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User`s Manual - BME Shared Lab Resource

1. Material Solidification Eutectic Pre Freeze Vacuum Set Point Temperature Temperatures Bacteria Virus 40 C and Colder 50 C amp 0 040 mBar amp Colder Lower Milk 5 to 13 15 to 23 1 65 to 0 77 Fungi 40 and Colder 50 amp Colder 0 04 and lower Vegetable Tissue 25 to 50 35 to 60 0 22 to 0 01 Human Tissue 30 to 40 40 to 50 0 12 to 0 04 Blood Plasma 10 to 25 20 to 35 1 03 to 0 22 Vaccine 30 to 40 40 to 50 0 12 to 0 04 Pre Freezing Samples Appropriate containers for freeze drying include ampules serum bottles and wide mouth freeze drying flasks Shell freezing of samples is recommended for wide mouth freeze drying flasks Smaller samples in ampules and serum bottles may be frozen in a freezer The sample container size should always be at least two to three times the sample size 1 e 40 ml samples should be prepared in 80 ml containers or larger The temperature required for pre freezing 1s dependent on the characteristics of the sample Pre freezing temperature typically is at least 10 to 20 C below the eutectic or collapse temperature of the sample Adding Sample The following procedure should be followed when using sample valves in the freeze dry process 1 Connect a pre frozen sample to a sample valve on the drying chamber or manifold using an adapter Turn the plastic valve knob to the VACUUM position to open the valve The bevel on the knob should be positio
2. a0 e y _ n gp iom Shipping weight 1 Ib 0 4 kg 2ml 7575000 7576010 7577010 Stoppering Adapter Body Serum Bottle 3 ml 1515210 7516010 7511010 Sml 7573010 7576210 T5TTMO 1577510 Valve Port N l ml 7522210 7576210 7577110 7577510 P Xm 752410 T7620 T5770 7575510 EL Wmi 752610 7576210 7577110 7577510 50ml 7573810 7576210 7577110 7577510 100ml 7574010 7576210 7577110 7577510 125ml 7574210 7576210 757100 757510 Vent Hole Ejector Tube 60 Product Service Domestic 1 800 522 7658 International 816 333 8811 Ampules Labconco Ampules are fabricated of highest quality borosili cate glass for strength and durability They are available in five different configurations to provide the ideal ampule for your specilic lyophilization requirements from tray drying to flame sealing applications Ampules Ampules are supplied in packages of 100 Size Straight Bulb Type Pre Scored Round Stoppering Flat Bottom Bottom 2ml 7570810 751240 5ml 7500210 7571010 25ml 7571810 Appendix D Freeze Dryer Accessories Oxygen Natural Gas Sealing Torch 7578500 Torch specifically designed for flame sealing freeze dry ampules Seals all types of heat resistant glass Connects to natural gas butane or propane and oxygen with 1 4 ID hose connectors Shipping weight 3 lbs 1 4 kg Ampule Valve Adapters 7593401 Adapter connects ampules to valve ports or s
3. Appendix D Freeze Dryer Accessories Serum Bottles amp Vials Threaded Vials Stoppers and Threaded Vials with Screw Caps are supplied in packages of 200 a ee ll Ji Size Vials with Stoppers Screw Caps 5ml 7162300 7762200 10 ml 7762600 7762200 ET Accessories Perfect for long term storage of freeze dried samples Labconco Serum Bottles and Threaded 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 Serum bottles also connect to valve Seal Crimper ports on drying chambers and manifolds Secures tear away Aluminum Seals Serum Bottles 7578000 Seal Crimper for 13 mm corkage Serum Bottles Stoppers and Seals are supplied in pack Shipping weight 3 Ibs 1 4 kg ages of 100 7578100 Seal Crimper for 20 mm corkage Shipping weight 3 Ibs 1 4 kg Vacuum Stoppering Adapter 7593000 Adapter connects to valve ports for manual stop pering of 20 mm corkage serum bottles under original vacu um The stopper and serum bottle are inserted into the adapter body and lyophilization begins After the process is completed the researcher slides the stopper into position so when the valve is turned from vacuum to vent the serum bottle is tightly sealed by the stopper The ejector tube is then used to force the serum bottle out of the adapter
4. 17 7432700 Vacuum Control Bleed Valve 18 7429700 Moisture Sensor 19 7418400 Wire Harness Control 115V and 230V Not Shown 20 1289320 Circuit Breaker 115V 20A 1289310 Circuit Breaker 230V 10A 21 1289200 Relay Vacuum Pump 115V 1289100 Relay Vacuum Pump 230V 22 1289200 Relay Refrigeration Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix A Freeze Dryer Components GG RH ACUTU m rad he ti VT Ca AES QV Ww Product Service Domestic 1 800 522 7658 International 816 333 8811 49 APPENDIX B FREEZE DRYER DIMENSIONS INCHES ICENTIMETERSI ge eee ru vn HH HBM MM Mr H M M a s Iam I XXX M Hmmm 50 Product Service Domestic 1 800 522 7658 International 816 333 8811 APPENDIX C FREEZE DRYER SPECIFICATIONS This Appendix contains technical information about the Freeze Dryer including electrical specifications and environmental operating conditions Electrical Specifications Catalog Voltage Frequency Phase Amperage Nominal Max with i Operating wio Nominal Vacuum Range Vacuum Pump Pump 7752020 115V 103 127 60 1 9 16 100V 90 110 50 1 9 16 7752021 115V 103 127 60 1 9
5. User s Manual FreeZone 6 Liter Benchtop Freeze Dry Systems Models 77520 Series To receive important product updates complete your product registration card online at register labconco com Protecting your y aN laboratory environment J LABCONCO 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 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 The warranty includes areas of defective material and workmanship provided such defect results from normal and proper use of the equipment The warranty for all Labconco products will expire one year from date of installation or two years from date of shipment from Labconco whichever is sooner except the following e Purifier amp Logic Biological Safety Cabinets and PuriCare Lab Animal Research Stations carry a three year warranty from date of installation or four years from date of shipment from Labconco
6. The FreeZone Freeze Dry System is designed to be chemically resistant to most compounds that are commonly used in freeze drying processes However by necessity the freeze dryer is comprised of a number of different materials some of which may be attacked and degraded by certain chemicals The degree of degradation is dependent on the concentration and exposure duration Some of the major components of the FreeZone Freeze Dry System that are susceptible to degradation are as follows Acids Buffers Solvents z 2 5 E o bud 3 5 E o 8 S S z i 2 z E E s amp 2 T a x D A E E o 5 S 5 a oO v E ta So 4 6 CY E B x gu Lug eges B g 2 97 8 Z 82 5 2 z e m B8 E 5 2 8g 8S 6 S 8 8 o p 3 5 o o e o z o7 uu 9 e pen S e 9 9 b Pa om z gt Component Material AS ome Rev EM E Valve Stem Acetal C D OD D D Collector Acrylic D D D D Lid Hoses Neoprene C D D C C D D D C D Gaskets amp Valve Bodies Flask Top Silicon C D D D D D C D Rubber Chamber amp Stainless C Fittings Steel An accessory glass lid is available C Moderate degradation Limited use D Severe degradation infrequent use recommended immediate thorough cleaning required 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 o
7. collector warms above safe limits when the power is restored the Freeze Dryer will not automatically restart This prevents melted sample from being drawn into the collector and prevents liquid from being sucked into the vacuum pump When power is restored the alarm indicator will flash and the alarm beeper will sound When the MENU button is pressed the display will show POWER FAIL HOLD SELECT TO CLEAR IT Press and hold SELECT for five seconds until the error message is cleared from the display Product Service Domestic 1 800 522 7658 International 816 333 8811 25 Chapter 4 Using Your Freeze Dryer Line Voltage Out of Range If the voltage supplied to the Freeze Dryer varies beyond allowable limits the alarm will be activated When an alarm occurs press MENU and the display will show LINE VOLTAGE ERROR The alarm will self cancel when the proper voltage is restored The high and low alarm points are preset at the factory to correspond to the normal allowable voltage variations based on the nominal voltage specified for the freeze dryer Some models may be operated outside the normal voltage limits See Appendix C If necessary the high and low alarm points may be adjusted for these models See Chapter 6 Temperature Out of Range An alarm will be activated if the collector temperature rises above 40 C If this occurs the display will show COLLECTOR TEMPERATURE HOLD SELECT TO CLEAR IT Press and
8. 16 100V 90 110 50 1 9 16 7752030 230V 198 254 50 1 3 8 7752031 230V 198 254 50 1 3 8 7152040 230V 187 253 60 1 3 8 7752041 230V 187 253 60 1 3 8 7152060 230V 198 254 50 1 3 8 7752061 230V 198 254 50 1 3 8 7152070 230V 198 254 50 1 3 8 7752071 230V 198 254 50 1 3 8 Product Service Domestic 1 800 522 7658 International 816 333 8811 51 Appendix C Freeze Dryer Specifications Environmental Conditions Indoor use only Maximum altitude 6562 feet 2000 meters Ambient temperature range 41 to 104 F 5 to 40 C Maximum relative humidity 8096 for temperatures up to 88 F 31 C decreasing linearly to 5096 relative humidity at 104 F 40 C e Main supply voltage fluctuations not to exceed 10 of the nominal voltage e Transient over voltages according to Installation Categories II Over voltage Categories per IEC 1010 Temporary voltage spikes on the AC input line that may be as high as 1500V for 115V models and 2500V for 230V models are allowed e Used in an environment of Pollution degrees 2 i e where normally only non conductive atmospheres are present Occasionally however a temporary conductivity caused by condensation must be expected in accordance with IEC 664 Product Service Domestic 1 800 522 7658 International 816 333 8811 APPENDIX D FREEZE DRYER ACCESSORIES The following accessories are available for the Freeze Dryer PART DESCRIPTION 14
