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FreeZone 2.5 Manual cover2003
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1. 7772100 Replacement Media for Soda Acid Trap 7772700 Vacuum Pump Oil 1L For vacuum pumps 7438700 7438800 7769600 7769800 Appendix D Freeze Dryer Accessories PART DESCRIPTION 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 Trap 9 high x 7 7 8 diameter 304 stainless steel with 34 vacuum connections For use with dry ice and solvent 7522800 12 Port Drying Chamber 9 high x 7 7 8 diameter 304 stainless steel with 12 freeze dry valves 7521000 Heated Drying Chamber 10 high x 9 diameter type 304 stainless steel The 3 shelf product heaters heat to 43 C 110 F 115V 7521001 Heated Drying Chamber 10 high x 9 diameter type 304 stainless steel The 3 shelf product heaters heat to 43 C 110 F 230V 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 7443500 Clear Drying Chamber with 8 Valves For bulk drying or drying in flasks 7442100 Drying Rack Unheated Provides three shelves For use in chambers 7443500 and 7522800 7442900 Clear Drying Chamber For bulk drying 65 Appendix D Freeze Dryer Accesso
2. TO MAXIMIZE THE STABILITY OF THE CONSOLE FREEZE DRYER POSITION THE VACUUM PUMP AS CLOSE TO THE CENTER OF THE CABINET FLOOR AS POSSIBLE Chapter 3 Getting Started 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 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 hole in the collector chamber lid When vacuum is applied to the system the chamber will be held securely in place Chemical Resistance of Freeze Dryer Components 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 th
3. 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 44 Chapter 8 Modifying Your Freeze Dryer Display Press SELECT until the appropriate offset is shown Each number represents 1 C Press MENU and the display will show VACUUM OFFSET O uBar Press SELECT until the appropriate offset is shown Each number represents 0 001 mBar 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 If 3 is entered into the display the low line alarm will alarm when the voltage drops to approximately 97V ie 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 ie 206 4x3 194V There will be no alarm indicated if DISABLED is selected Press MENU and the display will show HIGH 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 high line alarm will alarm when the voltage raises to approximately 133V ie 127 2x3 133V Ifthe Freeze Dryer is operating on nominal 230V each number represents 4V if 3 is entered into the display the l
4. and concentration 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 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 dry ice solvent trap can be used between the collector and t
5. 127 60 1 6 16 100V 90 110 50 1 6 16 7670530 230V 198 254 50 1 3 13 7670531 230V 198 254 50 1 3 13 7670540 230V 187 253 60 1 3 13 7670541 230V 187 253 60 1 3 13 7670020 115V 103 127 60 1 10 5 16 100V 90 110 50 1 10 5 16 7670021 115V 103 127 60 1 10 5 16 100V 90 110 50 1 10 5 16 7670030 230V 198 254 50 1 5 3 13 7670031 230V 198 254 50 1 5 3 13 7670040 230V 187 253 60 1 5 3 13 7670041 230V 187 253 60 1 5 3 13 7420020 115V 103 127 60 1 10 5 16 100V 90 110 50 1 10 5 16 7420021 115V 103 127 60 1 10 5 16 100V 90 110 50 1 10 5 16 7420030 230V 198 254 50 1 5 3 13 7420031 230V 198 254 50 1 5 3 13 7420040 230V 187 253 60 1 5 3 13 7420041 230V 187 253 60 1 5 3 13 57 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 80 for temperatures up to 88 F 31 C decreasing linearly to 50 relative humidity at 104 F 40 C Main supply voltage fluctuations not to exceed 10 of the nominal voltage Transient overvoltages according to Installation Categories II Overvoltage 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 Used in an environment of Pollution degrees 2 i e where normally only non conductive atmospheres are present Occasionally however a tem
6. 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 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 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 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 Chapter 4 Using Your Freeze Dryer 30 CHAPTER 5 MAINTAINING Y OUR FREEZE DRYER Under normal operation the Free
7. 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 CHAPTER 9 MoDIFYING Your FREEZE DRYER DisPLAY Y our 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 temperature or vacuum display Use an accurate known reference to compare the readings to Temperature offset may be varied 5 C in 1 C increments Vacuum offset may be varied 0 010 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 mod
8. location for your Freeze Dryer accommodates the installation and operational requirements you are ready to unpack and install your Freeze Dryer Proceed to Chapter 3 Getting Started 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 Freeze 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 2 5 Liter Benchtop Freeze Dryer System weighs over 82 lbs 37 kg The Benchtop FreeZone Plus 2 5 Liter Freeze Dry System weighs over 106 lbs 48 Kg The Console FreeZone Plus 2 5 Liter Freeze Dry System weighs over 152 Ibs 69 Kg If you must lift the Freeze Dryer manually use at least two 2 persons and follow safe lifting guidelines Chapter 3 Getting Started The United States Interstate Commerce Commission rules require that claims be filed with the delivery carrier within fifteen 15 days of delivery 10 Unpacking Your Freeze Dryer Carefully unpack your Freeze Dryer and inspect it for damage that may have occurred in transit If your Freeze Dryer is damaged notify the delivery carrier immediately and retain the entire shipment intact for inspection by the carrier DO NOT RETURN GOODS WITHOUT THE PRIOR AUTHORIZATION
