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Chapter 1: Introduction

 

 

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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 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 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 
may be used between the collector and the vacuum pump. 

 

 

Содержание FreeZone 76700 Series

Страница 1: ...tes complete your product registration card online at register labconco com User s Manual Please read the User s Manual before operating the equipment Labconco Corporation 8811 Prospect Avenue Kansas...

Страница 2: ...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 hou...

Страница 3: ...GETTING STARTED 8 Unpacking Your Freeze Dryer 9 Freeze Dryer Components 9 Setting Up Your Freeze Dryer 11 Component Orientation 11 Vacuum Pump Connection 11 Electrical Connection 12 Drying Chamber or...

Страница 4: ...TROUBLESHOOTING 32 Vacuum Pump 32 Gaskets Tubing Connections Sample Valves 33 System Components Collection Chamber Isolation 35 Refrigeration Module Operation 37 CHAPTER 8 MODIFYING YOUR FREEZE DRYER...

Страница 5: ......

Страница 6: ...ively 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 demonstra...

Страница 7: ...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...

Страница 8: ...ystem With any given instrument the capacity is based on the surface area of the sample the eutectic temperature and concentration of the sample and the rate and amount of heat transferred to the froz...

Страница 9: ...intenance 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...

Страница 10: ...y 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 Important information is presented...

Страница 11: ...let 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 11...

Страница 12: ...table 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...

Страница 13: ...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...

Страница 14: ...CEPTED 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 T...

Страница 15: ...enchtop Cascade Freeze Dryer 230 60 X 7670041 2 5L Benchtop Cascade Freeze Dryer 230 60 X X 7670060 2 5L Benchtop Cascade Freeze Dryer 230 50 X 7670061 2 5L Benchtop Cascade Freeze Dryer 230 50 X X 76...

Страница 16: ...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 th...

Страница 17: ...cuum 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 o...

Страница 18: ...damage to the vacuum pump Sugars and proteins typically will have minimal negative effect on any of the materials of construction When using compounds in the Freeze Dryer that are hostile to the mater...

Страница 19: ...lvents 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 vacu...

Страница 20: ...to begin using your Freeze Dryer Read this chapter to learn how to operate the controls understand the display connect samples Do not use the Freeze Dryer in a manner not specified by the manufacturer...

Страница 21: ...efrigeration 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 functio...

Страница 22: ...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 4 Remove the accessory drying chamber or m...

Страница 23: ...Press SELECT until the desired vacuum operating level is displayed See Setting the Operating Vacuum Level for guidelines If 0 is selected the vacuum control is disabled and the vacuum level in the Fre...

Страница 24: ...press SELECT The display will show If you want to reset the service hours to 0 continue to hold SELECT five seconds until hours are reset Press SELECT The display will show the RS 232 data transmissi...

Страница 25: ...um 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 M...

Страница 26: ...7 Fungi 40 and Colder 50 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...

Страница 27: ...quired 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...

Страница 28: ...cal damage to the collector chamber and collector coil will result 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...

Страница 29: ...When an alarm occurs press MENU and the display will show 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 n...

Страница 30: ...the operation of the Freeze Dryer The pump oil should be regularly monitored to verify that it is clean Moisture in Collector If there is liquid in the collector chamber and either a REFRIGERATION but...

Страница 31: ...bove 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 af...

Страница 32: ...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...

Страница 33: ...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 wit...

Страница 34: ...ure not available on 2 5L models PG Purge not available on 2 5L models There are several commercially available software packages which can read RS232 data and enter the data into a computer program s...

Страница 35: ...ode 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 Pr...

Страница 36: ...33 8811 or 1 800 522 7658 31 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 transmitt...

Страница 37: ...trical 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 wi...

Страница 38: ...plug is installed and the tube appears to be in good condition 4 Check all rubber vacuum tubing for signs of deterioration or cracking 5 Check all connections and make sure they are secure and leak ti...

Страница 39: ...chamber and a manifold Thrust Washer Valve Body Knob Stem Assembly Valve Body Trim Ring Manifold Assembly Knob Stem Assembly Bulkhead Nut Gasket No grease required Bulkhead Fitting Valve Body Thrust W...