9. Introduction Typographical Conventions Recognizing the following typographical conventions will help you understand and use this manual e Book chapter and section titles are shown in italic type e g Chapter 3 Getting Started e Steps required to perform a task are presented in a numbered format e Comments located in the margins provide suggestions reminders and references e Critical information is presented in boldface type in paragraphs 1 that are preceded by the exclamation icon Failure to comply with the information following an exclamation icon may result in injury to the user or permanent damage to your Freeze Dryer e Important information is presented in capitalized type in S paragraphs that are preceded by the pointer icon It is imperative that the information contained in these paragraphs be thoroughly read and understood by the user Refer to Chapter 7 Troubleshooting if you are experiencing problems with your Freeze Dryer 6 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 2 PREREQUISITES Before you install your Freeze Dryer you need to prepare your site for installation Carefully examine the location where you intend to install your Freeze Dryer You must be certain that the area is level and of solid construction An electrical source must be located near the installation site Carefully read this chapter to learn e the electrical supply requirements
10. Lid For use with solvlents that attack the acrylic lid 7439902 Glass Collector Chamber Lid For use with solvlents that attack the acrylic lid 7509300 Product Heater For use in chamber 7522900 7444000 and 7867000 Provides 3 heated shelves operating at 43 C 110 F 115V 7509301 Product Heater For use in chamber 7522900 7444000 and 7867000 Provides 3 heated shelves operating at 43 C 110 F 230V 7509400 Product Heater with Variable Heat For use in chamber 7522900 7444000 and 7867000 Provides variable heat up to 43 C 110 F 115V Product Service Domestic 1 800 522 7658 International 816 333 8811 55 Appendix D Freeze Dryer Accessories 56 PART DESCRIPTION 7509401 Product Heater with Variable Heat For use in chamber 7522900 7444000 and 7867000 7806020 Bulk Tray Dryer 115V 60 Hz three shelves 630 square inches of area provides heat control 7806021 Bulk Tray Dryer 115V 60 Hz three shelves 630 square inches of area provides heat control with 6 port manifold 7806022 Bulk Tray Dryer 115V 60 Hz three shelves 630 square inches of area provides heat control with RS232 output connection 7806023 Bulk Tray Dryer 115V 60 Hz three shelves 630 square inches of area provides heat control with 6 port manifold and RS232 output connection 7806030 Bulk Tray Dryer 230V 50 60 Hz Three shelves 630 square in
11. MENU and the display will show VACUUM OFFSET O uBar Press SELECT until the appropriate offset is shown Each number represents 0 001mBar Press MENU and the display will show LOW LINE OFFSET Press SELECT until the appropriate offset is shown If the Freeze Dryer is operating on nominal 115V each number represents 2V If3 is entered into the display the low line alarm will alarm when the voltage drops to approximately 97V for example 103 2x3 97V If the Freeze Dryer is operating on nominal 230V each number represents 4V if 3 is entered into the display the low line alarm will alarm when the voltage drops to approximately 194V for example 206 4x3 194V There will be no alarm indicated if DISABLED is selected Press MENU and the display will show HIGH LINE OFFSET Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 8 Modifying Your Freeze Dryer Display Press SELECT until the appropriate offset is shown If the Freeze Dryer is operating on nominal 115V each number represents 2V If 3 is entered into the display the high line alarm will alarm when the voltage raises to approximately 133V for example 127 2x3 133V If the Freeze Dryer is operating on nominal 230V each number represents 4V if 3 is entered into the display the low line alarm will alarm when the voltage drops to approximately 266V for example 254 4x3 266V There will be no alarm indicated if DISABLED i
12. SERVICE HOUR to 0 press SELECT This allows you to keep track of the time the refrigeration system operated since it was serviced e The display will show the refrigeration system hours REFRIG TOTAL HOUR XXXX RESET SERVICE HOUR e To reset the service hours to 0 continue to hold SELECT 5 seconds until hours are reset TOTAL HOUR cannot be reset Press SELECT e The display will show the vacuum pump hours VACUUM TOTAL HOUR XXXX SERVICE HOUR XXXX Product Service Domestic 1 800 522 7658 International 816 333 8811 19 Chapter 4 Using Your Freeze Dryer e To reset the SERVICE HOUR to 0 press SELECT e The display will show VACUUM TOTAL HOUR XXXX RESET SERVICE HOUR If you want to reset the service hours to 0 continue to hold SELECT five seconds until hours are reset e Press SELECT e The display will show the RS 232 data transmission rate RS 232 TRANSMISSION RATE 10 SECONDS e To change the rate press and hold SELECT until the desired time interval is shown The time between data transmissions may be set to occur at 10 30 60 300 or 600 second intervals e Press SELECT to return to display operating parameters or after a short delay the display will automatically switch to show operating parameters Automatic Start Up To run the Auto Mode press the panel switch labeled REFRIGERATION AUTO The green LED above the switch will illuminate This will start the refrigeration sy
13. be used with the Freeze Dryer 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 It is recommended that the vacuum pump is equipped with an exhaust filter to minimize oil mist exhausting from the vacuum pump The operating vacuum level may be set on the Freeze Dryer The higher the pressure is set the more likely it is that oil mist will be exhausted Vacuum pumps used with 115V models should be equipped with an 115V 15 Amp NEMA 5 15P plug Vacuum pumps used with 230V models should be equipped with a reverse IEC plug This plug is included with 230V models This will allow the vacuum pump to be plugged into the receptacle on the back panel of the freeze dryer See Appendix D Freeze Dryer Accessories for vacuum pumps available from Labconco Chamber or Manifold Requirements A freeze drying chamber is not included and must be purchased separately These allow samples to be attached to the Freeze Dryer See Appendix D Freeze Dryer Accessories for available chambers and manifolds 8 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 3 GETTING STARTED Now that the site for your Freeze Dryer is properly prepared you are ready to unpack inspect install and test your Freez
14. 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 the Lyph Lock Flasks based on your sample sizes Flasks should be filled to no more than one third of their volume so that maximum surface area is achieved and effi cient lyophilization is ensured A complete Lyph Lock Flask includes a glass top and bottom and a rubber ring seal Tops bottoms and seals are available separately as replacement components Adapters are required to attach flasks to freeze dry valve ports Flask Complete Complete Flask Flask Lock Flask Dimensions Size Flask Top Top d Bottom Flask Bottom 1958ST 2440ST 1938ST 2040ST HxID 2ml 7550000 7554000 7552000 7556000 7559000 7557000 37mmr34mm 50ml 7550200 7554200 7552000 7556000 7559000 7557200 67mmx34mm 100ml 7550400 7554400 7552200 7556200 7559200 7557400 50mmx592mm Om 7550600 7554600 7552200 7556200 7559200 7557600 ll0mmx592mm 500m 7550800 7554800 7552400 7556400 7559400 7557800 l mmr902mm TS0ml 7550900 7554900 7552400 7556400 7559400 7557900 M45 mmx 902mm 1000m1 7551000 7555000 7552400 7556400 7559400 7558000 187mmx902mm Appendix D Freeze Dryer Accessories Borosilicate glass Compatible with adapte
15. by the collector in order to condense the water vapor In essence the freeze dry process is a balance between the heat absorbed by the sample to vaporize the Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction ice and the heat removed from the collector to convert the water vapor into ice 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 Table 1 SAFE TEMPERATURE AND DRYING TIMES FOR SELECTED MATERIALS Material Safe Collector Hours 10mm Thick Temperature Temperature Approx C Ke 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 Up to the point of overloading the system the greater the surface area of the sample the faster the rate of freeze drying By contrast for a given surface area the thicker the sample th
16. checking the sample valves pull as much vacuum as possible If a vacuum indication is displayed wiggle or rotate the valves and watch the gauge for any fluctuations Fluctuations can indicate a potential vacuum leak If the valve seems to be in good condition remove the valve and apply a thin coat of vacuum grease to the stem and the outside sealing surface of the valve body and reinstall the valve DO NOT APPLY VACUUM GREASE TO THE SAMPLE VALVE GASKETS WHICH SEAL TO THE WALL OF THE DRYING CHAMBER If the valve still seems to be the source of the problem remove the valve and stopper the hole with a rubber stopper Continue checking the other valves 36 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting 7 Make sure that the sample valve bulkhead nuts are tight Either tighten by hand or use the wrench supplied with chambers To use the wrench first remove the knob and stem assembly and also the valve body The pins on the wrench fit into the round holes of the nut The nut should be snug but avoid over tightening Replace the valve body knob and stem assembly The illustrations below show how the sample valve installs on a chamber and a manifold Knob amp Stem Valve Body Assembly Valve Assembly Clear Chamber with Valves Product Service Domestic 1 800 522 7658 International 816 333 8811 37 Chapter 7 Troubleshooting Manifold Assembly Valve Body Bulkh