9. rate of freeze drying By contrast for a given surface area the thicker the sample the 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 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 condi
10. ratory freeze have 90 bend dry apparatus Required order separately Only three pieces per flask no dee or springs The complete Lyph Lock Flask m SC de The flexible ring op d holds securely igh strengt together during borosilicate pre freezing Silicone rubber glass and lyophiliza 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 EH sd 90 Bend Description Adapter 7568000 Connects 19 38 ST Flask Top to 1 2 valve 7568200 Connects 19 38 ST 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 Valves on the freeze dry systems drying 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 L abconco models and other freeze dryers Appendix D Freeze Dryer Accessories Serum Bottles and Vials Perfect for long term storage of freeze dried samples Labconco
11. second vacuum gauge capable of reading a vacuum of 0 010 mBar Itis often useful in determining if the vacuum pump is good 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 1 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 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 Chapter 7 Troubleshooting 6 When checking the sample valves pull as much vacuum as possible Ifa vacuum ind
12. 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 Shipping weight 1 Ib 0 4 kg Serum Bottle Stoppering Adapter B ody Valve Port vent de Ejector Tube Stopper 69 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 specific lyophilization requirements from tray drying to flame sealing applications Ampules Ampules are supplied in packages of 100 Size Straight Bulb Type Pre Scored Round Stopperin 9 T Flat Bottom Bottom pr lm 7572710 7570010 7570610 2ml 7570810 7572310 4ml 7572810 5 ml 7570210 7571010 10 ml 7571210 7571610 25 ml 7571810 50 ml 1512010 Appendix D Freeze Dryer Accessories 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 Ibs 1 4 kg CO Ampule Valve Adapters 7593401 Adapter connects ampules to valve ports or stainless steel stems Ten per package Shipping weig
13. 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 also not covered 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 Part 7426100 Rev A ECO C178 TABLE Or CONTENTS CHAPTER 1 INTRODUCTION Freeze Dry Process Freeze Dry Rates Freeze Dry Capacity Samples Containing Volatile Substances About This Manual Typographical Conventions Your Next Step CHAPTER 2 PREREQUISITES Electrical Requirements Location Requirements Vacuum Pump Requirements Chamber or Manifold Requirements Your Next Step CHAPTER 3 GETTING STARTED Unpacking Your Freeze Dryer Freeze Dryer Components Setting Up Your Freeze Dryer Component Orientation Vacuum Pump Connection Electric
14. 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 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 23 Chapter 4 Using Your Freeze Dryer 24 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 or in the center of the collector chamber The sample container size should always be at least two to three times the sample size i e 40 ml samples should be prepared in 80 ml containers or larger The temperature requ
15. 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 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 are equipped with a 20 Amp NEMA 5 20P plug 230V models are not equipped with a plug on the power cord It will be necessary to install a plug to match the available receptacle 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 through the rear panel and exhausts it through the sides A minimum of 3 must be allowed between the back and both sides of the Freeze Chapter 2 Prerequisites Dryer and adjacent wall surfaces Restriction of airflow during operation could adversely affect performan
16. 115 VAC 50 60 Hz single phase Includes Pump Exhaust Filter 7438800 Vacuum Pump Two stage direct drive pump 108 liters minute 230 VAC 50 60 Hz single phase Includes Pump Exhaust Filter 7769600 Vacuum Pump Chemical Resistant Two stage direct drive pump 108 liters minute 115 VAC 50 60 Hz single phase Includes Pump Exhaust Filter 7769800 Vacuum Pump Chemical Resistant Two stage direct drive pump 108 liters minute 115 VAC 50 60 Hz single phase Includes Pump Exhaust Filter 63 Appendix D Freeze Dryer Accessories 64 PART ft DESCRIPTION 1472200 Pump Inlet Filter Disposable filter that prevents oil back streaming and protects vacuum pump from submicron particles Fits vacuum pumps 1472100 and 7739402 1473400 Pump Exhaust Filter Disposable filter that removes visible oil mist and odor from vacuum pump exhaust Fits vacuum pumps 1472100 and 7739402 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 1472100 and 7739402 7438600 Replacement Filter Element Fits vacuum pumps 7438700 and 7438800 1988000 Vacuum Pump Oil 1 Liter For vacuum pumps 1472100 and 7739402 7772000 Soda Acid Trap Secondary trap that prevents migration of corrosive chemicals into vacuum pump
17. 42 43 43 43 44 44 47 53 57 57 58 59 60 63 71 CHAPTER 1 INTRODUCTION Congratulations on your purchase of a Labconco 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 prep procedures 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 microorganisms 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 materials by converting the frozen water directly into its 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
