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Product Service:  Domestic  1-800-522-7658, International  816-333-8811

Chapter 4: Using Your Freeze Dryer 

 

Adding Sample 

 
The following procedure should be followed when 
freeze drying: 
 
1.  Pre-freeze 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 is a freezer.  The sample container size should 
always be at least two to three times the sample size 
(i.e., 150 ml samples should be prepared in 300 ml 
containers or larger). 

2.  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. 

 

 

 

Note location of bevel on 
knob in “vacuum” position. 

Bevel in “vent” position 

Содержание FreeZone 6

Страница 1: ...55510 7753011 7753511 7754011 7754511 7755011 7755511 7753013 7753513 7754013 7754513 7755013 7755513 User s Manual LABCONCO CORPORATION 8811 PROSPECT AVENUE KANSAS CITY MO 64132 2696 800 821 5525 816...

Страница 2: ...Product designs are subject to change without notice 2002 Labconco Corporation Printed in U S A...

Страница 3: ...who sold you the product If the cause is determined to be a manufacturing fault the dealer or Labconco Corporation will repair or replace all defective parts to restore the unit to operation Under no...

Страница 4: ......

Страница 5: ...anifold Requirements 11 Space Requirements 11 Your Next Step 11 CHAPTER 3 GETTING STARTED 13 Unpacking Your Freeze Dryer 14 Freeze Dryer Components 14 Setting Up Your Freeze Dryer 16 Component Orienta...

Страница 6: ...BLESHOOTING 41 Vacuum Pump 41 Gaskets Tubing Connections Sample Valves 42 System Components Collection Chamber Isolation 44 Refrigeration Module Operation 48 APPENDIX A FREEZE DRYER COMPONENTS 49 APPE...

Страница 7: ...o install and maintain Proper care and maintenance of this product will result in many years of dependable service Freeze Dry Process Dehydration is an important process for the preservation and stora...

Страница 8: ...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...

Страница 9: ...ze 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...

Страница 10: ...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 eu...

Страница 11: ...e 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 dr...

Страница 12: ...how to attach a recorder or 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 o...

Страница 13: ...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 inf...

Страница 14: ...8 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 1 Introduction Refer to Chapter 7 Troubleshooting if you are experiencing problems with your Freeze Dryer...

Страница 15: ...he 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...

Страница 16: ...ocation 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 a...

Страница 17: ...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 samp...

Страница 18: ...12 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 2 Prerequisites...

Страница 19: ...ze 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 safel...

Страница 20: ...L 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 no...

Страница 21: ...Dryer with Purge Valve and PTFE coated Chamber 208 230V 60 Hz 12 Liter Freeze Dryer with Shell Freezer 208 230V 60 Hz 12 Liter Freeze Dryer with Shell Freezer 220 240V 50 Hz 12 Liter Freeze Dryer wit...

Страница 22: ...um Pump Connection A vacuum pump with a rated capacity of 150 liters per minute is required to operate your Freeze Dry System properly The unit is equipped with a 3 4 ID heavy wall vacuum hose for con...

Страница 23: ...y 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 vac...

Страница 24: ...cal regulations All users of this equipment are urged to become familiar with any regulations that apply in the user s area concerning the dumping of waste materials in or upon water land or air and t...

Страница 25: ...ed in Chapter 3 Getting Started you are ready 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...

Страница 26: ...mBar and collector temperature C Displays type of alarm when an alarm has occurred 3 Menu Switch This switch is used to change the display from system parameters to alarm messages 4 Vacuum Graph Disp...

Страница 27: ...art or stop the refrigeration and the Auto Mode process 9 Manual Operation Annunciator When lit the green LED indicates the Freeze Dryer unit is being controlled manually by the operator Each function...

Страница 28: ...rt and using a soft lint free cloth or paper towel wipe the port gasket and sealing surfaces of the dry chamber manifold to remove any dirt and contaminants that could cause a vacuum leak Reinstall th...

Страница 29: ...the warm pump oil is less likely to condense solvent vapors that are not trapped by the collector coil When the Freeze Dryer is operated in the Automatic Mode the purge valve and vacuum pump will ope...