17. dry valve ports See eee eee eee Flask Complete Flask Flask Flask Top Dimensions Size Flask Bottom Top Adapter Flask Bottom Diameter HxD 4 ml 7540000 7542000 7544000 1 2 76mm x 34 mm 0 ml 7540200 1542200 7544000 1 2 115 mm x 34 mm 120ml 7540200 7542200 7544200 3 4 68 mm x 59 2 mm 150ml 7540400 7542400 7544200 34 85 mm x 59 2 mm W0ml 7540600 7542600 7544200 3 4 145mm x59 2mm 600 ml 7540800 7542800 7544400 34 135 mm x 90 2 mm 900ml 7540900 7542900 7544400 3 4 190mmx90 2 mm 1200 ml 7541000 7543000 1544400 3 4 240 mm x 90 2mm 2000 ml 7541200 7543200 7544400 3 4 380 mm x 90 2 mm IM Valves om the reeze dry systenrs drybta Chambers and manifolds offered in this catalog fit adapters of both 1 2 and 3 4 sizes Size information is provided for selecting adapters for older Labconco mod els and other freeze dryers Variety of adapters available You may select from glass or stainless steel adapters available straight or with 45 bend Required order separately Top seals easily The flexible silicone rubber top snaps on and off easily yet provides a reliable high vacuum Compatible with all major brands of laboratory freeze dry apparatus No complex filter retainer is necessary For those who use filters they are easily inserted between the adapter and top of the flask One hun dred filters are sup plied with each flask say Pid es Wide mouth The complete o
18. e the vacuum pump requirements Refer to Appendix C Freeze Dryer Specifications for complete Freeze Dryer electrical and environmental conditions specifications and requirements Electrical Requirements The Freeze Dryer requires a dedicated electrical outlet This outlet requires a 20 Amp circuit breaker or fuse for models rated at 115V 60 Hz An outlet equipped with a 15 Amp circuit breaker or fuse is required for models rated at 230V 50 60 Hz The power cord on 115V models is equipped with a 20 Amp NEMA 5 20P plug Various power cord configurations are provided with 230V models If this does not match with the available receptacle remove this plug and replace it with an approved plug of the suitable style Product Service Domestic 1 800 522 7658 International 816 333 8811 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 rear and exhausts it through the sides 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 Refer to Appendix C Freeze Dryer Specifications for dimensional drawings of the Freeze Dryer The space for benchtop models must be large enough to accommodate the vacuum pump which will
19. hold SELECT for five seconds until the error message is cleared from the display Service Vacuum Pump The vacuum pump normally plugs into the vacuum pump electrical receptacle on the back of the Freeze Dryer When the Freeze Dryer has accumulated a total of 1000 operating hours the alarm indicator will flash Press MENU to display the alarm CHANGE VACUUM OIL HOLD SELECT TO CLEAR IT Press and hold SELECT for five seconds until the error message is cleared from the display This will reset the 1000 hour timer It may be necessary to service the vacuum pump more frequently than every 1000 hours depending on the operation of the Freeze Dryer The pump oil should be regularly monitored to verify that it is clean 26 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer Moisture in Collector If there is liquid in the collector chamber and either a REFRIGERATION button or the VACUUM button is pressed neither function will start and an alarm will be activated When MENU is pressed the display will show MOISTURE IN COLLECTOR When the collector is drained the alarm will self cancel This feature prevents the inadvertent start of the vacuum pump when liquid is in the collector and thereby can extend the life of the vacuum pump A few drops of liquid may remain in the drain hose after draining When the vacuum pump is started these drops may be sucked into the collector cham
20. is recommended Product Service Domestic 1 800 522 7658 International 816 333 8811 23 Chapter 4 Using Your Freeze Dryer Shut Down At the end of a run or when a sufficient amount of condensate accumulates on the collector coil to obstruct the flow of vapor to the collector chamber the Freeze Dryer should be defrosted First release system vacuum by turning the plastic knob on a valve to the open position or by pulling the collector chamber drain plug out of the drain hose Now press the Vacuum Switch on the control panel to turn the vacuum pump OFF Press the Refrigeration Switch next to the illuminated LED to turn OFF the refrigeration system Turn OFF the Main Power Switch on the left hand side of the cabinet Defrosting The following procedure should be followed when defrosting the collector coil 1 Pull the collector chamber drain hose out from the right hand side of the Freeze Dryer and remove the drain plug Place the drain hose in a suitable container to collect the condensate that will melt off the collector coil 2 Remove the collector chamber lid and allow ambient room air to melt the ice Dispose of the liquid appropriately Flush the collector chamber with water and wipe chamber dry 4 Ifrapid defrost is desired pour warm water over the collector coil Do not allow the liquid to enter the vacuum port on the upper rear of the chamber 5 Reinstall the drain hose plug and slide drain hose back into the si
21. pumps 1467700 and 7739403 1473200 Replacement Element Oil Mist Pump Exhaust Filter Fits pump exhaust filter 1473400 1473300 Replacement Element Odor Pump Exhaust Filter package of 5 Fits pump exhaust filter 1473400 or vacuum pumps 1467700 and 7739403 1988000 Vacuum Pump Oil 1 Liter A molecularly distilled hydrocarbon oil with low vapor pressure For vacuum pumps 1467700 and 7739403 7772000 Soda Acid Trap Secondary trap that prevents migration of corrosive chemicals into vacuum pump 7772100 Replacement Media for Soda Acid Trap 7584300 Vacuum Pump Oil 1 Liter For Hybrid vacuum pumps 7584000 7584002 7772500 Carbon Solvent Trap Secondary trap that prevents migration of organic solvents into vacuum pump 7772600 Replacement Activated Carbon Media for Carbon Solvent Trap 7538000 Secondary Vacuum Cold Trap Provides additional protection for the vacuum pump when processing low eutectic samples 9 34 high x 7 7 8 diameter 304 stainless steel with 3 4 vacuum connections For use with dry ice and solvent Cools to pproximately 75 C 7522800 12 Port Drying Chamber 9 24 high x 7 7 8 diameter 304 stainless steel with 12 freeze dry valves 7522900 16 Port Drying Chamber 13 high x 138 diameter 304 stainless steel with 16 freeze dry valves 7443500 Clear Drying Chamber with 8 Valves For bulk drying or drying in flasks 9 0 Dia 7444
22. status of the Stoppering Tray Dryer may be monitored simultaneously with the status of the Freeze Dryer Computer Connection for Computer Interface Check your computer to see which type of serial port is provided then use a connecting cable below 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 Dryer 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 Dryer The purpose of the RS232 interface is to send data to a data logging computer to monitor the state and activity of the Freeze Dryer This data is half duplex data The data properties are as follows Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 6 Using the RS232 Receptacle Data Rate 2400 Baud 8 Bit word length 1 Start bit 1 Stop bit No parity is transmitted Standard ASCII character set Urdu p rs 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 until the RS232 screen appears on the display RS 232 TRANSMISSION RATE 10 SECONDS Press select until the desired time interval is shown The format of the transmitted message is as follows B lt T 48 V 18 SF 999 C 999 PG 9 gt Where B Base Unit T Collector Temperat
23. 000 Clear Drying Chamber with 8 Valves For bulk drying or drying in flasks 12 0 Dia 7442900 Clearing Drying Chamber For bulk drying 9 0 Dia Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix D Freeze Dryer Accessories PART DESCRIPTION 7867000 Clear Drying Chamber For Bulk Drying 12 0 Dia 7509200 Product Heater For use in chamber 7522800 Provides 3 heated shelves operating at 43 C 110 F 115V 7509201 Product Heater For use in chamber 7522800 Provides 3 heated shelves operating at 43 C 110 F 230V 7442100 Drying Rack Unheated Provides three shelves For use in chambers 7443500 and 7522800 7441700 Drying Rack Unheated Provides three shelves for use in chambers 7444000 7867000 7522900 7522300 20 Port Manifold 10 high x 27 2 wide x 8 5 8 deep Type 304 stainless steel manifold with 20 freeze dry valves 7522400 10 Port Manifold with support shelf 10 high x 26 wide x 6 5 8 deep Type 304 Stainless Steel Manifold with 10 Freeze Dry Valves amp 1 Shelf 7522500 20 Port Manifold with support shelves 10 high x 26 wide x 9 1 2 deep Type 304 Stainless Steel Manifold with 20 Freeze Dry valves and 2 shelves 7868500 48 Port Ampule Manifold 28 5 8 high x 5 wide x 5 deep Type 304 stainless steel with 48 each 1 4 tube stems 7509600 Sample Valve Kit Includes neoprene valve body knob and installation parts 7439901 Glass Collector Chamber
24. 6 Product Service Domestic 1 800 522 7658 International 816 333 8811 10 11 12 13 Chapter 4 Using Your Freeze Dryer Auto Mode Indicator When lit the green LED indicates that the Freeze Dryer is in Auto Mode In this mode the vacuum pump will start when the collector temperature reaches 40 C Vacuum Graph Display This display indicates the relative system vacuum level The highest LED indicates that the vacuum level is above 2 0 mBar The indicators will sequence down when the vacuum level reaches 2 0 1 0 0 8 0 6 0 45 0 12 mBar The lower green LED flashes when the system vacuum level is 0 45 to 0 12 mBar and illuminates steadily below 0 133 mBar Collector Temperature Graph Display This display indicates the temperature of the collector The highest LED indicates the collector temperature is warmer than 10 C The indicators will sequence down when the temperature reaches 10 0 10 20 30 40 C When the collector temperature is 40 C or lower the green indicator will light Alarm Indicator This red LED indicates that a system alarm has occurred Press the Menu Switch to display the alarm message on the LCD display Main Power Switch Turns the Freeze Dryer on or off Not shown located on the left side of the cabinet Operation Checklist The following checklist should be followed prior to each use of your Freeze Dryer l 2 Wipe the interior of the collector chamber