18. 8VI ei ole YOSNIS MIL ani ANGA ATNO 32383438 404 VIG FLON u m 038 V QVOT83A0 9 amp 61 Wiring Diagram Catalog 7670030 7670031 7670040 7670041 and 7420030 7420031 7420040 and 7420041 230V 50 or 60 Hz Appendix C Freeze Dryer Specifications Models LINN INIDIAYIS OL YOIYA E ke 09 GR 394nos YIMOd MOYA 1293NNOOSIQ JOVISVI YILM S Z ANO 373384 PY ONINSVM AVSOVIG INISIM 979 sva 09NOJ99V1 LOS LZpL Nd UY3Y N d SS3NUVH Nd YW3Y A 9 28 NO SN340 JUNSSIVA HIH IHM V i 3918 YOSSIVdMOD e AAPP E amp E 8 6 340 NO N3MOd AV138 RI IN WNNIVA o o 1HM Bfl 1HM 11 1114971 N d SSINYVH O N 20A0 n El ATEO U U YOSNIS 3unisioM id A D AT A WOSN3S AL 03Y 8v ATNO 328383434 804 VIG 310N Vic IAA QA r4 bono E i a Ta HM Y ene gu KS D n S e rell Do DD PET dl E D ETE Y APPENDIX D FREEZE DRYER ACCESSORIES The following accessories are available for the Freeze Dryer PART DESCRIPTION 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 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 1473400 7438700 Vacuum Pump Two stage direct drive pump 108 liters minute
19. OF LABCONCO UNAUTHORIZED RETURNS WILL NOT BE ACCEPTED 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 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 Freeze Dryer you received in the following table Verify that the components listed are present and undamaged Chapter 3 Getting Started Catalog Product Description 7670520 2 5 Liter Benchtop Freeze Dryer 115V 60 Hz 7670521 2 5 Liter Benchtop Freeze Dryer with Teflon Coated Chamber 115V 60 Hz 7670530 2 5 Liter Benchtop Freeze Dryer 220 240V 50 Hz 7670531 2 5 Liter Benchtop Freeze Dryer with Teflon Coated Chamber 220 240V 50 Hz 7670540 2 5 Liter Benchtop Freeze Dryer 208 230V 60 Hz 7670541 2 5 Liter Benchtop Freeze Dryer with Teflon Coated Chamber 208 230V 60 Hz 7670020 2 5 Liter Benchtop Cascade Freeze Dryer 115V 60 Hz 7670021 2 5 Liter Benchtop Cascade Freeze Dryer with Teflon Coated Chamber 115V 60 Hz 7670030 2 5 Liter Benchtop Cascade Freeze Dryer 220 240V 50 Hz 7670031 2 5 Liter Benchtop Cascade Freeze Dryer with Teflon Coated Chamber 220 240V 50 Hz 7670040 2 5 Liter Benchtop Cascade Freeze Dryer 208 230V 60 Hz 7670041 2 5 Liter Benchtop Casca
20. 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 ports on drying chambers and manifolds Serum Bottles Serum Bottles Stoppers and Seals are supplied in pack ages of 100 Size 20 mm 13 mm Split Aluminum Sleeve Type Corkage Corkage Stoppers Seals Stoppers 2ml 1515010 1516010 7577010 3ml 7575210 7576010 7577010 5 ml 7573010 7576210 7577110 7577510 10 ml 7573210 7576210 7577110 7577510 20 ml 7573410 7576210 7577110 7577510 30 ml 7573610 7576210 7577110 7577510 50 ml 7573810 7576210 7577110 7577510 100ml 7574010 7576210 7577110 7577510 125ml 7574210 7576210 7577110 7577510 Threaded Vials Stoppers and Threaded Vials with Screw Caps are supplied in packages of 200 ollm i M Size Vials with Stoppers Screw Caps 5ml 7162300 1162200 10 ml 1162600 1162200 A Accessories Seal Crimper Secures tear away Aluminum Seals 7578000 Seal Crimper for 13 mm corkage Shipping weight 3 Ibs 1 4 kg 7578100 Seal Crimper for 20 mm corkage Shipping weight 3 lbs 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
21. T 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 e Press SELECT to return to display operating parameters or after a short delay the display will automatically switch to show operating parameters Baffle The cylindrical plastic component shipped with Cascade Freeze Dryers Models 76700XX and 74200X is a baffle which is designed to evenly distribute collected ice over the entire collector coil Proper positioning of the baffle is required to achieve maximum ice loading capabilities The baffle installs into the collection chamber with the flat flange upward The large boss on the flange should be positioned toward the rear of the chamber 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 system When the collector reaches 40 C the vacuum pump will start The Temperature and Vacuum Graph 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 20 mBar the vacuum display will indicate HI At 20 mBar and below the display will show the actual vacuum Chapter 4 Using Your Freeze Dryer When the system vacuum is between 0 450 and 0 133 mBar the lower green va
22. User s Manual FreeZone0 1 Liter Benchtop Freeze Dry Systems Models 7740020 7740021 7740030 7740031 7740040 7740041 Labconco s Mascot Labby the LABster Protecting vour VA laboratory environment V LABCONCO For more information please contact us E mail sales expotechusa com Website www ExpotechUSA com FreeZone is a registered trademark of Labconco Corporation 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 Delta Series Biological Safety Cabinets and PuriCare Lab Animal Products carry a three year warranty from date of installation or four years from date of shipment from Labconco whichever is sooner e Carts carry a lifetime warranty e 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
23. 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 Check that each sample valve is closed or in the vent position 19 Chapter 4 Using Your Freeze Dryer 20 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 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 mBa
24. al Connection Drying Chamber or Drying Manifold Installation Chemical Resistance of Freeze Dryer Components Solvent Safety Precautions Your Next Step CHAPTER 4 USING YOUR FREEZE DRYER Freeze Dryer Controls Operation Checklist Vacuum Pump Ballast Setting Operating the Freeze Dryer Set Up Baffle Automatic Start Up GAA KR P Y NN F Fa O0 O0 OO N N I 10 10 11 12 12 13 13 13 15 16 17 18 19 20 20 20 22 22 Manual Start Up Setting the Operating Vacuum Pre Freezing Samples Adding Sample Shut Down 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 Wiring Diagram 115V Wiring Diagram 230V APPENDIX D FREEZE DRYER ACCESSORIES DECLARATION OF CONFORMITY 23 23 24 24 26 26 Z 27 28 28 28 29 31 33 33 37 37 38 40
