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SP INDUSTRIES, INC. 

Freeze Dryer Operator's Manual 

 

 

VirTis BenchTop 2K, 4K and 6K

 

Freeze Dryers 

 

 

Summary of Contents for VirTis BenchTop 2K

Page 1: ...SP INDUSTRIES INC Freeze Dryer Operator s Manual VirTis BenchTop 2K 4K and 6K Freeze Dryers ...

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Page 3: ...orks from this Freeze Dryer Operator s Manual by any means and in any form or manner is expressly prohibited except with the prior written permission of SP Industries Inc Permitted copies of this document must retain all proprietary notices contained in the original The information in this document is subject to change without prior notice Always confirm with SP Industries Inc that you are using t...

Page 4: ...cuum and electrical systems 9 Always ensure that refrigeration air intake is clear and clean 9 Always ensure vacuum pump exhaust is properly ventilated and or contained 9 Always practice team lifting when moving heavy equipment 9 Always use a maximum one pound regulator if backfilling from an inert gas source 9 Always wear safety glasses when using glass flasks 9 Do carefully read the entire instr...

Page 5: ...any employees Replacement or repair of parts pursuant to this warranty shall not in any way extend the original warranty period The Company will not be responsible for any unauthorized repairs replacements or product modifications nor will it be responsible for any product failures resulting from such unauthorized repairs replacements or product modifications negligently or otherwise made by perso...

Page 6: ...iv Revision 004 12 09 SP Industries Inc 2009 ...

Page 7: ...ation 4 Installing the Vacuum Pump 4 Oil Mist Eliminators 5 Freeze Dryer Setup 6 Vacuum Baffle Plate 7 Freeze Drying Concepts 9 Elements of Freeze Drying 9 Freeze 9 Vacuum 9 Heat 10 Condenser 10 Product Dependencies 10 Sentry 2 0 Controls 11 LED Wave Display Qualitative Reference 11 Button Functions 12 Up Down Buttons 12 MENU Button 12 COND Button 12 VAC Button 12 AUTO Button 12 DEFR Button 12 LCD...

Page 8: ...ess End Point 25 Stoppering Optional 25 Cold Trap Condenser 27 Product Requirements 27 Cold Trap Setup 28 Optional Components 29 Manifolds 29 Shelf Racks 30 Liquid Nitrogen Trap 31 Filter Trap 32 BenchTop Cold Plate 33 Initial Setup of the BenchTop Cold Plate 33 Cold Plate Operation 33 General Maintenance 35 Vacuum System 35 Vacuum Pump 35 Changing Vacuum Pump Oil 35 Vacuum Tubing and Gaskets 36 D...

Page 9: ...VirTis BenchTop 2K 4K and 6K Contents Revision 004 12 09 vii SP Industries Inc 2009 Appendix D Spare Parts List 45 ...

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Page 11: ...hree to nine liter condenser capacity Variety of refrigeration system options Digital display of temperatures and setpoints Quickseal valves for processing flasks 1 Manual shelf stoppering optional BenchTop Usage BenchTop units are mechanically refrigerated condenser modules that can be utilized as freeze dryers or cold traps These versatile units can also be used for initial product freezing When...

Page 12: ...ith either a inch stainless steel port for the manifold plate or a plain cover plate which must be purchased separately if no manifold is ordered The manifold adapter plate is required when any manifold is purchased Cold Trap Condenser Module When using a vacuum concentrator or gel dryer with your BenchTop unit the condenser module can be used as a cold trap which traps vapors driven off of the pr...

Page 13: ... you making them a part of your claim Service Connections Make sure that the outlet you intend to use meets the voltage and amperage requirements listed on the serial tag of your unit CAUTION ONLY A QUALIFIED ELECTRICIAN SHOULD CONNECT THE UNIT TO THE AVAILABLE ELECTRICAL SUPPLY The line cord has three individual conductors inside the outer jacket 2 To make the appropriate plug connection 1 Trim b...

Page 14: ...e pump will be easily accessible during routine maintenance 2 Cut the supplied vacuum tubing as short as possible Allow enough length between the vacuum pump and the BenchTop unit Note Clamp and cut the inch ID vacuum hose If you do not wish to cut the hose it may be used at its full length but may take up more space than necessary 3 Locate the inlet port on your vacuum pump Refer to the vacuum pu...

Page 15: ...pump from a wall socket if it does not have an IEC connector but you will not be able to control the pump from the Sentry 2 0 Controller Only a qualified electrician should perform installation of an IEC connector The pump used should not exceed the amperage listed on the BenchTop serial tag 11 Enable power to the vacuum pump by switching the pump s circuit breaker to the on position Oil Mist Elim...

