Position the vacuum concentrator, BenchTop and vacuum pump in a convenient location with sufficient space to easily connect the units. 2. Place the vacuum cover plate (acrylic plate with stainless steel elbow) on the gasket of the BenchTop unit. 3.
Chapter Optional Components 7 The VirTis BenchTop series offers a wide variety of optional components to match a variety of product or process applications. Manifolds Many manifolds are available for BenchTop units. Optional manifolds include VirTis ¾-inch (19 mm) Quickseal valves for attaching a variety of flasks, ampoules or vials.
Optional Components VirTis BenchTop 2K, 4K and 6K Shelf Racks VirTis BenchTop units have a variety of shelf racks available for use with the optional stainless steel and acrylic drum manifolds. Racks are available in both heated and unheated configurations. Stoppering racks are also available. Available rack assemblies include: • Stoppering shelf rack with 1, 2, or 3 shelves available with heated or nonheated shelves (for use with acrylic drum manifolds only).
VirTis BenchTop 2K, 4K and 6K Optional Components Liquid Nitrogen Trap The optional Liquid Nitrogen (N2(liq)) Trap protects your vacuum pump from the corrosive properties of acid and alkaline vapors, as well as the low temperatures and organic solvents associated with the freeze-drying process. The trap is available in both 2.8- and 5-liter capacities. To Vacuum Pump To Condenser Vacuum bypass assembly with lever-activated ball valves To operate a liquid nitrogen trap: 1.
Optional Components VirTis BenchTop 2K, 4K and 6K Filter Trap VirTis filter traps protect your vacuum pump from damaging and corrosive vapors released during freeze-drying. If purchased, the filter trap is located on the side of your freeze dryer, near the vacuum pump. Disposable Sodasorb and activated charcoal drop-in wire mesh cartridges are available and must be purchased separately. To install the filter trap: 1. Connect the vacuum pump to the port marked OUT. 2.
VirTis BenchTop 2K, 4K and 6K Optional Components BenchTop Cold Plate The optional BenchTop cold plate can be cooled to -40 °C within 30 minutes when fully insulated and covered. The cold plate will remain lower than -40 °C after the cover is removed. These specifications are based on SP Industries test data from similar units operating with no load. Initial Setup of the BenchTop Cold Plate Remove all packing materials carefully and inspect for shipping damage.
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Chapter General Maintenance 8 Proper routine maintenance is the key to an efficiently operating unit with minimal downtime. The following section provides instructions on how to maintain your BenchTop series freeze dryer. Vacuum System Vacuum Pump Clean oil is necessary for the best vacuum and overall efficiency of the system. Checking and changing the oil on a consistent basis will greatly extend the life of the vacuum pump.
General Maintenance VirTis BenchTop 2K, 4K and 6K Scheduling Oil Changes After clean oil is loaded into the vacuum pump and all necessary connections have been made between the vacuum pump and the freeze dryer, perform a full capacity test cycle. Have a qualified technician check the oil after the test cycle. If the oil appears dirty, change the oil after every use. If the used oil appears clean, change the oil after the next two uses or cycles.
VirTis BenchTop 2K, 4K and 6K General Maintenance Quickseal Valves VirTis BenchTop units come equipped with Quickseal valves. These valves should be serviced at least once a year. To service the Quickseal valves: 1. Remove the valves from their ports. 2. Twist and pull the white selector until it is dislodged from the black rubber body. 3. Clean the valves thoroughly with isopropyl alcohol to remove grease and dirt. 4. Inspect each cleaned selector carefully for damage.
General Maintenance VirTis BenchTop 2K, 4K and 6K Condenser Chamber The condenser is fabricated from stainless steel. Under normal use, it can be rinsed and kept clean with a mild detergent. If corrosive materials are being freeze-dried, thoroughly clean and rinse all parts of the freeze dryer that come in contact with product vapor. This prevents build-up of corrosive materials, which protects the freeze dryer and subsequent product loads.
Appendix Appendix A: Troubleshooting A Vacuum Problems Remember that maximum vacuum is only achievable with a clean, dry system. Initial vacuum will be affected by the amount of product loaded on the unit. For efficient freeze-drying, vacuum should be below 200 mT. When using Quickseal valves, product may need to be introduced in stages to keep the vacuum below acceptable levels.
Appendix A: Troubleshooting VirTis BenchTop 2K, 4K and 6K If none of these suggestions eliminate the vacuum problem: 1. Change and flush the oil in vacuum pump. 2. Disassemble all vacuum tubing connections, clean with a mild alcohol (such as methanol), apply a light coating of vacuum grease and reassemble. 3. Check all threaded and welded connections and seal with vacuum sealant.
Appendix Appendix B: Serum Vial Capacities VirTis Part Number 8 Body OD (mm) Capacity (mL) 9 35 179275 10 85 12 2 179101 9 40 22 6 47 23 5 179077 179085 179143 9 18 2 50 23 10 54 26 10 62 28 20 178830 58 33 20 178897 63 37 30 178921 73 43 50 178954 95 52 100 178988 107 54 125 179135 178855 9 8 Add 8mm for partially inserted stopper. 9 Thin Wall. 10 Height (mm) B Special Stoppering Ampoule (add 10mm for partially inserted stopper).
Appendix B: Serum Vial Capacities 42 VirTis BenchTop 2K, 4K and 6K Revision 004, 12/09 © SP Industries, Inc.
Appendix Appendix C: Stainless Steel Cleaners C The following table lists possible problem situations and suggests corrective actions. For additional information, contact SP Industries. Cleaning Required HEAT TINT OR HEAVY DISCOLORATION. TENACIOUS DEPOSITS, RUSTY DISCOLORATIONS, INDUSTRIAL ATMOSPHERIC STAINS. HARD WATER SPOTS AND SCALE. Cleaning Agent 11 Application Method 12 Effect on Finish Penny-Brite or Copper-Brite Use in direction of polish lines on No.4 (polished) finish.
Appendix C: Stainless Steel Cleaners 44 VirTis BenchTop 2K, 4K and 6K Revision 004, 12/09 © SP Industries, Inc.
Appendix Appendix D: Spare Parts List D Refer to the following list for commonly used parts. 2K 4K 6K X X X 153650 Vacuum probe tube 10324pt.
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