25. 67700 Vacuum Pump Two stage direct drive pump 195 liters minute 115 VAC 50 60 Hz single phase 7 8 amps Includes Pump Exhaust Filter 1473400 Catalog 1473400 7739403 Vacuum Pump Two stage direct drive pump 195 liters minute 230 VAC 50 60 Hz single phase 4 0 amps Includes Pump Exhaust Filter 1473400 Catalog 1473400 1472100 Vacuum Pump Two stage direct drive pump 117 liters minute 115 VAC 50 60 Hz single phase 4 6 amps Includes Pump Exhaust Filter Catalog 1473400 7739402 Vacuum Pump Two stage direct drive pump 117 liters minute 230 VAC 50 60 Hz single phase 2 4 amps Includes Pump Exhaust Filter Catalog 1473400 7584000 Vacuum Pump Chemical Resistant Hybrid Combination two stage rotary vane pump and two stage chemistry diaphragm pump 98 115 liters minute 115 VAC 50 60 Hz single phase 7584002 Vacuum Pump Chemical Resistant Hybrid Combination two stage rotary vane pump and two stage chemistry diaphragm pump 98 115 liters minute 230 VAC 50 60 Hz single phase 1472200 Pump Inlet Filter Disposable filter that prevents oil back streaming and protects vacuum pump from sub micron particles Fits vacuum pumps 1466700 and 7739403 Product Service Domestic 1 800 522 7658 International 816 333 8811 53 Appendix D Freeze Dryer Accessories 54 PART DESCRIPTION 1473400 Pump Exhaust Filter Disposable filter that removes visible oil mist and odor from vacuum pump exhaust Fits vacuum
26. AMS ACCESSORIES COMMUNICATIONS The first time Hyper Terminal M 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 32 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 6 Using the RS232 Receptacle 5 The Com X Properties dialogue box will open Enter the appropriate data properties and press OK Product Service Domestic 1 800 522 7658 International 816 333 8811 33 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 BXT 40U 18 SF 999C 999PG 9 gt B lt T 40V 18 SF 999C 999PG 9 gt B lt T 40V 18 SF 999C 999P6 9 B T 40V 18 SF 999C 999PG 9 gt B T 40U 18 SF 999C 999PG 9 gt B lt T 40V 18 SF 999C 999PG 9 gt B lt T 40V 18 SF 999C 999P6 9 B T 40 18 SF 999C 999PG 9 gt B lt T 40V 18 SF 9990 999PG 9 gt 34 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 7 TROUBLESHOOTING Refer to the following
27. FreeZone Freeze Dry System 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 Freeze Dry Process Freeze drying is an important process in sample preparation and for the preservation and storage of biologicals pharmaceuticals and foods Of the various methods of dehydration freeze drying lyophilization is especially suited for substances that are heat sensitive Other than food processing e g coffee whole dinners freeze drying has been extensively used in the development of pharmaceuticals e g antibiotics and preservation of biologicals e g proteins plasma viruses and cell lines The nondestructive nature of this process has been demonstrated by the retention of viability in freeze dried viruses and microorganisms Freeze drying is a process whereby water or other solvent is removed from frozen material by converting the frozen water directly into vapor without the intermediate formation of liquid water The basis for this sublimation process involves the absorption of heat by the frozen sample in order to vaporize the ice the use of a vacuum pump to enhance the removal of water vapor from the surface of the sample the transfer of water vapor to a collector and the removal of heat
28. ay information This can be done anytime throughout the Modifying the Display routine Product Service Domestic 1 800 522 7658 International 816 333 8811 APPENDIX A FREEZE DRYER COMPONENTS The following pages list components that are available for your Freeze Dryer The parts shown are the most common replacement parts If other parts are required contact Product Service Product Service Domestic 1 800 522 7658 International 816 333 8811 47 Appendix A Freeze Dryer Components Item Part No Description 77690800 Lid Gasket 7532900 Lid 7448000 Printed Circuit Board RS232 7953800 Motor Fan 115V 7953801 Motor Fan 230V 5 7150607 Compressor 115V 60 Hz 7750606 Compressor 230V 50 Hz 7750605 Compressor 230V 60 Hz Bl WwW NY 6 1302300 Switch 7 7426000 Control Panel Label 8 7445590 Printed Circuit Board 9 7728000 Drain Plug 10 1643600 O Ring 11 7645904 Drain Hose 12 7373450 Vacuum Hose Not Shown 13 1336400 Power Cord 115V 60Hz Not Shown 1336500 Power Cord 230V 50Hz EU Not Shown 1342100 Power Cord 230V 60Hz Not Shown 1332601 Power Cord 230V 50Hz UK Not Shown 1332701 Power Cord 230V 50Hz China Not Shown 14 7445400 Vacuum Sensor 15 7515300 Temperature Sensor Not Shown 16 7304700 Wire Harness Power 115V Not Shown 7304701 Wire Harness Power 230V Not Shown
29. ber This is normal Product Service Domestic 1 800 522 7658 International 816 333 8811 27 28 CHAPTER 5 MAINTAINING YouR FREEZE DRYER Under normal operation the Freeze Dryer requires little maintenance The following maintenance schedule is recommended As needed 1 Clean up all spills remove liquids from the chamber 2 Clean lid and gasket using soft cloth sponge or chamois and a mild non abrasive soap or detergent 3 Check oil level of the vacuum pump It should be between MIN and MAX If the oil level is less than an inch 25 4 mm above MIN add oil to proper level 4 If oil shows cloudiness particles or discoloration drain the pump and replace with fresh oil 5 Utilization of acids requires immediate cleaning and neutralization after a run or physical damage to the collector chamber and collector coil will result 6 Check the collection chamber for condensed or frozen solvents and dispose of appropriately Completely empty the collector chamber before the next run or before attempting to start the vacuum pump 7 Ifsample valves leak or stems become difficult to turn pull the stem out of the rubber valve body and apply a thin coat of vacuum grease to the stem Reinsert the stem into the valve body Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 5 Maintaining Your Rapid Vap Monthly 1 The rubber components on the Freeze Dryer may eventually deteriorate a
30. ches of area provides heat control 7806031 Bulk Tray Dryer 230V 50 60 Hz Three shelves 630 square inches of area provides heat control With 6 port manifold 7806032 Bulk Tray Dryer 230V 50 60 Hz Three shelves 630 square inches of area provides heat control With RS232 output connection 7806033 Bulk Tray Dryer 230V 50 60 Hz Three shelves 630 square inches of area provides heat control With 6 port manifold and RS232 output connection 7948020 Stoppering Tray Dryer 115V 60 Hz three shelves 600 square inches of area provides temperature control and stoppering under vacuum 7948030 Stoppering Tray Dryer 230V 50 Hz three shelves 600 square inches of area provides temperature control and stoppering under vacuum 7948040 Stoppering Tray Dryer 230V 60 Hz three shelves 600 square inches of area provides temperature control and stoppering under vacuum 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 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix D Freeze Dryer Accessories PART DESCRIPTION 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 7537801 Cable Connects the RS232 output from the Freeze Dr
31. ctory default setting Modifying the Display To enter an offset or to configure the alarms perform the following steps Press and hold MENU button approximately 10 seconds until the display shows PRODUCTION MENU MASTER RESET It is recommended that you do NOT perform a Master Reset because all offsets and configurations that have been entered will be lost If you must perform a Master Reset hold SELECT approximately 5 seconds This will reset Vacuum units to mBar Vacuum set point to 0 mBar Temperature units to C Refrigeration total hours to 0 Vacuum pump total hours to 0 RS232 transmission rate to 10 seconds Temperature offset to 0 C Vacuum offset to 0 mBar Low line voltage to 0 V offset High line voltage to 0 V offset Moisture sensor to enabled Refrigeration to operate in Manual Mode Product Service Domestic 1 800 522 7658 International 816 333 8811 43 Chapter 8 Modifying Your Freeze Dryer Display The display will default to the main freeze dry display information If you do not want to restore all factory settings but want to adjust offsets press MENU briefly and the display will show COLLECTOR TEMP OFFSET OC Press SELECT until the appropriate offset is shown Each number represents 1 C Press MENU and if the drying chamber has been installed the display will show SDC TEMP OFFSET OC Press SELECT until the appropriate offset is shown Each number represents 1 C Press
32. cuum 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 For example a solution of sodium chloride and water would freeze dry at a slower rate than pure water The eutectic temperature of a sodium chloride solution is about 21 C and at this temperature the vapor pressure is about 1 16 that of water at 0 C Although the eutectic temperature is not dependent upon the concentration of sodium chloride the vapor pressure of the water would decrease as the concentration of sodium chloride increased This is due to the fact that as the solute concentration increases less of the surface area of the frozen sample is occupied by water In general most solutions or biological samples will have a eutectic temperature of 10 to 25 C However if the sample contains a simple sugar such as glucose or if the sample is animal or plant tissue the eutectic temperature may be as low as 30 to 50 C 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 concentra