Page 16: ...a second condenser gasket around the bottom lip of the manifold BenchTop with acrylic manifold d If you are using a stainless steel manifold place the supplied O ring in the groove of the manifold adapter plate 3 If using a manifold attach Quickseal valves to each port on the manifold and ensure that each is in the closed position For more information refer to the Quickseal valve section in Chapte...

Page 17: ...be more convenient to remove the baffle plate completely and freeze items directly on the bottom of the chamber Note Freeze drying cannot be performed with the baffle on the chamber bottom position 1 since the vacuum port will be blocked and the product will remain too cold for water vapor transfer Baffle Plate in Raised Position Position 2 Lower the baffle plate handle to raise the baffle plate w...

Page 18: ...Installation and Setup VirTis BenchTop 2K 4K and 6K 8 Revision 004 12 09 SP Industries Inc 2009 ...

Page 19: ...to attract product moisture Many products require a secondary drying process to remove moisture that did not convert to vapor during the first process During secondary drying BenchTop units remove the remaining bound moisture by slightly warming the product Note To prevent meltback the product should not be warmed above its eutectic point until all free ice has sublimated Elements of Freeze Drying...

Page 20: ...n through the acrylic cover Condenser Trapping water vapor molecules in the form of ice on the condenser surface effectively removes moisture from the product The refrigeration system cools the internal condenser at the bottom of the chamber to attract and trap vapors migrating off the product The condenser is located under the manifold to provide the shortest vapor path to achieve the maximum dry...

Page 21: ... display which allows you to assess the status of the system quickly and easily Tactile buttons located on the membrane which allow you to activate specific functions and navigate through the menus within the LCD display An LCD display which shows the status of the unit and allows you to adjust the alarm and control parameters as well as modify system configurations LED Wave Display Qualitative Re...

Page 22: ...corner of the LCD screen and press the MENU button COND Button The COND button activates the refrigeration system This provides system cooling for vapor condensing VAC Button The VAC button enables the vacuum pump and opens the vacuum brake solenoid VBS valve allowing the system to be evacuated Vacuum level control options can be programmed from the User Options screen Note If your vacuum pump is ...

Page 23: ...splays the Main Menu If Main Menu M Pr the unit goes idle no input after three minutes the system will default back to the Synoptic screen User Options Alarms Setpoints Vacuum Control 0000 Purge Off Bath Off Heat Off Note Tem are disabled except when the Synoptic avigation within the menu screens is accomplished using the Up Down arrow perature and vacuum control functions screen is displayed Bath...

Page 24: ...t function gives the ability to add controlled heat to product shelves for enhanced drying If installed you can set the temperature of the manifold shelves up to 60 C Note Optional features will only be displayed if the factory installed options were purchased with your unit User Options Menu To access the User Options menu highlight User Options from the Main Menu and press the MENU button User O...

Page 25: ...tton and each of the outputs of the selected relay bank will fire for approximately two seconds each Relay positions preceded by a highlighted box indicate the output is active Vacuum Pump Maintenance The Vacuum Pump Maintenance screen is used to adjust vacuum maintenance alarm parameters and maintenance time durations Vacuum Pump Maintenance Alarm Setpoint 240 Current Hours 0000 min 007 The Alarm...

Page 26: ...tpoints Condenser Temperature 60 Vacuum OK 0500 Power Save Deadband 050 PRESS AND HOLD MENU BUTTON TO ADJUST Condenser Temperature The Condenser Temperature setpoint is the temperature at which the vacuum will energize in auto mode The Condenser Over Temperature alarm is also referenced from this value The alarm will be triggered when 1 the condenser temperature rises more than 10 C above the setp...

Page 27: ...ontrol Calibration Factory Options The Factory Options screen is used to configure the bath purge defrost and heat options Factory options Bath Option YES Purge Option YES Hot Gas Defrost YES Heat Option No ZL Defrost No The optional Heat and Purge components are enabled when set to YES This results in changes to the Main Menu and Synoptic screens adding control of these features Note The Heat and...

Page 28: ...emp recovers Calibration The Calibration screen allows modification and control of condenser temperature and vacuum settings The following procedures require removal of the electrical box cover under the unit s right side panel CAUTION REMOVAL OF THE ELECTRICAL BOX EXPOSES HIGH VOLTAGE COMPONENTS USE EXTREME CAUTION AND FOLLOW ELECTRICAL SAFETY PRACTICES Calibration Temperature Span 070 Temperatur...

Page 29: ... counter clockwise to decrease the pressure Once the rough vacuum has been set connect a reference tube Adjust the Vacuum value located on the LCD screen up to increase the Vacuum reading Adjust the Vacuum value down to decrease the Vacuum reading Note SP Industries recommends the use of a Varian Vacuum Reference Tube for vacuum calibration PRACTICAL OPERATING TIP ENSURE THAT THE GROUND WIRE IS FI...