25. andled 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 15 Chapter 3 Getting Started 16 materials in or upon water land or air and to comply with such regulations Your Next Step The installation and setup of your Freeze Dryer is now complete To learn how to load and operate your Freeze Dryer proceed to Chapter 4 Using Your Freeze Dryer To perform additional diagnostics on your Freeze Dryer proceed to Chapter 7 Troubleshooting To learn about the maintenance requirements for your Freeze Dryer proceed to Chapter 5 Maintaining Your Freeze Dryer 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 understand the display e connect samples Do not use the Freeze Dryer in a manner not specified by the manufacturer refer to Appendix C Freeze Dryer Specifications The electrical protection properties of the Freeze Dryer may be impaired if the Freeze Dryer is used inappro
26. ast Freeze Flask cleans easily has only two components I e a high strength Horizontal shell borosilicate 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 a flexible non contaminating T silicone rubber Available in nine top convenient sizes No vacuum grease is necessary Flat bottom No threads reduces spills hooks or springs provides better are needed balance Entire flask may be autoclaved Adapters Add the Adapters for connecting the Fast Freeze Flasksto the valve ports on your drying chamber or manifold Choose borosilicate glass or stainless steel adapters in 1 2 and 3 4 diameters EE 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 EECH 7544810 pieta Filter Paper 1000 10 packages of 100 1 diameter 28mm Pore size 17 microns Shipping weight 0 5 Ib 67 Appendix D Freeze Dryer Accessories Lyph Lock Flasks Lyph Lock Flasks simplify your lyophilization procedures because they have only three pi
27. bbyWear of your choice Please select from one of the three items listed or collect Labby Bucks and redeem for other LabbyWear merchandise Then just complete the information requested on the reverse side fold tape edges and mail Labby The LABster A T shirt 100 cotton short sleeved white with Labby The LABster embroidered on the front left side Specify unisex size UA Large Q XLarge Q Twill cap Pigment dyed two color with six panels and Labby The LABster embroidered on the front Q Lunch bag Insulated teal with royal blue accent and Labby The LABster embroidered on the front A 10 Labby Bucks and LabbyWear Catalog For more information please contact us E mail sales expotechusa com Website www ExpotechUSA com
28. ce IT IS RECOMMENDED THAT THE CONSOLE MODEL FREEZE DRYER IS SECURELY ATTACHED TO THE FLOOR AFTER IT IS LOCATED WHERE IT WILL BE USED THIS WILL PREVENT ACCIDENTAL TIPPING AND POSSIBLE INJURY SEE INSTRUCTIONS IN CHAPTER 3 GETTING STARTED 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 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 86 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 Vacuum pumps used with 115V models should be equipped with a 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 or manifold 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 Your Next Step After you have determined that the
29. cuum graph LED will flash When the system vacuum level is lt 0 133 mBar the green LED will be lit steadily indicating that most samples may be added 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 Graph 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 20 mBar the vacuum display will indicate HI At 20 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 lt 0 133 mBar the 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
30. de Freeze Dryer with Teflon Coated Chamber 208 230V 60 Hz 7420020 2 5 Liter Console Cascade Freeze Dryer 115V 60 Hz 7420021 2 5 Liter Console Cascade Freeze Dryer with Teflon Coated Chamber 115V 60 Hz 7420030 2 5 Liter Console Cascade Freeze Dryer 220 240V 50 Hz 7420031 2 5 Liter Console Cascade Freeze Dryer with Teflon Coated Chamber 220 240V 50 Hz 7420040 2 5 Liter Console Cascade Freeze Dryer 208 230V 60 Hz 7420041 2 5 Liter Console Cascade Freeze Dryer with Teflon Coated Chamber 208 230V 60 Hz Plus the Following Part Component Description 7426100 User s Manual 1336400 Power Cord 115V or 1337300 Power Cord 230V 1291000 Plug 230V models only 7646000 Vacuum Hose 1967600 Hose Clamps 2 7690000 Lid Chamber 7688500 Lid Gasket 7419300 Baffle Cascade Models Only 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 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 11 Chapter 3 Getting Started 12 Component Orientation The refrigeration system in the Freeze Dryer draws air in through the rear of the cabinet and exhausts air out through the sides A minimum of 3 should be allowed between the back and sides of the Fre
31. e 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 right 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 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
32. e major components of the FreeZone Freeze Dry System that are susceptible to degradation are as follows 13 Chapter 3 Getting Started Acids Buffers Solvents 2 a 5 E v 3 do 2 E E S lt m a s 2 2 T oe cH 2 B 8 3 2 3 2 A B m A ea w Q lt 5 S g E v D D dan 2 o a E z S E gt 2 S E o s o E E 2 3 o 3 5D 8 BS E o e fam S e o o Ki m 5 Component Material End SS O A A GR m Valve Stem Acetal C D D D D Delrin Collector Acrylic D D D Lid Hoses Neoprene C D D c 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 C Moderate degradation Limited use D Severe degradation infrequent use recommended immediate thorough cleaning required e Most common compounds used in freeze dying processes if allowed to enter the vacuum pump will degrade the oil and cause damage to the vacuum pump e Sugars and proteins typically will have minimal negative effect on any of the materials of construction An accessory glass lid is available 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 mus
