User’s Manual
FreeZone 2.5 Liter Freeze Dry Systems
Models
74200 Series
76700 Series
76705 Series
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Labconco Corporation
8811 Prospect Avenue Kansas City, MO 64132-2696 800-821-5525, 816-333-8811 FAX 816-363-0130
E-MAIL labconco@labconco.com HOME PAGE www.labconco.com
Please read the User’s Manual before operating the equipment.
Copyright © 2004, 2007, 2012, 2013, 2014 Labconco Corporation. All rights reserved.
The information contained in this manual and the accompanying products are copyrighted and all rights reserved by Labconco Corporation. Labconco Corporation reserves the right to make periodic design changes without obligation to notify any person or entity of such change.
Warranty
Labconco provides a warranty on all parts and factory workmanship. The warranty includes areas of defective material and workmanship, provided such defect results from normal and proper use of the equipment. Glassware is not warranted from breakage when dropped or mishandled.
The warranty for FreeZone® Freeze Dry Systems will expire one year from date of installation or two years from date of shipment from Labconco, whichever is sooner. Warranty is non-transferable and only applies to the owner (organization) of record.
This limited warranty covers parts and labor, but not transportation and insurance charges. In the event of a warranty claim, contact Labconco Corporation or the dealer who sold you the product. If the cause is determined to be a manufacturing fault, the dealer or Labconco Corporation will repair or replace all defective parts to restore the unit to operation. Under no circumstances shall Labconco Corporation be liable for indirect, consequential, or special damages of any kind. This statement may be altered by a specific published amendment. No individual has authorization to alter the provisions of this warranty policy or its amendments. Lamps and filters are not covered by this warranty. Damage due to corrosion or accidental breakage is not covered.
Returned or Damaged Goods
Do not return goods without the prior authorization from Labconco. Unauthorized returns will not be accepted. If your shipment was damaged in transit, you must file a claim directly with the freight carrier. Labconco Corporation and its dealers are not responsible for shipping damages.
The United States Interstate Commerce Commission rules require that claims be filed with the delivery carrier within fifteen (15) days of delivery.
Limitation of Liability
The disposal and/or emission of substances used in connection with this equipment may be governed by various federal, state, or local regulations. All users of this equipment are required to become familiar with any regulations that apply in the user’s area concerning the dumping of waste materials in or upon water, land, or air and to comply with such regulations. Labconco Corporation is held harmless with respect to user’s compliance with such regulations.
Contacting Labconco Corporation
If you have questions that are not addressed in this manual, or if you need technical assistance, contact
Labconco’s Customer Service Department or Labconco’s Product Service Department at 1-800-821-5525 or 1-816-333-8811, between the hours of 7:00 a.m. and 6:00 p.m., Central Standard Time.
Part #7426100, Rev. H
ECO J323
TABLE OF CONTENTS
CHAPTER 1: INTRODUCTION |
1 |
Freeze Dry Process |
1 |
Freeze Dry Rates |
2 |
Freeze Dry Capacity |
3 |
Samples Containing Volatile Substances |
4 |
About This Manual |
4 |
Typographical Conventions |
5 |
Your Next Step |
5 |
CHAPTER 2: PREREQUISITES |
6 |
Electrical Requirements |
6 |
Location Requirements |
6 |
Vacuum Pump Requirements |
7 |
Chamber or Manifold Requirements |
7 |
CHAPTER 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 |
Vacuum Pump Ballast Setting |
17 |
Operating the Freeze Dryer |
17 |
Set-Up |
17 |
Baffle |
20 |
Automatic Start-Up |
20 |
Manual Start-Up |
20 |
Setting the Operating Vacuum Level |
20 |
Pre-Freezing Samples |
21 |
Adding Sample |
21 |
Shut Down |
22 |
Defrosting |
23 |
Alarms |
23 |
Power Failure |
23 |
Line Voltage Out of Range |
24 |
Temperature Out of Range |
24 |
Service Vacuum Pump |
25 |
Moisture in Collector |
25 |
CHAPTER 5: MAINTAINING YOUR FREEZE DRYER |
26 |
CHAPTER 6: USING THE RS232 RECEPTACLE |
28 |
Computer Connection for Computer Interface |
28 |
CHAPTER 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 |
48 |
APPENDIX C: FREEZE DRYER SPECIFICATIONS |
51 |
Electrical Specifications |
51 |
Environmental Conditions |
52 |
APPENDIX D: FREEZE DRYER ACCESSORIES |
53 |
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 preparation and for the preservation and storage of biologicals, pharmaceuticals and foods. Of the various methods of dehydration, freeze drying (lyophilization) is especially suited for substances that are heat sensitive. Other than food processing (e.g., coffee, whole dinners), freeze drying has been extensively used in the development of pharmaceuticals (e.g., antibiotics) and preservation of biologicals (e.g., proteins, plasma, viruses and cell lines). The nondestructive nature of this process has been demonstrated by the retention of viability in freeze dried viruses and microorganisms.