Page 30: ...Sentry 2 0 Controls VirTis BenchTop 2K 4K and 6K 20 Revision 004 12 09 SP Industries Inc 2009 ...

Page 31: ...g As an alternative to using flasks you may use an optional drum manifold and shelves to dry vials of product To prepare samples for shelf drying Fill vials or other suitable containers with product 3 Do not fill containers to more than half of their total capacity Pre freeze product samples This can be accomplished directly on the shelves or in a laboratory freezer dry ice bath or shell bath free...

Page 32: ...of the container 7 4 Close and secure the chamber lid PRACTICAL OPERATING TIP TO MINIMIZE DRYING TIME ALWAYS FREEZE PRODUCTS IN AS THIN A LAYER AS POSSIBLE NEVER FILL A CONTAINER TO MORE THAN HALF ITS TOTAL CAPACITY Quickseal Valves Quickseal valves are utilized in many method of drying They permit the attachment of flasks for in vitro freeze drying They are also used to break vacuum after a cycle...

Page 33: ...low the system to proceed through the freeze drying process using the defined settings If using the AUTO function skip to step 8 6 Enable vacuum by pressing VAC Allow the system to evacuate the system Before proceeding confirm that the vacuum status light is green on the LED Wave display and that the desired vacuum level is displayed on the Synoptic screen Note If your vacuum pump is not connected...

Page 34: ...o the drain receptacle on the front of the unit To open the drain push the fitting into the drain receptacle To close the drain line press the small gray release button on the top of the receptacle The fitting will pop out Note The quick connect fitting must be removed prior to freeze drying or else the appropriate vacuum pressure will not be achieved 14 Once the ice has melted away from the conde...

Page 35: ...s the product ice inside the glassware gradually sublimes the frost on the outside of the glassware slowly recedes and eventually disappears By this point approximately 98 of product moisture has been removed You can assume drying is complete 1 moisture content when the exterior of the glassware is at room temperature Stoppering Optional The stoppering option applies pressure to partially inserted...

Page 36: ...Basic Operation VirTis BenchTop 2K 4K and 6K 26 Revision 004 12 09 SP Industries Inc 2009 ...

Page 37: ...ing this vapor pressure differential These migrating vapors can be pulled directly into the vacuum pump if condensation does not occur BenchTop series freeze dryers can be utilized as a Cold Trap Condenser Module to condense and collect vapors being driven out of a product in a vacuum concentrator Condensing the vapors prevents them from migrating to the vacuum pump and causing damage Product Requ...

Page 38: ...o easily connect the units 2 Place the vacuum cover plate acrylic plate with stainless steel elbow on the gasket of the BenchTop unit 3 Connect the BenchTop unit to the vacuum concentrator using inch tubing 4 Estimate the length of tubing required to adequately reach the back of the vacuum concentrator without any tension 5 If necessary cut the tubing to the proper length and secure both ends with...

Page 39: ...ertical manifolds are available for flask drying while stainless steel and acrylic drum manifolds are available for the versatility of both flask and shelf rack drying The top plug on acrylic drum manifolds is removable to allow for installation of an optional stoppering assembly Available manifolds include Stainless steel vertical manifolds with 4 8 12 or 24 ports Stainless steel drum manifolds w...

Page 40: ...ted configurations Stoppering racks are also available Available rack assemblies include Stoppering shelf rack with 1 2 or 3 shelves available with heated or non heated shelves for use with acrylic drum manifolds only Bulk processing shelf rack with 3 4 or 5 shelves available with heated for use with acrylic drum manifolds only or non heated shelves For more information about shelf racks and curre...

Page 41: ...stic cover from the stainless steel vessel and add a small amount of liquid nitrogen to the center well If adding liquid nitrogen from a tank use adequate ventilation to protect from gaseous vapors Note The liquid nitrogen will expand and bubble when it meets the warm center well Wear protective eyewear and gloves to avoid contact with skin 3 Replace cover and wait one minute 4 Open center well an...

Page 42: ...as filter trap cartridges vacuum pump down may take significantly longer Degassing is also necessary each time you change your filter trap cartridge Most filters need to be degassed overnight in order to allow proper vacuum to be established To degas the filter trap cartridge 1 Unscrew the clear polypropylene housing from the white plastic top 2 To begin degassing enable the vacuum pump open the g...

Page 43: ...e hose between the plate and the unit is very flexible and can also be inserted into the rear of the unit approximately 10 inches so that the length can be adjusted 2 Verify the outlet you intend to use provides the same voltage and ampacity listed on the serial tag of your unit i e 100 115 Volts 15 Amps 60Hz 3 Verify the shelf thermocouple probe is inserted into the well at the rear of the cold p...