33. eces 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 EEE ON Flask Complete Complete Flask Flask Lyph Lock Flask Dimensions Size Flask Fla Top Top Seal Bottom Flask Bottom 19 38 ST 24 40 ST 19 38 ST 20 40 ST HxID 25ml 7550000 7554000 7552000 7556000 75590 00 7557000 37mmx34mm 50ml 7550200 7554200 7552000 7556000 7559000 7557200 67 mm x 34 mm 100 ml 7550400 7554400 7552200 7556200 7559200 7557400 50 mm x 59 2mm 250ml 7550600 7554600 7552200 7556200 7559200 7557600 110 mm x 59 2 mm 500 ml 7550800 7554800 7552400 7556400 7559400 7557800 103 mm x 90 2 mm 750ml 7550900 7554900 7552400 7556400 7559400 7557900 145 mm x 90 2 mm 1000 ml 7551000 7555000 7552400 7556400 7559400 7558000 187 mm x 90 2 mm Tl Borosilicate glass Compatible with adapters with all major either 19 38 or 24 40 brands of labo standard taper joints
34. els 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 43 Chapter 8 Modifying Your Freeze Dryer Display Low line limit may be lowered in 5 steps in approximately 2 to 3V increments for 115V models or disabled Low line limit may be lowered in 5 steps in approximately 4 to SV increments for 230V models or disabled High line limit may be raised in 5 steps in approximately 2 to 3V increments for 115V models or disabled High line limit may be raised in 5 Steps in approximately 4 to SV increments for 230V models or disabled Moisture Sensor Alarm The moisture sensor alarm may be disabled Itis shipped enabled as the factory 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 If you want to restore all factory settings 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
35. eze Dryer and the adjacent wall surface Restriction of the airflow through the cabinet during operation could adversely affect performance After the console model is positioned at the location where it will be operated it should be securely attached to the floor Use 2 1 4 x 5 0 long wood screws or lag bolts if the floor is wood or concrete anchors if the floor is concrete Two 312 diameter holes are located in the floor of the lower cabinet Using these holes as a template mark the floor directly under the two holes Roll the Console Freeze Dryer aside and drill suitable pilot holes for the selected screws anchors Install the vacuum pump prior to securing the Console Freeze Dryer to the floor Roll the Console Freeze Dryer back into position and install the screws anchors through the holes in the cabinet floor and into the building floor FAILURE TO ATTACH THE CONSOLE FREEZE DRYER TO THE FLOOR COULD RESULT IN ACCIDENTAL TIPPING AND POSSIBLE INJURY Vacuum Pump Connection A vacuum pump as described in Chapter 2 Prerequisites 18 required to operate your Freeze 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 models For console models from the back of the unit place the vacuum pump on the floor of the cabinet
36. g 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 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 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 27 Chapter 4 Using Your Freeze Dryer 28 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
37. he 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 freeze drying 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 Chapter 1 Introduction Chapter 2 Prerequisites explains what you need to do to prepare your site before you install your Freeze Dryer Electrical requiremen
38. he Labconco Freeze Dryer The purpose of the RS232 interface is to send data to a data collection computer to monitor the state and activity of the Freeze Dryer This data is half duplex data The data properties are as follows 1 Data Rate 2400 Baud 2 8 Bit word length 3 1 Start bit 1 Stop bit 4 No parity is transmitted 5 Standard ASCII character set 33 Chapter 6 Using the RS232 Receptacle KEE eee OB GM MI GRUT 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 Temperature AN Collector Temperature in Celsius V Vacuum 18 Vacuum Level in Micro Bars SF Shell Freezer 9 Feature not installed or out of range C Drying Chamber Temperature PG Purge 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 catalog regarding the latest software available The following describes how to use an IBM compatible computer with Hyper Ter
39. hown 1337300 Power Cord 230V Not Shown 14 7445400 Vacuum Sensor 15 7515300 Temperature Sensor Not Shown 16 7419600 Wire Harness Power 115V Not Shown 7419700 Wire Harness Power 230V Not Shown 17 7432700 Vacuum Control Bleed Valve 18 7429700 Moisture Sensor 19 7418400 Wire Harness Control 115V and 230V Not Shown Appendix A Freeze Dryer Components PU PU PM 3 MUM E Ke MU HHHH a MUM a i i AAA GE DOWN Y e SI Appendix A Freeze Dryer Components Models 76700xx and 74200xx Item PartNo Description 1 7688500 Lid Gasket 2 7690000 Lid 3 7435800 Back Panel Assembly 115V 7435900 Back Panel Assembly 230V 4 7953800 Motor Fan 115V 7953801 Motor Fan 230V 5 7437700 Compressor 115V 60 Hz Lo Stage 7437701 Compressor 230V 50 Hz Lo Stage 7437702 Compressor 230V 60 Hz Lo Stage 7591800 Compressor 115V 60 Hz Hi Stage 7591801 Compressor 230V 50 Hz Hi Stage 7591802 Compressor 230V 60 Hz Hi Stage 1302300 Switch 7426000 Control Panel Label 00 I AN 7445500 PC Board 9 7728000 Drain Plug 10 1643600 O Ring 11 7424100 Drain Hose 12 7646000 Vacuum Hose Not Shown 13 1336400 Power Cord 115V Not Shown 1337300 Power Cord 230V Not Shown 14 7445400 Vacuum Sensor Not Shown 15 7515300 Temperature Sensor Co
40. ht 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 Register Online Go to P RO D U CT R EG ST RATIO N CA R D www labconco com productreg html By registering your product you will receive these important benefits Warranty Confirmation Product Registration e Product Protection Free LabbyWear Merchandise NAME TITLE DEPARTMENT INSTITUTION ADDRESS CITY STATE ZIP COUNTRY TELEPHONE EXT FAX E MAIL Which of the following comes closest to describing the type of activity in which you are engaged Q Quality Control Q Teaching Instructional Q Testing Q Other please specify Q Clinical Diagnostic C Research amp Development Q Production Of what type organization is your work a part A Industrial Manufacturing Utility A Government except Medical Q Educational Institution except Medical School A Independent Foundation Consulting C Medical Medical School Hospital Public Health Q Other please specify Which comes closest to describing your scientific discipli