Freeze drying is a process whereby water or other solvent is removed from frozen material by converting the frozen water directly into vapor without the intermediate formation of liquid water. The basis for this sublimation process involves the absorption of heat by the frozen sample in order to vaporize the ice; the use of a vacuum pump to enhance the removal of water vapor from the surface of the sample; the transfer of water vapor to a collector; and the removal of heat 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
ice and the heat removed from the collector to convert the water vapor into ice.
Product Service 1-800-522-7658 |
1 |
Chapter 1: Introduction
Freeze Dry Rates
The efficiency of the Freeze Drying process is dependent upon the surface area and the thickness of the sample, the collector temperature and vacuum obtained, the eutectic point and solute concentration of the sample. It is important to remember these factors when trying to obtain efficient utilization of your Freeze Dry system. A listing of selected materials and their approximate drying times are shown in Table 1 for your reference.
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Table 1 |
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SAFE TEMPERATURE AND DRYING TIMES |
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FOR SELECTED MATERIALS |
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Material |
Safe |
Collector |
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Hours |
10mm Thick |
Temperature |
Temperature |
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(Approx.) |
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°C |
°C |
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Milk |
-5 |
-40 |
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10 |
Urea |
-7 |
-40 |
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10 |
Blood Plasma |
-10 to -25 |
-40 |
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16 |
Serum |
-25 |
-40 |
|
18 |
Vaccinia |
-30 to -40 |
-50 |
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22 |
Influenza Vaccine |
-30 |
-50 |
|
24 |
Human Tissue |
-30 to -40 |
-50 |
|
48 |
Vegetable Tissue |
-50 |
-80 |
|
60 |
*Total sample quantities are contingent on various freeze dryer capacities.
Up to the point of overloading the system, the greater the surface area of the sample, the faster the rate of freeze drying. By contrast, for a given surface area, the thicker the sample 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 sample. The volume of the freeze dry flask should be two to three times the volume of the sample.
In order for lyophilization to occur, ice must be removed from the frozen sample via sublimation. This is accomplished by the collector and the vacuum pump. The collector, which should be at least 15 to 20°C colder than the eutectic temperature (melting temperature) of the sample, traps vapor as ice. Since the vapor pressure at the collector is lower than that of the sample, the flow of water vapor is from the sample to the collector. Since this vapor diffusion process occurs very slowly under normal atmospheric conditions, a good vacuum is essential to maintain an
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Product Service 816-333-8811 or 1-800-522-7658 |
Chapter 1: Introduction
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.
Product Service 816-333-8811 or 1-800-522-7658 |
3 |
Chapter 1: Introduction
Samples Containing Volatile Substances
In certain cases the solvent in a sample to be freeze dried may contain volatile components such as acetonitrile, methanol, acetic acid, formic acid or pyridine. In addition to these substances having an effect on the eutectic temperature, they may increase the vapor pressure at the surface of the sample. Also, compared to water, they will require the absorption of less heat for sublimation to occur. Hence, samples that contain volatile substances will have a greater tendency to melt, particularly when placed in flasks or exposed to room temperature. If a sample containing a volatile substance tends to melt when placed on a freeze dry system, dilution of the sample with more water will help keep the sample frozen. For example, a 0.2M solution of acetic acid is much easier to freeze dry than a 0.5M solution.
About This Manual
This manual is designed to help you learn how to install, use, and maintain your Freeze Dryer. Instructions for performing routine maintenance and making minor modifications to your Freeze Dryer are also included.
Chapter 1: Introduction provides a brief overview of the Freeze Dryer, explains the organization of the manual, and defines the typographical conventions used in the manual.
Chapter 2: Prerequisites explains what you need to do to prepare your site before you install your Freeze Dryer. Electrical requirements are discussed.