Страница 30: ...quipped with the optional purge valve the vacuum pump will start two seconds after the REFRIGERATION AUTO switch is pressed The purge valves will be closed as indicated by the green annunciator above...

Страница 31: ...lve the vacuum pump may be started when the REFRIGERATION MAN switch is pressed The purge valves must be closed as indicated by the green annunciator above the PURGE switch When the collector temperat...

Страница 32: ...s and serum bottles may be frozen is a freezer The sample container size should always be at least two to three times the sample size i e 150 ml samples should be prepared in 300 ml containers or larg...

Страница 33: ...e 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 5 T...

Страница 34: ...tor will flash The display will continue to show the operating parameters of the system Press MENU to display the alarm POWER FAIL Pressing MENU multiple times will identify other alarms if they have...

Страница 35: ...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 moni...

Страница 36: ...l condensate is defrosted from the collector coil Dispose of the liquid appropriately 3 Flush the collector chamber with water and wipe chamber dry 4 If rapid defrost is desired pour warm water over t...

Страница 37: ...unciator above the switch will illuminate The shell freezer refrigeration module will start and the bath rollers will begin rotating The LCD display will show the shell freezer bath temperature Above...

Страница 38: ...32 Product Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 4 Using Your Freeze Dryer...

Страница 39: ...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 lev...

Страница 40: ...th sponge or chamois and a mild non abrasive soap or detergent clean the acrylic chamber lid 3 Using a soft cloth sponge or chamois and a mild non abrasive soap or detergent clean the exterior surface...

Страница 41: ...Freeze Dryer interpret the data received Recorder Jack Pin Configuration The system vacuum and collector temperature can be recorded during operation by connecting an appropriate device to the record...

Страница 42: ...for connection cable configuration Either of these cables can be purchased from Labconco as an accessory The part numbers for these cables are listed with the following schematics and are also listed...

Страница 43: ...TR 48 indicates the temperature of the collector in degrees Celsius VAC 0018 indicates the vacuum level of the system in mBar x 10 3 SHELL 40 indicates the temperature of the shell freezer bath RFG ON...

Страница 44: ...puter with Hyper TerminalTM 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...

Страница 45: ...Modifying Your Freeze Dryer 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 5 The Com X Prope...

Страница 46: ...uct Service Domestic 1 800 522 7658 International 816 333 8811 Chapter 6 Modifying Your Freeze Dryer 6 When the Freeze Dryer main power switch is on the data will be transmitted and updated every ten...

Страница 47: ...ng 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 elec...

Страница 48: ...the pump is capable of achieving an ultimate vacuum less than 10 x 10 3 mBar or approximately 10 microns If an inadequate vacuum reading is obtained the pump has most likely failed and may need to be...

Страница 49: ...apply vacuum grease and reinstall the valve DO NOT APPLY VACUUM GREASE TO THE GASKETS ON A DRYING CHAMBER SAMPLE VALVE If the valve still seems to be the source of the problem remove the valve and sto...

Страница 50: ...nd 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...

Страница 51: ...and slide the cover off 2 Take a 3 or 4 inch piece of vacuum hose and place it over the vacuum tube Stopper and clamp the vacuum hose to the tube Restart the system and check your vacuum indication In...

Страница 52: ...ough to cover all fittings Replace the collection chamber lid and turn on the vacuum pump Allow the vacuum pump to run for approximately 5 to 10 seconds If the vacuum pump is left on the water will be...

Страница 53: ...a second wrench to turn the nut on the bottom of the chamber Be careful not to damage the evaporator coils or the brazed joints to the refrigeration system Once the fitting is tightened perform the te...

Страница 54: ...ole Freeze Dry System can achieve a collector temperature of 50 C or lower depending on ambient temperature and humidity If the collector temperature does not reach 50 C within 40 minutes then the ref...

Страница 55: ...PP PE EN ND DI IX X A A F FR RE EE EZ ZE E D DR RY YE ER R C CO OM MP PO ON NE EN NT TS S The following pages list components that are available for your Freeze Dryer The parts shown are the most com...