33. de of the cabinet Dispose of the liquid appropriately Utilization of acid requires immediate cleaning 1 and neutralization after defrost or physical damage to the collector chamber and collector coil will result ios Do not attempt to chip ice from the collector coil as damage may occur to the coil Never attempt to start the vacuum pump when there is liquid in the collector chamber This could result in damage to the vacuum pump 24 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer Alarms A number of unusual events may occur during a lyophilization procedure that can adversely effect the operation of the Freeze Dryer If an event occurs the alarm indicator will flash and the beeper will sound The beeper will automatically mute itself after one minute The specific alarm can be identified by pressing MENU Pressing MENU multiple times will display multiple alarms if they have occurred The following out of specification conditions will initiate an alarm Power Failure If a power failure occurs during a Freeze Dry process the vacuum control valve will allow air to bleed into the Freeze Dryer System If the failure is of a short duration and the collector does not warm up excessively when power is restored the Freeze Dryer will restart and resume operation of the refrigeration and vacuum systems If the power failure lasts for a longer duration and the
34. e Dry System properly The Freeze Dryer is equipped with a 3 4 ID heavy wall vacuum hose for connecting the collector chamber to the vacuum pump Make certain that the oil in the vacuum pump is at the proper level Place the vacuum pump near the Benchtop Freeze Dryer Connect the vacuum pump power cord to the receptacle on the back of the cabinet labeled vacuum pump If the vacuum pump has an off on switch turn the switch on The vacuum pump will be controlled by the Freeze Dryer Connect the vacuum pump inlet port to the vacuum tube on the back of the cabinet with the vacuum hose and clamps provided If necessary cut the hose to proper length to allow for gentle bends without kinks Models rated for use on 230V have a reverse IEC connector for attaching the vacuum pump power cord A plug is supplied that can be installed on the vacuum pump power cord if necessary Electrical Connection Plug the power cord into the receptacle on the back of the Freeze Dryer and plug the other end into a suitable power receptacle Drying Chamber or Drying Manifold Installation The drying chamber or drying manifold purchased separately may be positioned directly above the 3 inch port on the top of the Freeze Dryer Follow the instructions supplied with the selected accessory Product Service Domestic 1 800 522 7658 International 816 333 8811 11 Chapter 3 Getting Started 12 Chemical Resistance of Freeze Dryer Components
35. e Dryer Read this chapter to learn how to unpack and move your Freeze Dryer set up your Freeze Dryer connect the electrical supply source to your Freeze Dryer properly exhaust your Freeze Dryer safely use solvents with your Freeze Dryer The FreeZone 6 Liter Benchtop Freeze Dry System weighs over 135 Ibs 61 kg If you must lift the Freeze Dryer manually use at least two 2 persons and follow safe lifting guidelines Unpacking Your Freeze Dryer Carefully unpack your Freeze Dryer and inspect it for damage that The United States may have occurred in transit If your Freeze Dryer is damaged Interstate Commerce notify the delivery carrier immediately and retain the entire Commission rules shipment intact for inspection by the carrier filed w Me deer carrier within fifieen 15 DO NOT RETURN GOODS WITHOUT THE days of delivery PRIOR AUTHORIZATION OF LABCONCO ke UNAUTHORIZED RETURNS WILL NOT BE ACCEPTED Product Service Domestic 1 800 522 7658 International 816 333 8811 9 Chapter 3 Getting Started 10 Catalog 7752020 IF YOUR FREEZE 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 Ee PACKING MATERIAL FOR YOUR FREEZE DRYER UNTIL YOU HAVE CHECKED ALL OF THE COMPONENTS AND INSTALLED AND TESTED THE FREEZE DRYER Freeze Dryer Components Locate the model of Fre
36. e 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 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 Look inside the chamber for any bubbling while the pump is running and after you shut the pump off 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 Should the bubbling still be present loosen the bulkhead fittings and apply vacuum grease to the O rings then reassembly and test 40 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting O Ring and Collector Coil Vacuum Grease 4 If bubbling was observed on the chamber surface the chamber must be replaced Thi
37. e slower the rate of freeze drying This is based on the fact that the heat of sublimation is usually absorbed on one side of the frozen sample and must travel through the frozen layer to vaporize water at the other surface In addition as the sample is freeze dried the water vapor must travel through the layer of dried material The thicker the sample the greater the chance that the dried layer may collapse which would cause an additional decrease in the rate of freeze drying The surface area and thickness of the sample can usually be ignored when each sample contains only a few milliliters However for larger volumes the samples should be shell frozen to maximize the surface area and minimize the thickness of the 2 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction sample The volume of the freeze dry flask should be two to three times the volume of the sample In order for lyophilization to occur ice must be removed from the frozen sample via sublimation This is accomplished by the collector and the vacuum pump The collector which should be at least 15 to 20 C colder than the eutectic temperature melting temperature of the sample traps vapor as ice Since the vapor pressure at the collector is lower than that of the sample the flow of water vapor is from the sample to the collector Since this vapor diffusion process occurs very slowly under normal atmospheric conditions a good va
38. ead Nut M Knob amp Stem im Ri Valve Bod Trim Ring Assembly alve body Knob amp Stem Thrust Washer Gasket Bulkhead Assembly No grease Fitting required Valve Assembly Manifold Valve Assembly Stainless Steel Chamber Ill System Components and Collection Chamber Isolation 1 Remove the drying chamber or manifold 2 Leave the gasket on and turn a large freeze dry flask upside down to cover the connection port 3 Start the freeze dryer and observe the vacuum indication If the vacuum indication is good then the problem is in the drying chamber or manifold and you should return to Section IT Gaskets Tubing Connections Sample Valves 38 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 7 Troubleshooting FREEZE DRY FLASK 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 Insufficient vacuum indicates a bad pump or a leak in the connections from the pump to the side of the chamber Collector Product Service Domestic 1 800 522 7658 International 816 333 8811 39 Chapter 7 Troubleshooting The following test is used to check the collection chamber integrity The figur
39. eze Dryer you received in the following table Verify that the components listed are present and undamaged PTFE Coated Description Chamber 6 Liter Benchtop Freeze Dryer 1336500 7752021 Xx 1336400 6 Liter Benchtop Freeze Dryer 7752030 6 Liter Benchtop Freeze Dryer 7752031 6 Liter Benchtop Freeze Dryer 7752040 6 Liter Benchtop Freeze Dryer 7752041 6 Liter Benchtop Freeze Dryer 7752060 6 Liter Benchtop Freeze Dryer 7752061 6 Liter Benchtop Freeze Dryer 7752070 6 Liter Benchtop Freeze Dryer 7752071 6 Liter Benchtop Freeze Dryer Plus the following Part Component Description 7400209 User s Manual 1291000 Plug 230V models only 7373450 Vacuum Hose 1488800 Hose Clamps 2 7532900 Chamber Lid 7690800 Lid Gasket If you did not receive one or more of the components listed for your Freeze Dryer or if any of the components are damaged contact Labconco Corporation immediately for further instructions Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 3 Getting Started Setting Up Your Freeze Dryer After you verify receipt of the proper components move your Freeze Dryer to the location where you want to install it Then follow the steps listed below Vacuum Pump Connection A vacuum pump as described in Chapter 2 Prerequisites is required to operate your Freez
40. f construction Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 3 Getting Started 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 e Rubber and plastic components that have been exposed to damaging compounds should be removed and flushed with water e The oil in the vacuum pump should be checked often It must be changed if it is cloudy shows particles or is discolored The useful life of vacuum pump oil can be extended if the vacuum pump is operated for an extended period of time after a freeze dry run This allows contaminants to be purged from the hot oil This must be done with the inlet to the pump blocked off to prevent air from free flowing through the pump This is accomplished by closing all sample valves on a clean dry freeze dry system and turning on the vacuum pump If the pump is operated at an elevated vacuum level gt 10mBar oil may be expelled from the pump and damage could occur Another way to extend the life of the vacuum pump is to install an optional secondary trap in the line between the Freeze Dryer 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 If you have questions about using spec
41. he green LED will be lit steadily indicating that samples may be added Setting the Operating Vacuum Level The vacuum level may be set by the user to optimize the freeze dry process Normally the sublimation rate will increase if there is less vacuum a higher pressure in the Freeze Dryer A good starting place is to set the vacuum so its level is equivalent to about 10 C colder than the eutectic or collapse temperature of the sample Adjustments to the vacuum level must be made for various freeze drying conditions Factors that must be considered are whether the sample is freeze dried on heated shelves or in glassware attached to manifold valves the volatility of the sample itself the size of the sample and the heat energy supplied to the sample When the vacuum control is set to operate at less vacuum the ice holding capacity of the collector may be decreased This can be improved by installing a baffle in the collector See Appendix D Freeze Dryer Accessories for the baffle part number Position the baffle so it rests on the top of the collector coil The arrow should point toward the front Product Service Domestic 1 800 522 7658 International 816 333 8811 21 Chapter 4 Using Your Freeze Dryer Some guidelines for setting the Freeze Dryer are shown below These show pre freezing temperatures and vacuum levels Exact protocols must be determined by the user for the specific samples that are being freeze dried
