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ABLE

ONTENTS

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

CHAPTER

GETTING

STARTED

Unpacking

Your

Freeze

Dryer

Freeze

Dryer

Components

Setting

Your

Freeze

Dryer

Component

Orientation 11

Vacuum

Pump

Connection

Electrical

Connection

Drying Chamber or Drying Manifold Installation

Chemical Resistance of Freeze Dryer Components

Solvent

Safety

Precautions

CHAPTER 4: USING YOUR FREEZE DRYER

Freeze

Dryer

Controls

Operation

Checklist

Vacuum

Pump

Ballast

Setting

Operating

the

Freeze

Dryer

Set-Up

Baffle

Automatic

Start-Up

Manual Start-Up

Setting

the

Operating

Vacuum

Level

Содержание FreeZone 74200 Series

Страница 1: ...ates 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 City MO 64132 2696 800 821 5525 816 333 8811 FAX 816 363 0130 E MAIL labconco labconco com HOME PAGE www labconco com ...

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 hours of 7 00 a m and 6 00 p m Central Standard Time Part 7426100 Rev I ECO J719 Warranty Labconco provides a warranty on all parts and factory workmanship The warranty includes areas of defective mater...

Страница 3: ...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 Drying Manifold Installation 12 Chemical Resistance of Freeze Dryer Components 12 Solvent Safety Precautions 14 CHAPTER 4 USING YOUR FREEZE DRYER 15 Freeze Dryer Controls 16 Operation Checklist 17 V...

Страница 4: ...7 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 DISPLAY 38 Temperature and Vacuum Display 38 Line Voltage Alarm Points 38 Moisture Sensor Alarm 39 Modifying the Display 39 APPENDIX A FREEZE DRYER COMPONENTS 43 APPENDIX B FREEZE DRYER DIMENSIONS 4...

Страница 5: ......

Страница 6: ...sively used in the development of pharmaceuticals e g antibiotics and preservation of biologicals e g proteins plasma viruses and cell lines The nondestructive nature of this process has been demonstrated by the retention of viability in freeze dried viruses and microorganisms Freeze drying is a process whereby water or other solvent is removed from frozen material by converting the frozen water d...

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 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 decreas...

Страница 8: ...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 bec...

Страница 9: ...aintenance 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 2 Prerequisites explains what you need to do to prepare your site before you install your Freeze Dryer Electrical requirements are discussed ...

Страница 10: ...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 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 St...

Страница 11: ...tlet 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 Various power cord configurations are provided with 230V models If this does not match the available receptacle remove this plug and replace it wi...

Страница 12: ...itable for 3 4 ID vacuum hose which is provided It is recommended that the vacuum pump is equipped with an exhaust filter to minimize oil mist exhausting from the vacuum pump The operating vacuum level may be set on the Freeze Dryer The higher the pressure is set the more likely it is that oil mist will be exhausted Vacuum pumps used with 115V models should be equipped with a 115V 15 Amp NEMA 5 15...

Страница 13: ...r 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 lbs 69 Kg If you must lift the Fre...

Страница 14: ...CCEPTED 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...

Страница 15: ...Benchtop 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 7670070 2 5L Benchtop Cascade Freeze Dryer 230 50 X 7670071 2 5L Benchtop Cascade Freeze Dryer 230 50 X X 7420020 2 5L Console Cascade Freeze Dryer 115 60 X 7420021 2 5L Console Cascade Freeze Dryer 11...

Страница 16: ...g 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 Dr...

Страница 17: ...acuum pump power cord if necessary Electrical Connection Plug the power cord into the receptacle on the back of the Freeze Dryer and plug the other end into a suitable power receptacle Drying Chamber or Drying Manifold Installation The drying chamber or drying manifold purchased separately may be positioned directly above the 3 inch hole in the collector chamber lid When vacuum is applied to the s...

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 materials of construction it is imperative the equipment is thoroughly cleaned after use Rubber and plastic components that have been exposed to damaging compounds should be removed and flushed with water...

Страница 19: ...olvents used in the Freeze Dryer may be flammable or hazardous to your health Use extreme caution and keep sources of ignition away from the solvents When using flammable or hazardous solvents the vacuum pump must be vented to or operated inside a fume hood Hazardous materials such as strong acids or bases radioactive substances and volatile organics must be handled carefully and promptly cleaned ...

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 refer to Appendix C Freeze Dryer Specifications The electrical protection properties of the Freeze Dryer may be impaired if the Freeze Dryer is used inappropriately ...

Страница 21: ...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 ...

Страница 22: ...r 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 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 coul...

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 Freeze Dry System will be determined by the capabilities of the vacuum pump Press MENU The display will show Press SELECT until the desired units are flashing Press MENU The display will show VACUUM UNI...

Страница 24: ...0 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 transmission rate To change the rate press SELECT until the desired time interval is shown The time between data transmissions may be set to occur at 10 30 60 300 or 600 second intervals Press MENU to return t...

Страница 25: ...uum 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 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 tem...

Страница 26: ...77 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 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...

Страница 27: ...equired connect the gas supply line to the vent port on the valve before turning the plastic knob on the valve to vent position The sample container may now be removed In the vent position the bevel on the valve knob should point away from the sample port 5 Ampules may be flame sealed while connected to a valve by using a sealing torch Care must be taken not to burn the valve An insulation materia...