Chapter 3: Getting Started contains the information you need to properly unpack, inspect and install your Freeze Dryer.
Chapter 4: Using Your Freeze Dryer discusses the basic operation of your Freeze Dryer. Information on how to attach samples and run the Freeze Dryer is included.
Chapter 5: Maintaining Your Freeze Dryer explains how to perform routine maintenance on your Freeze Dryer.
Chapter 6: Using the RS232 Receptacle describes how to connect a computer for monitoring the operation.
Chapter 7: Troubleshooting contains a table of problems you may encounter while using your Freeze Dryer, including the probable causes of the problems, and suggested corrective actions.
Chapter 8: Modifying Your Freeze Dryer Display explains how to recalibrate your Freeze Dryer display.
Appendix A: Freeze Dryer Components contains labeled diagrams of the components of the Freeze Dryer.
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Product Service 816-333-8811 or 1-800-522-7658 |
Chapter 1: Introduction
!
Appendix B: Freeze Dryer Dimensions contains comprehensive diagrams showing the dimensions for the Freeze Dryer.
Appendix C: Freeze Dryer Specifications contains product specifications.
Appendix D: Freeze Dryer Accessories lists the part numbers and descriptions of all of the accessories available for your Freeze Dryer.
Typographical Conventions
Recognizing the following typographical conventions will help you understand and use this manual:
Book, chapter, and section titles are shown in italic type (e.g., Chapter 3: Getting Started).
Steps required to perform a task are presented in a numbered format.
Comments located in the margins provide suggestions, reminders, and references.
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.
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.
Product Service 816-333-8811 or 1-800-522-7658 |
5 |
CHAPTER 2
PREREQUISITES
Before you install your Freeze Dryer, you need to prepare your site for installation. Carefully examine the location where you intend to install your Freeze Dryer. You must be certain that the area is level and of solid construction. An electrical source must be located near the installation site.
Carefully read this chapter to learn:
the electrical supply requirements.
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. Various power cord configurations are provided with 230V models. If this does not match the available receptacle, remove this plug and replace it with an approved plug of the suitable style.
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 Dryer and adjacent wall surfaces. Restriction of airflow during operation could adversely affect performance.
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Product Service 1-800-522-7658 |
Chapter 2: Prerequisites
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.IT IS RECOMMENDED THAT THE CONSOLE MODEL
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. 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 5-15P 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.
Product Service 816-333-8811 or 1-800-522-7658 |
7 |
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.
!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 Freeze Dryer manually, use at least two (2) persons and follow safe lifting guidelines.The FreeZone 2.5 Liter Benchtop Freeze Dryer System weighs
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Product Service 1-800-522-7658 |
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.
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.
AUTHORIZATION OF LABCONCO. UNAUTHORIZED RETURNS WILL NOT BE ACCEPTED.DO NOT RETURN GOODS WITHOUT THE PRIOR
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.IF YOUR FREEZE DRYER WAS DAMAGED IN TRANSIT,
Freeze Dryer Components
Locate the model of Freeze Dryer you received in the following table. Verify that the components listed are present and undamaged.