Page 44: ...Optional Components VirTis BenchTop 2K 4K and 6K 34 Revision 004 12 09 SP Industries Inc 2009 ...

Page 45: ...ination Cloudy gray vacuum pump oil indicates water contamination Changing Vacuum Pump Oil Change the oil immediately after shutting down the freeze dryer while the oil is still hot 1 Protect your hands from the hot oil 2 Make sure vacuum is released from the system 3 Remove the top fill plug and open the drain valve located at the bottom of the pump Drain the contaminated oil into a suitable cont...

Page 46: ...removed routinely and inspected for cracks To check the condenser gasket 1 Remove the condenser gasket 2 Take the gasket in both hands and turn it inside out 3 Inspect the inside of the gasket This is where you are most likely to find a potential problem 4 If you find the slightest inconsistency in the surface of the material e g cuts cracks dry rot rippling replace the gasket as soon as possible ...

Page 47: ...igeration System The Air Cooled Condenser It is very important to keep the air cooled condenser clean This is where high pressure vapor from the compressor is converted to liquid refrigerant by rejecting the heat gained from the vapor condenser into the ambient air Reduced airflow over the condenser can result in severely reduced performance and may shorten the life of the compressor To maintain t...

Page 48: ... Oil R Ammonium Chloride Saturated R Formaldehyde 40 R Phenol Solution 5 N Ammonium Hydroxide 10 R Gasoline Regular Leaded LR Soap Solution Ivory R Ammonium Hydroxide Conc R Glycerine R Sodium Carbonate 2 R Aniline N Heptane R Sodium Carbonate 20 R Battery Acid R Hexane Commercial Grade R Sodium Chloride 10 R Benzene N Hydrochloric Acid N Sodium Hydroxide 1 R Benzyl Alcohol N Hydrofluoric Acid 40 ...

Page 49: ...good condition Is a light coating of vacuum grease visible on the valve plug and on the stainless steel valve port Is the vacuum pump oil clean and at the proper level Check sight glass Is the condenser maintaining the proper temperature If the temperature rises due to refrigeration problems moisture may be leaving the condenser walls and migrating to the vacuum pump causing poor vacuum If none of...

Page 50: ... a good vacuum reading the problem is likely related to the vacuum probe Replace the vacuum probe tube and retest Note If this does not resolve your vacuum problem contact SP Industries for assistance Product Melting The most common reason for product melting is poor vacuum Adequate vacuum is required to keep products in a frozen state Check for a vacuum leak or possible restrictions in the vacuum...

Page 51: ...pacity mL 179077 9 35 18 2 179275 10 85 12 2 179101 9 40 22 6 179085 47 23 5 179143 9 50 23 10 179135 54 26 10 178855 9 62 28 20 178830 58 33 20 178897 63 37 30 178921 73 43 50 178954 95 52 100 178988 107 54 125 8 Add 8mm for partially inserted stopper 9 Thin Wall 10 Special Stoppering Ampoule add 10mm for partially inserted stopper ...

Page 52: ...Appendix B Serum Vial Capacities VirTis BenchTop 2K 4K and 6K 42 Revision 004 12 09 SP Industries Inc 2009 ...

Page 53: ...f polish lines on No 4 polished finish May scratch No 2 mill and Nos 7 and 8 polished finishes TENACIOUS DEPOSITS RUSTY DISCOLORATIONS INDUSTRIAL ATMOSPHERIC STAINS Oakite No 33 Dilac Texo 12 Texo N Y Flash Klenz Caddy Cleaner Turco Scale 4368 or Permag 57 Swab and soak with clean cloth Allow to stand 15 minutes or more per directions on package Then rinse and dry Satisfactory for use on all finis...

Page 54: ...Appendix C Stainless Steel Cleaners VirTis BenchTop 2K 4K and 6K 44 Revision 004 12 09 SP Industries Inc 2009 ...

Page 55: ... 266783 Molecular Sieve Cartridge for water vapor X X X 272310 Free Standing Filter Trap X X X 277228 One liter of synthetic oil X X X 354506 Drain hose clear tubing 36 inches recommended X X X 356808 90 degree rubber elbow for vacuum port connection to vacuum pump tubing X X X 357699 High Vacuum grease 10 each 5 oz tubes X 364604 Circuit breaker 10 Amp ES X 366658 Oil Separator XL X X X 367424 Pl...

Page 56: ...SP Industries 3538 Main Street Stone Ridge NY 12484 USA www SPIndustries com 800 824 0400 845 687 0071 ...

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