42. if your Freeze Dryer fails to operate properly If the suggested corrective actions do not solve your problem contact Labconco for additional assistance Labconco Freeze Dry Systems that are clean dry and without samples attached should reach a vacuum of 0 133 mBar within 10 minutes and should achieve an ultimate vacuum of 0 033 mBar within 18 hours when the refrigeration is operating If the Freeze Dryer does not obtain a satisfactory vacuum perform the following maintenance tests l Vacuum Pump First make sure that the vacuum pump operates If it fails to operate check the electrical connections of the Freeze Dryer to the power source and then check the electrical connection of the vacuum pump to the Freeze Dryer If the vacuum pump has a power switch make sure that it is turned on If the vacuum is not adequate when the vacuum pump is operating proceed with the following steps 1 Check the oil and ensure it is clear and clean If the oil looks cloudy or has any particulates replace the pump oil Sometimes it may be necessary to flush the pump with clean oil several times To flush the pump run the pump 5 to 10 minutes to allow the oil to warm up Drain the oil and refill with clean oil Repeat as necessary 2 Check the oil level in the pump Ensure it is filled to the correct level 3 Check vacuum hose connections from the pump to the Freeze Dryer and try running the unit Product Service Domestic 1 800 522 7658 Internat
43. ific compounds in the Freeze Dryer contact Labconco Technical Service at 1 800 821 5525 or 816 333 8811 or e mail labconco labconco com 1 Solvent Safety Precautions Solvents used in the Freeze Dryer may be flammable or hazardous to your health Use extreme caution and keep sources of ignition away from the solvents When using flammable or hazardous solvents the vacuum pump must be vented to or operated inside a fume hood Product Service Domestic 1 800 522 7658 International 816 333 8811 13 Chapter 3 Getting Started Hazardous materials such as strong acids or bases radioactive substances and volatile organics must be handled carefully and promptly cleaned up if spilled If a sample is spilled in the collector chamber it must immediately be cleaned up WARNING The disposal of substances used in connection with this equipment may be governed by various Federal State or local regulations All users of this equipment are urged to become familiar with any regulations that apply in the user s area concerning the dumping of waste materials in or upon water land or air and to comply with such regulations 14 Product Service Domestic 1 800 522 7658 International 816 333 8811 CHAPTER 4 Usinc Your FREEZE DRYER After your Freeze Dryer has been installed as detailed in Chapter 3 Getting Started you are ready to begin using your Freeze Dryer Read this chapter to learn how to e operate the controls e u
44. ional 816 333 8811 35 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 Dryer 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 ll Gaskets Tubing Connections Sample Valves l Check all sample valves on the drying chamber manifold and ensure all valves are closed or in the vent position Check to ensure all fittings are tight and sealed properly against the chamber Inspect valves for cracks or cuts Inspect gasket s for cracks or defects Ensure the gasket is clean Apply a thin coat of vacuum grease to the gasket Keep in mind too much vacuum grease can actually cause leaks Check the drain line and ensure the drain plug is installed and the tube appears to be in good condition Check all rubber vacuum tubing for signs of deterioration or cracking Check all connections and make sure they are secure and leak tight When
45. isites explains what you need to do to prepare your site before you install your Freeze Dryer Electrical requirements are discussed Chapter 3 Getting Started contains the information you need to properly unpack inspect and install your Freeze Dryer Chapter 4 Using Your Freeze Dryer discusses the basic operation of your Freeze Dryer Information on how to attach samples and run the Freeze Dryer is included Chapter 5 Maintaining Your Freeze Dryer explains how to perform routine maintenance on your Freeze Dryer Chapter 6 Using the RS232 Receptacle describes how to connect a computer for monitoring the operation Chapter 7 Troubleshooting contains a table of problems you may encounter while using your Freeze Dryer including the probable causes of the problems and suggested corrective actions Chapter 8 Modifying Your Freeze Dryer Display describes how to calibrate the vacuum display and restore factory settings Appendix A Freeze Dryer Components contains labeled diagrams of the components of the Freeze Dryer Appendix B Freeze Dryer Dimensions contains comprehensive diagrams showing the dimensions for the Freeze Dryer Appendix C Freeze Dryer Specifications contains product specifications Appendix D Freeze Dryer Accessories lists the part numbers and descriptions of all of the accessories available for your Freeze Dryer Product Service Domestic 1 800 522 7658 International 816 333 8811 5 Chapter 1
46. n options 79600 followed by two digit number based on options 74200 followed by two digit number based on options 738 followed by two digit number based on model size followed by another two digit number based on options Manufacturer Labconco Corporation 8811 Prospect Avenue Kansas City MO 64132 USA Ph 816 333 8811 Fax 816 363 0130 labconco labconco com is in conformity with the standards listed below EN61010 1 EN61326 1 EN55022 EN61000 3 2 3 following the provisions of the following directives 2006 42 EC 2004 108 EC 2006 95 EC 2011 65 EU when installed and operated in accordance with the manufacturers installation and operating instructions Cousas Cory JA Jum 2S 2012 1 i Mark Schmitz Place and date of issue Vice President Research and Engineering Labconco Corporation Labconco P N 3696002 Rev I ECO G970 Product Service Domestic 1 800 522 7658 International 816 333 8811
47. nd 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 chamber lid 3 Using a soft cloth sponge or chamois and a mild non abrasive soap or detergent clean the exterior surfaces of the Freeze Dryer 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 Every 12 months or more often if the Freeze Dryer is operated in a dusty environment the refrigeration system condenser should be cleaned Using a vacuum cleaner with brush attachment clean the condenser to ensure proper airflow for peak performance Product Service Domestic 1 800 522 7658 International 816 333 8811 29 CHAPTER 6 Usinc THe RS232 RECEPTACLE The operation of the Freeze Dryer can be monitored using a computer when it is connected to the RS232 receptacle on the rear panel The computer cannot control the operation of the Freeze Dryer The monitored parameters are the collector temperature in C and vacuum in microbars When a Labconco Stoppering Tray Dryer is connected to a Labconco Freeze Dryer as detailed in the Stoppering Tray Dryer User s Manual the
48. nderstand the display e connect samples C Freeze Dryer Specifications The electrical protection properties of the Freeze Dryer may be impaired if the Freeze Dryer is used inappropriately Do not use the Freeze Dryer in a manner not 1 specified by the manufacturer refer to Appendix Product Service Domestic 1 800 522 7658 International 816 333 8811 15 Chapter 4 Using Your Freeze Dryer Freeze Dryer Controls The control panel for the Freeze Dryer is shown below with a description about its function bh B 9 S og os SOO TEMP 1 LCD Display Displays system operating parameters set up parameters and alarm messages 2 Menu Switch This switch is used to change the display from operating system parameters to set up parameters 3 Select Switch Used to select set up parameters 4 Vacuum Switch Used to start or stop the vacuum pump when operating in manual start up mode 5 Vacuum Indicator This green LED indicates that power is being supplied to the vacuum pump receptacle on the back of the Freeze Dryer 6 Manual Refrigeration Switch Used to start only the refrigeration module 7 Manual Operation Indicator When lit the green LED indicates the Freeze Dryer is being controlled manually by the operator The operator must start each function 8 Auto Mode Switch Used to start or stop the refrigeration and the Auto Mode process 1
49. ned toward the sample port to apply vacuum to the sample 22 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer Bevel in vent position Vent Backfill Port Bevel in vacuum position Adapter 2 Before adding another sample allow system vacuum to return to 0 133 mBar or lower Any combination of valves and sample sizes may be utilized at one time provided that the system vacuum and collector temperature remain sufficiently low to prevent melting of the frozen sample 3 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 4 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 Should backfilling with an inert gas be required connect the gas supply line to the vent port on the valve before turning the plastic knob on the valve to vent position The sample container may now be removed In the vent position the bevel on the valve knob should point away from the sample port 5 Ampules may be flame sealed while connected to a valve by using a sealing torch Care must be taken not to burn the valve An insulation material placed between the valve and the torch