Product Service 816-333-8811 or 1-800-522-7658 |
9 |
Chapter 3: Getting Started
Power Cords
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PTFE |
1336400 |
1336500 |
1342100 |
1332601 |
1332701 |
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Coated |
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Catalog # |
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Description |
Volts |
Hz |
Chamber |
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7670520 |
2.5L Benchtop Freeze Dryer |
115 |
60 |
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X |
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7670521 |
2.5L Benchtop Freeze Dryer |
115 |
60 |
X |
X |
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7670530 |
2.5L Benchtop Freeze Dryer |
230 |
50 |
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X |
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7670531 |
2.5L Benchtop Freeze Dryer |
230 |
50 |
X |
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X |
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7670540 |
2.5L Benchtop Freeze Dryer |
230 |
60 |
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X |
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7670541 |
2.5L Benchtop Freeze Dryer |
230 |
60 |
X |
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X |
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7670560 |
2.5L Benchtop Freeze Dryer |
230 |
50 |
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X |
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7670561 |
2.5L Benchtop Freeze Dryer |
230 |
50 |
X |
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X |
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7670570 |
2.5L Benchtop Freeze Dryer |
230 |
50 |
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X |
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7670571 |
2.5L Benchtop Freeze Dryer |
230 |
50 |
X |
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X |
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7670020 |
2.5L Benchtop Cascade Freeze Dryer |
115 |
60 |
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X |
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7670021 |
2.5L Benchtop Cascade Freeze Dryer |
115 |
60 |
X |
X |
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7670030 |
2.5L Benchtop Cascade Freeze Dryer |
230 |
50 |
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X |
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7670031 |
2.5L Benchtop Cascade Freeze Dryer |
230 |
50 |
X |
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X |
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7670040 |
2.5L Benchtop Cascade Freeze Dryer |
230 |
60 |
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X |
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7670041 |
2.5L Benchtop Cascade Freeze Dryer |
230 |
60 |
X |
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X |
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7670060 |
2.5L Benchtop Cascade Freeze Dryer |
230 |
50 |
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X |
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7670061 |
2.5L Benchtop Cascade Freeze Dryer |
230 |
50 |
X |
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X |
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7670070 |
2.5L Benchtop Cascade Freeze Dryer |
230 |
50 |
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X |
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7670071 |
2.5L Benchtop Cascade Freeze Dryer |
230 |
50 |
X |
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X |
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7420020 |
2.5L |
Console Cascade Freeze Dryer |
115 |
60 |
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X |
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7420021 |
2.5L |
Console Cascade Freeze Dryer |
115 |
60 |
X |
X |
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7420030 |
2.5L |
Console Cascade Freeze Dryer |
230 |
50 |
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X |
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7420031 |
2.5L |
Console Cascade Freeze Dryer |
230 |
50 |
X |
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X |
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7420040 |
2.5L |
Console Cascade Freeze Dryer |
230 |
60 |
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X |
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7420041 |
2.5L |
Console Cascade Freeze Dryer |
230 |
60 |
X |
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X |
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7420060 |
2.5L |
Console Cascade Freeze Dryer |
230 |
50 |
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X |
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7420061 |
2.5L |
Console Cascade Freeze Dryer |
230 |
50 |
X |
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X |
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7420070 |
2.5L |
Console Cascade Freeze Dryer |
230 |
50 |
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X |
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7420071 |
2.5L |
Console Cascade Freeze Dryer |
230 |
50 |
X |
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X |
Plus the following: |
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Part # |
Component Description |
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7426100 |
User’s Manual |
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1291000 |
Plug (230V models only) |
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7373450 |
Vacuum Hose |
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1488800 |
Hose Clamps (2) |
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7395801 |
Chamber Lid |
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7395800 |
Lid Gasket |
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7419300 |
Baffle (Cascade Models Only) |
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7386901 |
Fitting |
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Product Service 816-333-8811 or 1-800-522-7658 |
Chapter 3: Getting Started
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.
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 Freeze 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.
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FAILURE TO ATTACH THE CONSOLE FREEZE DRYER TO |
THE FLOOR COULD RESULT IN ACCIDENTAL TIPPING |
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AND POSSIBLE INJURY |
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Vacuum Pump Connection
A vacuum pump as described in Chapter 2: Prerequisites is 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.
!Makelevel. certain that the oil in the vacuum pump is at the proper
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.
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Chapter 3: Getting Started
DRYER, POSITION THE VACUUM PUMP AS CLOSE TO THE CENTER OF THE CABINET FLOOR AS POSSIBLE.TO MAXIMIZE THE STABILITY OF THE CONSOLE FREEZE
Connect the vacuum pump power cord to the receptacle on the back of the cabinet labeled “vacuum pump.” If the vacuum pump has an off/on switch, turn the switch on. The vacuum pump will be controlled by the Freeze Dryer. Connect the vacuum pump inlet port to the vacuum tube on the back of the cabinet with the vacuum hose and clamps provided. If necessary, cut the hose to proper length to allow for gentle bends without kinks.
Models rated for use on 230V have a reverse IEC connector for attaching the vacuum pump power cord. A plug is supplied that can be installed on the vacuum pump power cord if necessary.
Electrical Connection
Plug the power cord into the receptacle on the back of the Freeze Dryer and plug the other end into a suitable power receptacle.