41. ication 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 The illustrations below show how the sample valve installs on a chamber and a manifold Manifold Assembly Valve Body Bulkhead Nut Knob amp Stem Valve Body Trim Ring Knob amp Stem Thrust Washer Gasket Bulkhead Assembly Assembly No grease Fitting required Valve Assembly Manifold Valve Assembly Chamber 39 Chapter 7 Troubleshooting Ill System Components and Collection Chamber Isolation This test determines if the source of a leak is in the drying chamber 1 Remove the drying chamber or manifold 2 Leave the gasket on and turn a large freeze dry flask upside down and 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 Sa
42. ired for pre freezing is 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 After connecting a pre frozen sample to a valve turn the plastic valve knob to the VACUUM position to open the valve which connects the attached sample to system vacuum The bevel on the knob should be positioned toward the sample port Chapter 4 Using Your Freeze Dryer Bevel in vent position Vent Backfill Port Bevel in vacuum position 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 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 To remove a container after drying is complete turn the plastic knob on the valve to the VENT position which closes the valve and ve
43. ll melt off the collector coil 2 Remove the collector chamber top 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 side of the cabinet Dispose of the liquid appropriately Utilization of acid requires immediate cleaning and neutralization after defrost or physical damage to the collector chamber and collector coil will result LA 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 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 had occurred The following out of specification conditions will initiate an alarm Power Failure If a power failure occurs durin
44. llector Not Shown 16 7427500 Wire Harness 115V Not Shown 7427501 Wire Harness 230V Not Shown 17 7432700 Vacuum Control Bleed Valve 18 7429700 Moisture Sensor 19 7418400 Wire Harness Control 115V and 230V Not Shown 50 Appendix A Freeze Dryer Components Models 76700xx and 74200xx Te og MUMMY MMMM MATET HEIE AAA 51 Appendix A Freeze Dryer Components 52 APPENDIX B FREEzE DRYER DIMENSIONS Model 76705xx INCHES ICENTIMETERSI cse o c c c c c c c ce c c gt c c e 53 Appendix B Freeze Dryer Dimensions Model 76700xx INCHES CENTIMETERS 0000000000000000000000 0000000000000000000000 54 Appendix B Freeze Dryer Dimensions Model 74200xx INCHES CENTIMETERS c c e c c c c 55 Appendix B Freeze Dryer Dimensions 56 APPENDIX C FREEZE DRYER SPECIFICATIONS This Appendix contains technical information about the Freeze Dryer including electrical specifications environmental operating conditions and wiring diagrams Electrical Specifications Catalog Voltage Frequency Phase Amperage Nominal Max with Nominal Operating ud Vacuum Range Vacuum Pump Pump 7670520 115V 103 127 60 1 6 16 100V 90 110 50 1 6 16 7670521 115V 103
45. minal software included with Windows 95 98 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 i WindowsQ 95 or 98 use START PROGRAMS ACCESSORIES ii Windows 2000 use START ROGRAMS ACCESSORIES COMMUNICATIONS 34 Chapter 6 Using the RS232 Receptacle The first time Hyper Terminal is opened a dialogue box requesting an area code and phone number will appear Enter the appropriate numbers and continue 3 The Connection Description dialogue box will open Type in a user defined name and select an icon for the new connection Press OK 4 The Connect To dialogue box will open Using the down arrow selection button select the communication port to which the cable has been connected Press OK 35 Chapter 6 Using the RS232 Receptacle 5 The Com X Properties dialogue box will open Enter the appropriate data properties and press OK 6 When the Freeze Dryer main power switch is on the data will be transmitted and updated at the time intervals selected by the user LABCONCO HyperTerminal SF 999C 999PG 9 gt SF 999C 999PG 9 gt SF 999C 999PG 9 gt SF 999C 999PG 9 gt B lt T 40Y 18 SF 999C 999PG 9 gt 36 CHAPTER 7 TROUBLESHOOTING Refer to
46. mple Valves Freeze Dry Flask Gasket Isolating the freeze dry system from the accessory chamber manifold 40 Chapter 7 Troubleshooting The next test determines if a vacuum leak is in the collection chamber l 2 Insert a rubber stopper in the small hole in the rear of the chamber Start the Freeze Dryer and observe the vacuum indication If the vacuum is good the problem is in the collection chamber If it is bad the problem is in the plumbing connections from the collection chamber to the vacuum pump If the leak is in the chamber check the drain hose hose connections and the drain plug If the leak is in the plumbing connections check all rubber parts fittings and clamps Stopper Checking the connections to the pump and the vacuum tube 41 Chapter 7 Troubleshooting 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 vacuum pump is operating depending on ambient temperature and humidity FreeZone Cascade Freeze Dry Systems should achieve a collector temperature of 84 C or lower when the vacuum pump is operating Ifthe collector temperature does not reach the design temperature within 40 minutes then the refrigeration module is not functioning properly If any repairs are required on the refrigeration module contact your local laboratory supply