Страница 28: ...ical 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 is liquid in the collector chamber This could result in damage to the vacuum pump Alarms A number of unusual events may occur during a lyophilization procedure that can adversely effect the operation...

Страница 29: ...d 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 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 l...

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 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 When the collector is drained the alarm will self cancel This...

Страница 31: ...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 ...

Страница 32: ...s and polishes may be used on the exterior surfaces Do not use solvents to remove stains from the exterior surfaces as they may damage the finish Annually 1 Every 12 months or more often if the Freeze Dryer is operated in a dusty environment the refrigeration system condenser should be cleaned Using a vacuum cleaner with brush attachment clean the condenser to ensure proper airflow for peak perfor...

Страница 33: ...e a connecting cable below 1 Computers with a 25 pin D sub male serial connector should use Connect Cable Labconco part number 7537801 to connect a computer to the Labconco Freeze Dryer 2 Computers with a 9 pin D sub male serial connector should use Connect Cable Labconco part number 7537800 to connect a computer to the Labconco Freeze Dryer The purpose of the RS232 interface is to send data to a ...

Страница 34: ...ture 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 such as a word processor to create a text file or spreadsheet to tabulate and plot the data Consult your laboratory supply dealer regarding the latest software available The following describes how to...

Страница 35: ...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 ...

Страница 36: ...333 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 transmitted and updated at the time intervals selected by the user ...

Страница 37: ...ctrical 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...

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 tight 6 When checking the sample valves pull as much vacuum as possible If a vacuum indication is displayed wiggle or rotate the valves and watch the gauge for any fluctuations Fluctuations can indicat...

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 Washer Valve Assembly Manifold Valve Assembly Stainless Steel Chamber Valve Body Knob Stem Assembly Valve Assembly Clear Chamber with Valves ...

Страница 40: ...ber or manifold 2 Leave the gasket on and turn a large freeze dry flask upside down to cover the connection port 3 Start the Freeze Dryer and observe the vacuum indication If the vacuum indication is good then the problem is in the drying chamber or manifold and you should return to Section II Gaskets Tubing Connections Sample Valves Freeze Dry Flask Isolating the freeze dry system from the access...

Страница 41: ...ottom 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 collection chamber to the vacuum pump 3 If the leak is in the chamber check the drain hose hose connections and the drain plug 4 If the leak is in the plumbing connections check all rubber parts fittings and...

Страница 42: ...system 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 takes place in the heat exchanger The low stage and high stage systems are balanced by design however sometimes that balance can be disrupted during operation and the unit will not function properly I...

Страница 43: ...mpare 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 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 ...

Страница 44: ...a Master Reset because all offsets and configurations that have been entered will be lost If you must perform a Master Reset hold SELECT approximately 5 seconds This will reset Vacuum units to mBar Vacuum set point to 0 mBar Temperature units to C Refrigeration total hours to 0 Vacuum pump total hours to 0 RS232 transmission rate to 10 seconds Temperature offset to 0 C Vacuum offset to 0 mBar Low ...

Страница 45: ...V if 3 is entered into the display the low line alarm will alarm when the voltage drops to approximately 194V for example 206 4x3 194V There will be no alarm indicated if DISABLED is selected Press MENU and the display will show Press SELECT until the appropriate offset is shown If the Freeze Dryer is operating on nominal 115V each number represents 2V If 3 is entered into the display the high lin...

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 information If you do not want to set Total Hours press MENU and the display will show The routine will repeat by pressing MENU or wait approximately 10 seconds for the display to default to the main...

Страница 47: ...800 522 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 information This can be done anytime throughout the Modifying the Display routine PASSWORD ...

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 required contact Product Service ...

Страница 49: ...el 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 EU Not Shown 1342100 Power Cord 230V 60 Hz Not Shown 1332601 Power Cord 230V 50Hz UK Not Shown 1332701 Power Cord 230V 50Hz China Not Shown 14 7445400 Vacuum Sensor 15 7515300 Temperature Sensor Not S...

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: ...le 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 1643600 O Ring 11 7645906 Drain Hose 12 7373450 Vacuum Hose Not Shown 13 1336400 Power Cord 115V 60Hz Not Shown 1336500 Power Cord 230V 50Hz EU Not Shown 1342100 Power Cord 230V 60 Hz Not Shown 1332601 ...

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: ...0 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 7 7670570 230V 198 254 50 1 2 5 7 7670571 230V 198 254 50 1 2 5 7 7670020 115V 103 127 60 1 10 0 16 100V 90 110 50 1 10 0 16 7670021 115V 103 127 60 1 10 0 16 100V 90 110 50 1 10 0 16 7670030 230V 1...

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 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 Overvoltag...

Страница 58: ...rect 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 Includes Pump Exhaust Filter Cat 1473400 7584000 Vacuum Pump Chemical Resistant Hybrid Combination two stage rotary vane pump and two stage chemistry diaphragm pump 98 115 liters minute 115 VAC 50 60...

Страница 59: ...Odor 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 pressure For vacuum pumps 1472100 and 7739402 7772000 Soda Acid Trap Secondary trap that prevents migration of corrosive chemicals into vacuum pump 7772100 Replacement Media for Soda Acid Trap 7772700 Vacuu...

Страница 60: ...ce 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 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...

Страница 61: ...x 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 stainless steel with 16 freeze dry valves 7419300 Baffle Mounts in the collector chamber to increase ice holding capacity when operating with the vacuum control ...

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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