Drying Chamber or Drying Manifold Installation
The drying chamber or drying manifold, purchased separately, may be positioned directly above the 3-inch 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 the major components of the FreeZone Freeze Dry System that are susceptible to degradation are as follows:
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Product Service 816-333-8811 or 1-800-522-7658 |
Chapter 3: Getting Started
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Solvents |
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Acetic Acid 20% |
Formic Acid |
Trifluoroacetic Acid (TFA) |
Calcium Chloride |
Sodium Phosphate |
Acetone |
Acetonittirle |
Carbon Tetrochloride |
Cyclohexane |
Dioxane |
Methyl t-Butyl Ether (BTBE) |
Pyridine |
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Valve Stem |
Acetal |
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D |
D |
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Collector |
Acrylic |
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D |
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Lid |
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Hoses, |
Neoprene |
C |
D |
D |
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D |
D |
D |
C |
D |
Gaskets & |
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Valve |
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Bodies |
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Flask Top |
Silicon |
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C |
D |
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C |
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Rubber |
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Chamber & |
Stainless |
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C |
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Fittings |
Steel |
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C – Moderate degradation; Limited use
D – Severe degradation; infrequent use recommended; immediate thorough cleaning required.
Most common compounds used in freeze drying processes, if allowed to enter the vacuum pump, will degrade the oil and cause damage to the vacuum pump.
Sugars and proteins typically will have minimal negative effect on any of the materials 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.
The oil in the vacuum pump should be checked often. It must be changed if it is cloudy, shows particles or is discolored. The useful life of vacuum pump oil can be extended if the vacuum pump is operated for an extended period of time after a freeze dry run. This allows contaminants to be purged from the hot oil. This must be done with the inlet to the pump blocked off to prevent air from free flowing through the pump. If the pump is operated at an elevated vacuum level (> 10mBar), oil may be expelled from the pump and damage could occur.
Product Service 816-333-8811 or 1-800-522-7658 |
13 |
Chapter 3: Getting Started
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.
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Solvent Safety Precautions |
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Solvents used in the Freeze Dryer may be flammable or |
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hazardous to your health. Use extreme caution and keep |
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sources of ignition away from the solvents. When using |
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flammable or hazardous solvents, the vacuum pump must be |
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vented to or operated inside a fume hood. |
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Hazardous materials such as strong acids or bases, radioactive |
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substances and volatile organics must be handled carefully and |
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promptly cleaned up if spilled. If a sample is spilled in the |
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collector chamber it must immediately be cleaned up. |
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WARNING: The disposal of substances used in connection with |
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this equipment may be governed by various Federal, State or |
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local regulations. All users of this equipment are urged to |
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become familiar with any regulations that apply in the user’s |
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area concerning the dumping of waste materials in or upon |
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water, land or air and to comply with such regulations. |
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Product Service 816-333-8811 or 1-800-522-7658 |
CHAPTER 4
USING 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:
operate the controls.
understand the display.
connect samples.
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Do not use the Freeze Dryer in a manner not specified by the |
manufacturer (refer to Appendix C: Freeze Dryer |
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Specifications). The electrical protection properties of the |
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Freeze Dryer may be impaired if the Freeze Dryer is used |
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inappropriately. |
Product Service 1-800-522-7658 |
15 |
Chapter 4: Using Your Freeze Dryer
Freeze Dryer Controls
The control panel for the Freeze Dryer is shown below with a description about its function.
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1.LCD Display – Displays system operating parameters, set-up parameters and alarm messages.
2.Menu Switch – This switch is used to change the display from operating system parameters to set-up parameters.
3.Select Switch – Used to select set-up parameters.
4.Vacuum Switch – Used to start or stop the vacuum pump when operating in manual start-up mode.
5.Vacuum Indicator – This green LED indicates that power is being supplied to the vacuum pump receptacle on the back of the Freeze Dryer.
6.Manual Refrigeration Switch – Used to start only the refrigeration module.
7.Manual Operation Indicator – When lit, the green LED indicates the Freeze Dryer is being controlled manually by the operator. 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 Auto Mode. In this mode, the vacuum pump will start when the collector temperature reaches –40°C.
10.Vacuum Graph Display – This display indicates the relative system vacuum level. The highest LED indicates that the vacuum level is above 2.0 mBar. The indicators will sequence down when the vacuum level reaches 2.0, 1.0, 0.8, 0.6, 0.45, 0.12 mBar. The lower green LED flashes when the system vacuum level is 0.45 to 0.12 mBar and illuminates steadily below 0.133 mBar.
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Product Service 816-333-8811 or 1-800-522-7658 |
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