47. ne O Biological Science A Inorganic Chemistry O Physical Chemistry Q Bio Chemistry Q Analytical Chemistry R amp D C Engineering or Physics Q Polymer Chemistry Q Analytical Chemistry Quality Control Q Other please specify A Organic Chemistry Which FreeZone 1 Liter Freeze Dry System did you purchase O Model 7740020 A Model 7740021 A Model 7740030 Q Model 7740031 Q Model 7740040 Q Model 7740041 Serial Number Date of Installation Model and serial numbers are located on the back of the unit How did you learn about the FreeZone Freeze Dry System Q Dealer Sales Rep Q Dealer Catalog C Colleague O Advertisement C Labconco Sales Rep Q Labconco Literature O Trade Show UO Internet WWW Q Other please specify What factors most influenced your decision to purchase a FreeZone Freeze Dry System Number up to 3 1 being the most important Appearance Reputation Service Program __ Performance Specifications __ Ease of Operation __ Safety Features __ Price __ Dealer Recommendation __ Availability __ Colleague Recommendation Other please specify From whom did you purchase your FreeZone Freeze Dry System DEALER Please fold card over tape edges and mail No postage is required FREEZONE FREEZE DRY SYSTEMS My REV 8 03 LabbyWear is the official uniform of LABsters everywhere Be a LABster As a token of our thanks for returning your Product Registration Card we would like to send you the La
48. nts 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 knob should point away from the sample port 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 is recommended 25 Chapter 4 Using Your Freeze Dryer 26 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 right 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 left hand side of the Freeze Dryer and remove the drain plug Place the drain hose in a suitable container to collect the condensate that wi
49. 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 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 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 three 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 SR SE 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 guantities 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
50. ow line alarm will alarm when the voltage drops to approximately 266V ie 254 4x3 266V There will be no alarm indicated if DISABLED is selected Press MENU and the display will show MOISTURE SENSOR INSTALLED 45 Chapter 8 Modifying Your Freeze Dryer Display Press and hold SELECT if you want to disable the moisture sensor Press MENU and the display will again show PRODUCTION MENU MASTER RESET Press and hold MENU until display shows PASSWORD Wait approximately 10 seconds and the display will default to the main freeze dry display information 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 47 Appendix A Freeze Dryer Components Model 76705xx Item Part No Description 1 7688500 Lid Gasket 2 7690000 Lid 3 7435800 Back Panel Assembly 115V 7435900 Back Panel Assembly 230V 4 7953800 Motor Fan 115V 7953801 Motor Fan 230V 5 7437700 Compressor 115V 60 Hz 7437701 Compressor 230V 50 Hz 7437702 Compressor 230V 60 Hz 6 1302300 Switch 7 7426000 Control Panel Label 8 7445500 PC Board 9 7728000 Drain Plug 10 1643600 O Ring 11 7645904 Drain Hose 12 7646000 Vacuum Hose Not Shown 13 1336400 Power Cord 115V Not S
51. porary conductivity caused by condensation must be expected in accordance with IEC 664 Appendix C Freeze Drver Specifications Wiring Diagram Catalog 7670520 and 7670521 115V 60 Hz Models 8 01 AYT38 annava B 01141171 N d SSINYVH Nd UVIN Y A38 0086 4 N d ZH 0S AO00 ZH 09 AGII VILT GZ AUG 323383 WVYOVIC ONISIM OJNOJAV 328NOS YIMOS WOYI 193NN Wa im ININIVM YOSSIYAMOI x S NY4 1HM BYR L N d WOSN3S dil 94 f MAL AWO 39NGW34TM NOS VId LLON Appendix C Freeze Dryer Specifications Wiring Diagram Catalog 7670530 7670531 7670540 and 7670541 230V 50 or 60 Hz Models Lt VACUUM iT VALVE EI U 12v0c MOISTURE SENSOR d HARNESS P N 7418400 REAR PNL z Za Cp 25 az lt WARNING DISCONNECT FROM POWER SOURCE PRIOR TO 60 HZ 230V Y P N 7419900 REV A LABCONCO PREEDE DRY 25 UTER Appendix C Freeze Drver Specifications Wiring Diagram Catalog 7670020 7670021 7570020 7570021 and 7420020 7420021 115V 60 Hz Models LINN ONIOIAY3S OL 40 4d ZH ocho EH 328NOS YIMOd MOYA 193NNOOSIQ 30V9SVI N31ll SZ ANG 323394 ONINSVM AYHDVIG ONIJIM OJNOJAV O0GLT L Nd UVU N d SS3NUVH mc ae AV130 NING Na 1311n0 WNNIVA 1HM QZ onj 18 01 AV138 de WANIYA 00 8IrL N d SS3NNVH NW A8NISIOW r TE 09N028Y1 O N 20461 H n E Q0334
52. priately 17 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 Ja bl U LNICOINCGO O o NN o 5 ei s BE d m O 1 LCD Display Displays system operating parameters and 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 Each function must be started by the operator 8 Auto Mode Switch Used to start or stop the refrigeration and the Auto Mode process 9 Auto Mode Indicator When lit the green LED indicates that the Freeze Dryer is in the Auto Mode In this mode the vacuum pump will start when the collector temperature reaches 40 C 10 11 12 13 Chapter 4 Using Your Freeze Dryer Vacuum Graph Display This display indicates the relative system vacuum level Th
53. r 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 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 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 Your Next Step If your Freeze Dryer needs to be installed proceed to Chapter 2 Prerequisites to ensure your installation site meets all of the requirements Then go to Chapter 3 Getting Started for instructions on how to install your Freeze Dryer and make all of the necessary connections For information on the operational characteristics of your Freeze Dryer go to Chapter 4 Using Your Freeze Dryer If your Freeze Dryer is installed and you need to perform routine maintenance on the Freeze Dryer proceed to Chapter 5 Maintaining Your Freeze Dryer Refer to Chapter 7 Troubleshooting if you are experiencing problems with your Freeze Dryer CHAPTER 2 PREREQUISITES Before you install your Freeze Dryer you need to prepare