Страница 40: ...er 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 g...

Страница 41: ...ttom 2 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 collecti...

Страница 42: ...ystem has a compressor condenser capillary tube metering device and an evaporator During the operation the evaporator of the high stage system refrigerates the condenser of the low stage system This t...

Страница 43: ...pare the readings Temperature offset may be varied 5 C in 1 C increments Vacuum offset may be varied 0 020 mBar in 0 001 mBar increments Line Voltage Alarm Points The Freeze Dryer is designed to alarm...

Страница 44: ...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 Vac...

Страница 45: ...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 MEN...

Страница 46: ...to change the status Press MENU and the display will show 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...

Страница 47: ...00 522 7658 42 In order to store offsets in memory you Must Press and Hold MENU until display shows Wait approximately 10 seconds and the display will default to the main freeze dry display informatio...

Страница 48: ...7658 43 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 require...

Страница 49: ...l 8 7445500 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 E...

Страница 50: ...Appendix A Freeze Dryer Components Product Service 816 333 8811 or 1 800 522 7658 45 Model 76705xx 1 2 17 18 9 10 14 3 4 5 6 11 8 7...

Страница 51: ...e Stage 7591806 Compressor 230V 50 Hz Single Stage 7591807 Compressor 230V 60 Hz Single Stage 6 1302300 Switch 7 7426000 Control Panel Label 8 7445590 Printed Circuit Board 9 7728000 Drain Plug 10 164...

Страница 52: ...Appendix A Freeze Dryer Components Product Service 816 333 8811 or 1 800 522 7658 47 Models 76700xx and 74200xx 5 1 2 14 18 9 10 3 4 17 5 7 8 6...

Страница 53: ...Product Service 1 800 522 7658 48 APPENDIX B FREEZE DRYER DIMENSIONS Model 76705xx...

Страница 54: ...Appendix B Freeze Dryer Dimensions Product Service 816 333 8811 or 1 800 522 7658 49 Model 76700xx...

Страница 55: ...Appendix B Freeze Dryer Dimensions Product Service 816 333 8811 or 1 800 522 7658 50 Model 74200xx...

Страница 56: ...50 1 6 14 7670530 230V 198 254 50 1 2 5 7 7670531 230V 198 254 50 1 2 5 7 7670540 230V 187 253 60 1 2 5 7 7670541 230V 187 253 60 1 2 5 7 7670560 230V 198 254 50 1 2 5 7 7670561 230V 198 254 50 1 2 5...

Страница 57: ...1 10 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 decre...

Страница 58: ...ect drive pump 195 liters minute 115 VAC 50 60 Hz single phase Includes Pump Exhaust Filter Cat 1473400 7739403 Vacuum Pump Two stage direct drive pump 195 liters minute 230 VAC 50 60 Hz single phase...

Страница 59: ...dor Pump Exhaust Filter package of 5 Fits pump exhaust filter 1473400 or vacuum pumps 1472100 and 7739402 1988000 Vacuum Pump Oil 1 Liter A molecularly distilled hydrocarbon oil with low vapor pressur...

Страница 60: ...e and solvent Cools to approximately 75 C 7522800 12 Port Drying Chamber 9 high x 7 7 8 diameter 304 stainless steel with 12 freeze dry valves 7509200 Product Heater For use in chamber 7522800 Provide...

Страница 61: ...5 deep Type 304 stainless steel with 48 each 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 sta...

Страница 62: ...Appendix D Freeze Dryer Accessories Product Service 816 333 8811 or 1 800 522 7658 57...

Страница 63: ...Appendix D Freeze Dryer Accessories Product Service 816 333 8811 or 1 800 522 7658 58...

Страница 64: ...Appendix D Freeze Dryer Accessories Product Service 816 333 8811 or 1 800 522 7658 59...

Страница 65: ...Appendix D Freeze Dryer Accessories Product Service 816 333 8811 or 1 800 522 7658 60 Ampules...

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