Страница 56: ...losure Assembly Electrical 115V 60 Hz w Purge Valve 7515902 Enclosure Assembly Electrical 230V 50 60 Hz w Shell Freezer 7515903 Enclosure Assembly Electrical 115V 60 Hz w Shell Freezer 7515904 Enclosu...

Страница 57: ...51 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix A Freeze Dryer Components...

Страница 58: ...52 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix A Freeze Dryer Components...

Страница 59: ...53 Product Service Domestic 1 800 522 7658 International 816 333 8811 A AP PP PE EN ND DI IX X B B F FR RE EE EZ ZE E D DR RY YE ER R D DI IM ME EN NS SI IO ON NS S...

Страница 60: ...54 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix B Freeze Dryer Dimensions...

Страница 61: ...V 7 5 Amps 60 Hz 1 7754001 12 Liter Freeze Dryer 220 240V 6 5 Amps 50 Hz 1 7754003 12 Liter Freeze Dryer 208 230V 7 5 Amps 60 Hz 1 7754010 12 Liter Freeze Dryer 208 230V 7 5 Amps 60 Hz 1 7754011 12 Li...

Страница 62: ...ty 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 v...

Страница 63: ...57 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix C Freeze Dryer Specifications Wiring Diagram 115V 60 Hz Models...

Страница 64: ...58 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix C Freeze Dryer Specifications Wiring Diagram 230V 50 or 60 Hz Models...

Страница 65: ...ngle phase 7 8 amps Includes Pump Exhaust Filter 1473400 7739401 Vacuum Pump Two stage direct drive pump 195 liters minute 230 VAC 50 60 Hz single phase 4 0 amps Includes Pump Exhaust Filter 1473400 7...

Страница 66: ...e shelves 600 square inches of area provides temperature control and stoppering under vacuum 1472200 Pump Inlet Filter Disposable filter that prevents oil back streaming and protects vacuum pump from...

Страница 67: ...ap 9 high x 7 7 8 diameter 304 stainless steel with vacuum connections For use with dry ice and solvent 7538400 Secondary Vacuum Trap 7 7 8 high x 6 5 8 diameter 304 stainless steel with vacuum connec...

Страница 68: ...chamber 7522800 Provides 3 heated shelves operating at 43 C 110 F 230V 7509300 Product Heater For use in chamber 7522900 Provides 3 heated shelves operating at 43 C 110 F 115V 7509301 Product Heater F...

Страница 69: ...28 5 8 high x 5 wide x 5 deep Type 304 stainless steel with 48 each tube stems 7726500 6 Port Manifold for use with Stoppering Tray Dryer Mounts between the Stoppering Tray Dryer and the base unit an...

Страница 70: ...asily inserted between the adapter and top of the flask One hun dred filters are sup plied with each flask Compatible with all major brands of laboratory freeze dry apparatus Wide mouth opening loads...

Страница 71: ...ne rubber seal grasps top and bottom The flexible ring holds securely together during pre freezing and lyophiliza tion Compatible with all major brands of labo ratory freeze dry apparatus Flat bottom...

Страница 72: ...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 an...

Страница 73: ...d Stoppering Flat Bottom Bottom 1 ml 7572710 7570010 7570610 2 ml 7570810 7572310 4 ml 7572810 5 ml 7570210 7571010 10 ml 7571210 7571610 25 ml 7571810 50 ml 7572010 Ampule Valve Adapters 7593401 Adap...

Страница 74: ...68 Product Service Domestic 1 800 522 7658 International 816 333 8811 Appendix D Freeze Dryer Accessories...

Страница 75: ...69 Product Service Domestic 1 800 522 7658 International 816 333 8811...

Страница 76: ...are engaged Quality Control Teaching Instructional Testing Other please specify Clinical Diagnostic Research Development Production _______________________________ Of what type organization is your wo...

Страница 77: ...collect Labby Bucks and redeem for other LabbyWear merchandise Then just complete the information requested on the reverse side fold tape edges and mail LabbyWear is the official uniform of LABsters e...

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