54. r 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 e Press SELECT until the desired vacuum operating level is displayed e If 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 Chapter 4 Using Your Freeze Dryer e Press MENU e The display will show TEMPERATURE UNITS E F 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 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 The display will show the vacuum pump hours VACUUM TOTAL HOUR XXXX SERVICE HOUR XXXX e To reset the SERVICE HOUR to 0 press SELECT e The display will show 21 Chapter 4 Using Your Freeze Dryer 22 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 SELEC
55. ries PART DESCRIPTION 7522300 20 Port Manifold 10 high x 27 W wide x 8 5 8 deep Type 304 stainless steel manifold with 20 freeze dry valves 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 7522900 16 Port Drying Chamber 13 high x 138 diameter 304 stainless steel with 16 freeze dry valves 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 dry val
56. t be changed if it is cloudy shows particles or is discolored The Chapter 3 Getting Started 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 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 specific compounds in the Freeze Dryer contact Labconco Technical Service at 1 800 821 5525 or 816 333 8811 or e mail labconco labconco com o Solvent Safety Precautions Solvents used in the Freeze Dryer may be flammable or hazardous Use extreme caution and keep sources of ignition away from the solvents When using flammable or hazardous solvents the vacuum pump should be vented to or operated inside a fume hood Hazardous materials such as strong acids or bases radioactive substances and volatile organics must be h
57. the following 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 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 I 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 37 Chapter 7 Troubleshooting 38 Check the oil level in the pump Ensure it is filled to the correct level Check vacuum hose connections from the pump to the Freeze Dryer and try running the unit If vacuum problems continue consider obtaining a
58. tion Using a soft cloth sponge or chamois and a mild non abrasive soap or detergent clean the acrylic chamber lid 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 l 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 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 mBar 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 t
59. tions a good vacuum is essential to maintain an efficient rate In many applications the maintenance of a vacuum of 0 133 mBar or less is recommended The rate of freeze drying is directly proportional to the vapor pressure and the vapor pressure is dependent upon both eutectic temperature and solute concentration of the sample 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
60. ts 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 3 Maintaining Your Freeze Dryer explains how to perform routine maintenance on your Freeze Dryer Chapter 6 Using the Computer Jack 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 explains how to recalibrate your Freeze Dryer display 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 A wiring diagram for the Freeze Dryer is also included Appendix D Freeze Dryer Accessories lists the part numbers and descriptions of all of the accessories available for your Freeze Dryer Chapter 1 Introduction Typographical Conventions Recognizing the following typographical conventions will help you understand and use this manual e Book chapte
61. ve ports Flask Complete Flask Flask Flask Top Dimensions Size Flask Bottom Top Adapter Flask Bottom Diameter HxD 40 ml 7540000 7542000 7544000 i 76 mm x34 mm 80 ml 7540200 7542200 7544000 12 115 mm x34 mm 120 ml 7540300 7542300 75442 00 3 4 68 mm x59 2 mm 150ml 7540400 7542400 7544200 3 4 85mmx59 2 mm 300 ml 7540600 7542600 7544200 34 145 mm x 59 2 mm 600m 7540800 7542800 7544400 3 4 135 mm x 90 2 mm 900 ml 7540900 7542900 7544400 3 4 190 mm x 90 2 mm 1200 ml 7541000 7543000 7544400 3 4 240 mm x 90 2 mm 2000 ml 7541200 7543200 7544400 3 4 380 mm x 90 2 mm Valves on the freeze dry systems drying 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 L abconco mod els and other freeze dryers Variety of adapters Gs Compatible with available You may S all major brands of select from glass or p laboratory freeze dry stainless steel if apparatus adapters available straight or with 45 i No complex filter bend Reguired retainer is necessary order separately For those who use filters they are easily Top seals easily The inserted between the flexible silicone rubber adapter and top of top snaps on and off the flask One hun easily yet provides a dred filters are sup reliable high vacuum plied with each flask seal B Only two pieces per ase Wide mouth The complete opening loads fast F
62. ze 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 starting the vacuum pump 7 If chamber or manifold 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 31 Chapter 5 Maintaining Your Freeze Dryer Monthly l Ps 3 The rubber components on the Freeze Dryer may eventually deteriorate and require replacement The effective life of rubber parts depends upon both their usage and the surrounding environment Check all rubber hoses and gaskets and replace any that show signs of hardening permanent set or deteriora
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