50. nifold Installation Chemical Resistance of Freeze Dryer Components Solvent Safety Precautions CHAPTER 4 USING YOUR FREEZE DRYER Freeze Dryer Controls Operation Checklist Vacuum Pump Ballast Setting Operating the Freeze Dryer Set Up Automatic Start Up Manual Start Up Setting the Operating Vacuum Pre Freezing Samples Adding Sample Shut Down DNA BWN oo oo OO N N 10 11 11 11 11 12 13 15 16 17 18 18 18 20 21 21 22 22 24 Defrosting Alarms Power Failure Line Voltage Out of Range Temperature Out of Range Service Vacuum Pump Moisture in Collector CHAPTER 5 MAINTAINING YOUR FREEZE DRYER CHAPTER 6 USING THE RS232 RECEPTACLE Computer Connection for Computer Interface CHAPTER 7 TROUBLESHOOTING Vacuum Pump Gaskets Tubing Connections Sample Valves System Components amp Collection Chamber Isolation Refrigeration Module Operation CHAPTER 8 MODIFYING YOUR FREEZE DRYER DISPLAY Temperature and Vacuum Display Line Voltage Alarm Points Moisture Sensor Alarm Modifying the Display APPENDIX A FREEZE DRYER COMPONENTS APPENDIX B FREEZE DRYER DIMENSIONS APPENDIX C FREEZE DRYER SPECIFICATIONS Electrical Specifications Environmental Conditions APPENDIX D FREEZE DRYER ACCESSORIES DECLARATION OF CONFORMITY 24 25 25 26 26 26 2 28 30 30 35 35 36 38 41 42 42 42 43 43 47 50 51 51 52 53 62 CHAPTER 1 INTRODUCTION Congratulations on your purchase of a Labconco
51. of the Freeze Dry System If the gas ballast is left open for extended periods of operation the oil can be pumped out the exhaust causing the pump to fail Operating the Freeze Dryer Set Up The Freeze Dryer may be configured to automatically start the vacuum pump when the collector temperature reaches 40 C The display units for vacuum may be selected to be mBar Pascal Pa or Torr and the temperature may be displayed as F or C The run time of the refrigeration system and the vacuum pump may be monitored To configure your Freeze Dryer turn the main power switch ON and press MENU The display will show VACUUM UNITS mBar Pa e Press SELECT until the desired units are flashing e Press MENU e The display will show VACUUM SET POINT XXXX YYY Where YYY is the units selected above 18 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer e Press SELECT until the desired vacuum operating level is displayed See Setting the Operating Vacuum Level for guidelines e f O is selected the vacuum control is disabled and the vacuum level in the Freeze Dry System will be determined by the capabilities of the vacuum pump e Press MENU e The display will show TEMPERATURE UNITS C SE e Press SELECT until the desired units are flashing e Press MENU e The display will show REFRIG TOTAL HOUR XXXX SERVICE HOUR XXXX e To reset the
52. ommission rules require that claims be filed with the delivery carrier within fifteen 15 days of delivery Limitation of Liability The disposal and or emission of substances used in connection with this equipment may be governed by various federal state or local regulations All users of this equipment are required to become familiar with any regulations that apply in the user s area concerning the dumping of waste materials in or upon water land or air and to comply with such regulations Labconco Corporation is held harmless with respect to user s compliance with such regulations Contacting Labconco Corporation If you have questions that are not addressed in this manual or if you need technical assistance contact Labconco s Customer Service Department or Labconco s Product Service Department at 1 800 821 5525 or 1 816 333 8811 between the hours of 7 00 a m and 6 00 p m Central Standard Time Part 7400209 Rev E ECO H435 TABLE Or 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 Chamber or Manifold Requirements CHAPTER 3 GETTING STARTED Unpacking Your Freeze Dryer Freeze Dryer Components Setting Up Your Freeze Dryer Vacuum Pump Connection Electrical Connection Drying Chamber or Drying Ma
53. pening loads fast Fast Freeze Flask cleans easily has only two components ea high strength borosilicate Horizontal shell freezing Flask glass bottom may be placed in to withstand a horizontal posi extreme tion and rotated temperatures in a bath for shell and high freezing vacuum e a flexible non contaminating silicone rubber top No vacuum grease is necessary No threads reduces spills hooks or springs provides better are needed balance Entire flask may be autoclaved Available in nine convenient sizes Adapters Add the Adapters for connecting the Fast Freeze Flasks to the valve ports on your drying chamber or manifold Choose borosilicate glass or stainless steel adapters in 1 2 and 3 4 diameters Diameter Straight 45 Bend Adapter Adapter Borosilicate Glass 1 2 flask top to 1 2 valve 7545000 7545600 3 4 flask top to 3 4 valve 7545200 7545800 1 2 flask top to 3 4 valve 7545400 7546000 3 4 flask top to 1 2 valve 7545400 7546000 Stainless Steel 1 2 flask top to 1 2 valve 7547000 7547400 3 4 flask top to 3 4 valve 7547200 7547600 oe 75448 10 Replacement Filter Paper 1000 10 packages of 100 1 diameter 28mm Pore size 17 microns Shipping weight 0 5 Ib Product Service Domestic 1 800 522 7658 International 816 333 8811 Lyph Lock Flasks Lyph Lock Flasks simplify your lyophilization procedures
54. rs with all major either 1938 or24 40 brands of labo standard taper joints ratory freeze have 90 bend dry apparatus Required order separately Only three pieces per flask no a or springs Silicone rubber The complete seal t Lyph Lock Flask er n includes The flexible ring e a flask top of holds securely high strength l borosilicate together during fi des LABCONCO Enia e a flexible non tion contaminating silicone rubber seal e a flask bottom of borosilicate glass to with stand extreme temperatures and high vacuum Available in seven convenient sizes Flat bottom reduces spills Entire flask may provides better be autoclaved Provides a high vacuum seal for efficient lyophilization Adapters Add the Adapters for connecting the Lyph Lock Flasks to the valve ports on your drying chamber or manifold a 90 Bend Description Adapter 7568000 Connects 1938 STJ Flask Top to 1 2 valve 7568200 Connects 19 38 STJ Flask Top to 3 4 valve 7568400 Connects 24 40 ST Flask Top to 1 2 valve 7568600 Connects 24 40 ST Flask Top to 3 4 valve SSS Valves on the freeze dry systems drying chambers and manifolds offered in this catalog fit adapters of both 1 2 and 3 4 sies Size information is provided for selecting adapters for older Labconco models and other reeze dryers Product Service Domestic 1 800 522 7658 International 816 333 8811 59
55. s selected Press MENU and the display will show DRYING CHAMBER NOT INSTALLED Press and hold SELECT to change the status Press MENU and the display will show PURGE VALVE NOT INSTALLED Press and hold SELECT to change the status Press MENU and the display will show DEFROST HEATER NOT INSTALLED Press and hold SELECT to change the status Press MENU and the display will show MOISTURE SENSOR INSTALLED Press and hold SELECT if you want to disable the moisture sensor Press MENU and the display will show SHELL FREEZER NOT INSTALLED Press and hold SELECT to change the status Product Service Domestic 1 800 522 7658 International 816 333 8811 45 46 Chapter 8 Modifying Your Freeze Dryer Display Press MENU and the display will show HOLD SELECT TO CLEAR ALL TOTAL HOURS If you want to reset Total Hours press and hold SELECT until an audible beep is heard The display will default to the main freeze dry display information If you do not want to set Total Hours press MENU and the display will show PRODUCTION MENU MASTER RESET The routine will repeat by pressing MENU or wait approximately 10 seconds for the display to default to the main freeze dry information display information In order to store offsets in memory you Must Press and Hold MENU until display shows PASSWORD Wait approximately 10 seconds and the display will default to the main freeze dry displ
56. s type of leak cannot be successfully repaired The leading cause of a chamber surface leak is corrosive residue left in the chamber after use Refrigeration Module Operation Under a no load condition the FreeZone Single Stage Freeze Dry System can achieve a collector temperature of 50 C or lower when the system is under vacuum within 30 minutes when the vacuum pump is running depending on ambient temperature and humidity 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 Product Service Domestic 1 800 522 7658 International 816 333 8811 41 42 CHAPTER 8 Mopiryinc Your FREEZE DRYER DisPLAY Your Freeze Dryer has been carefully calibrated and tested before shipping however under certain circumstances it may be necessary to adjust the calibration of the temperature and or vacuum display or to modify alarm points Adjustments may be necessary if the Freeze Dryer requires service or if it is operating on a line voltage outside the voltage range at which the alarm was preset This DOES NOT mean that the Freeze Dryer may be operated at a voltage outside the ranges shown in Appendix C Temperature and Vacuum Display An offset may be added to the collector temperat
57. stem When the collector reaches 40 C the vacuum pump will start The Temperature and Vacuum Graphs will indicate collector temperature and system vacuum The LCD display will show the actual temperature of the collector When the vacuum in the system is above 5 mBar the vacuum display will indicate HI At 5 mBar and below the display will show the actual vacuum When the system vacuum is between 0 450 and 0 133 mBar the lower green vacuum graph LED will flash When the system vacuum level is 0 133 mBar the green LED will be lit steadily indicating that most samples may be added 20 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer Manual Start Up To manually run the freeze dry process press the REFRIGERATION MAN switch This will start the refrigeration system The green LED above the switch will illuminate When the collector temperature reaches 40 C the vacuum pump may be started by pressing the VACUUM switch The Temperature and Vacuum Graphs will indicate collector temperature and system vacuum The LCD display will show the actual temperature of the collector When the vacuum in the system is above 5 mBar the vacuum display will indicate HI At 5 mBar and below the display will show the actual vacuum When the system vacuum is between 0 450 and 0 133 mBar the lower green vacuum graph LED will flash When the system vacuum level is 0 133 mBar t
58. tainless steel stems Ten per package Shipping weight 0 5 Ib 0 2 kg Stoppers 7572510 Stopper for Stoppering Ampules 75723 10 100 per package Shipping weight 3 Ibs 1 4 kg Trident Adapter 7762700 Three Way Adapter permits attachment of three ampules to a single valve port Ampules are attached using Ampule Valve Adapters or 1 8 surgical tubing not provided Cavity in adapter body can be filled with cotton fiber media to help prevent contamination between samples Shipping weight 3 oz 0 1 kg Product Service Domestic 1 800 522 7658 International 816 333 8811 61 62 Protecting your laboratory environment LABCONCO CORPORATION 816 333 8811 00 821 5525 8811 Prospect Avenue FAX 818 363 01 Kansas City MO 64132 2696 www labconco nm CE Declaration of Conformity Labconco Corporation 8811 Prospect Avenue Kansas City MO 64132 USA Ph 816 333 8811 Fax 816 363 0130 labconco labconco com being the representative party in the EU solely responsible for this certification hereby declare that the following product Equipment Laboratory Equipment FreeZone Freeze Dryers Type Model 775 followed by two digit number based on model size followed by another two digit number based on options 77400 followed by two digit number based on options 79340 followed by two digit number based on options 767 followed by two digit number based on model size followed by another two digit number based o
59. tion of the sample and the rate and amount of heat transferred to the frozen sample Of these factors the eutectic temperature is the most important factor in determining the amount of sample that can be freeze dried at one time particularly when flasks are used This is because as the eutectic temperature decreases the vapor pressure decreases but the rate of heat absorption by the sample does not change This tends to promote melting of the sample which leads to a marked increase in vapor Product Service Domestic 1 800 522 7658 International 816 333 8811 3 Chapter 1 Introduction pressure and ultimately overloads the collector and vacuum pump Samples that have eutectic temperatures of 20 C or lower should be placed on the freeze dry system one flask at a time so that the vacuum in the system may recover before adding another sample to the system If the vacuum does not recover the capacity of the freeze dry system has been exceeded and the sample should be removed If there is a problem with a particular type of sample melting when placed on the freeze dry system dilution of the sample with more water or providing some insulation around the flask to decrease the rate of heat absorption by the sample may help If the eutectic temperature of the sample is 40 to 60 C the freeze dry system selected for use must be equipped with cascade type refrigeration so that the collector temperature can be cooled to below 75 C or a dr
60. ure 48 Collector Temperature in Celsius V Vacuum 18 Vacuum Level in Micro Bars SF Shell Freezer Temperature not available on 6L Benchtop models 9 Feature not installed or out of range C Vacuum Chamber Temperature not available on 6L Benchtop models PG Purge not available on 6L Benchtop models If a Stoppering Tray Dryer is attached to the Freeze Dryer and the data interconnect cable is installed additional data about that accessory will be transmitted from the Freeze Dryer See the User s Manual for the Stoppering Tray Dryer for a description of the data 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 The Product Service Domestic 1 800 522 7658 International 816 333 8811 31 Chapter 6 Using the RS232 Receptacle following describes how to use an IBM compatible computer with Hyper Terminal software included with Windows 95 98 XP or 2000 operating systems to collect the RS232 data from your Freeze Dryer 1 Make sure that the Freeze Dryer is properly connected to the communication port on the computer 2 Open Hyper Terminal software 1 Windows 95 or 98 use START PROGRAMS ACCESSORIES ii Windows 2000 or XP use START PROGR
61. ure or vacuum display Use an accurate traceable reference to compare the readings Temperature offset may be varied 5 C in 1 C increments Vacuum offset may be varied 40 020 mBar in 0 001 mBar increments Line Voltage Alarm Points The Freeze Dryer is designed to alarm if the line voltage varies more than 10 from nominal line voltage Models rated to operate on 115V are preset to alarm if the voltage drops below approximately 103V or rises above approximately 127V Models rated to operate on 230V will alarm if the voltage drops below approximately 206V or rises above approximately 254V Some models are designed to operate below these ranges see Appendix C In these cases it is permissible to lower the low voltage alarm point to prevent nuisance alarms from occurring Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 8 Modifying Your Freeze Dryer Display Low line limit may be lowered in 5 increments of approximately 2 to 3V increments for 115V models or disabled Low line limit may be lowered in 5 increments of approximately 4 to 5V increments for 230V models or disabled High line limit may be raised in 5 increments of approximately 2 to 3V increments for 115V models or disabled High line limit may be raised in 5 increments of approximately 4 to 5V increments for 230V models or disabled Moisture Sensor Alarm The moisture sensor alarm may be disabled It is shipped enabled as the fa
62. whichever is sooner SteamScrubber amp FlaskScrubber Glassware Washers carry a two year warranty from date of installation or three years from date of shipment from Labconco whichever is sooner Blood Drawing Chairs carry a ten year warranty Carts carry a lifetime warranty Glassware is not warranted from breakage when dropped or mishandled 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 Under no circumstances shall Labconco Corporation be liable for indirect consequential or special damages of any kind This statement may be altered by a specific published amendment No individual has authorization to alter the provisions of this warranty policy or its amendments Lamps and filters are not covered by this warranty Damage due to corrosion or accidental breakage is not covered Returned or Damaged Goods Do not return goods without the prior authorization from Labconco Unauthorized returns will not be accepted If your shipment was damaged in transit you must file a claim directly with the freight carrier Labconco Corporation and its dealers are not responsible for shipping damages The United States Interstate Commerce C
63. with a soft cloth or paper towel to remove any accumulated moisture Check the collector chamber drain hose to ensure that the hose is free of moisture and that the drain plug is securely installed The Freeze Dryer will not start if moisture is detected Using a soft lint free cloth or paper towel wipe the collector chamber lid gasket to remove any dirt and contaminants that could cause a vacuum leak Vacuum grease is not required on the lid gasket to obtain a proper vacuum seal Remove the accessory drying chamber or manifold from the connection port and using a soft lint free cloth or paper towel wipe the port gasket and sealing surfaces of the drying chamber manifold to remove any dirt and contaminants that could cause a vacuum leak Reinstall the drying chamber or manifold on the port Vacuum grease is not required on the port gasket to obtain a proper vacuum seal Product Service Domestic 1 800 522 7658 International 816 333 8811 17 Chapter 4 Using Your Freeze Dryer 5 Inspect each sample valve on the accessory drying chamber or manifold and check for any visible damage and for improper installation that might cause a vacuum leak Also check that each sample valve is closed or in the vent position Vacuum Pump Ballast Setting Most vacuum pumps are equipped with a gas ballast mechanism The freeze dry process requires high vacuum Therefore it is recommended that the gas ballast be closed during the operation
64. y ice solvent trap can be used between the collector and the vacuum pump 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 Hence samples that contain volatile substances will have a greater tendency to melt particularly when placed in flasks or exposed to room temperature If a sample containing a volatile substance tends to melt when placed on a freeze dry system dilution of the sample with more water will help keep the sample frozen For example a 0 2M solution of acetic acid is much easier to freeze dry than a 0 5M solution About This Manual This manual is designed to help you learn how to install use and maintain your Freeze Dryer Instructions for performing routine maintenance and making minor modifications to your Freeze Dryer are also included Chapter 1 Introduction provides a brief overview of the Freeze Dryer explains the organization of the manual and defines the typographical conventions used in the manual 4 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction Chapter 2 Prerequ
65. yer or Freeze Dryer Tray Dryer combination to an IBM compatible computer with a 25 pin serial data port 7761500 Isolation Valve Mounts between the Stoppering Tray Dryer and the base unit which provides a way to isolate the base unit vacuum system from the Stoppering Tray Dryer vacuum system 7390702 Baffle Mounts in the collector chamber to increase ice holding capacity when operating with the vacuum control Product Service Domestic 1 800 522 7658 International 816 333 8811 57 Appendix D Freeze 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 How to select Fast Freeze Flasks for your Freeze Dry System Select Fast Freeze Flasks based on your sample sizes Flasks should be filled no more than one third of their volume so that maximum surface area is achieved and efficient lyophilization is assured A complete Fast Freeze Flask includes a rubber top glass bottom and a supply of filter paper Tops bottoms and filter paper are available separate ly as replacement components Adapters are required to attach flasks to freeze

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