Labconco FreeZone Bulk Tray Dryer User Manual
FreeZone
Models
78060 Series
User’s Manual
®
Bulk Tray Dryers
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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, 2010, 2012, 2013 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.
The warranty for all Labconco products will expire one year from date of installation or two years from
date of shipment from Labconco, whichever is sooner, except the following;
• Purifier® Logic® Biological Safety Cabinets and PuriCare® Lab Animal Research Stations
carry a three-year warranty from date of installation or four years from date of shipment from
Labconco, whichever is sooner.
• SteamScrubber® & FlaskScrubber® Glassware Washers carry a two-year warranty from date
of installation or three years from date of shipment from Labconco, whichever is sooner.
• Blood Drawing Chairs carry a ten year warranty.
• Carts carry a lifetime warranty.
• Glassware is not warranted from breakage when dropped or mishandled.
This limited warranty covers parts and labor, but not transportation and insurance charges. In the event
of a warranty claim, contact Labconco Corporation or the dealer who sold you the product. If the cause
is determined to be a manufacturing fault, the dealer or Labconco Corporation will repair or replace all
defective parts to restore the 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 #7594900 Rev. F
ECO H435
T
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T
CHAPTER 1: INTRODUCTION 1
Freeze Dry Process 1
Freeze Dry Rates 2
Freeze Dry Capacity 3
Samples Containing Volatile Substances 4
CHAPTER 2: PREREQUISITES 4
Electrical Requirements 4
Location Requirements 4
Vacuum Pump Requirements 5
CHAPTER 3: GETTING STARTED 6
Unpacking Your Bulk Tray Dryer 6
Bulk Tray Dryer Components 7
Setting Up Your Bulk Tray Dryer 7
Installing the Tray Dryer on the Freeze Dry System 7
Venting the Vacuum Pump 9
Electrical Connection 9
Chemical Resistance of Freeze Dryer Components 9
Solvent Safety Precautions 10
CHAPTER 4: USING YOUR BULK TRAY DRYER 11
Bulk Tray Dryer Controls 12
Operation Checklist 12
Operating the Bulk Tray Dryer 13
Freeze Drying Using the Manifold Valves 15
CHAPTER 5: MAINTAINING YOUR BULK TRAY DRYER 17
CHAPTER 6: USING THE RS232 RECEPTACLE 19
Computer Connection for Computer Interface 19
O
O
FF
C
C
OONNTTEENNTTSS
CHAPTER 7: TROUBLESHOOTING 23
Vacuum Pump 23
Gaskets, Tubing, Connections, Sample Valves 24
System Components & Collection Chamber Isolation 25
Bulk Tray Dryer 29
APPENDIX A: BULK TRAY DRYER COMPONENTS 30
APPENDIX B: BULK TRAY DRYER DIMENSIONS 32
APPENDIX C: BULK TRAY DRYER SPECIFICATIONS 33
Electrical Specifications 33
Environmental Conditions 33
APPENDIX D: BULK TRAY DRYER ACCESSORIES 34
DECLARATION OF CONFORMITY 39
CChhaapptteerr 11::
IInnttrroodduuccttiioonn
Congratulations on your purchase of a Labconco FreeZone® Bulk Tray Dryer,
which is designed for laboratory lyophilization procedures. 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.
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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Chapter 1: Introduction
SAFE TEMPERATURE AND DRYING TIMES FOR SELECTED MATERIALS
Material 10mm Thick Safe Temp °C Collector Temp °C Hours (Approx.)
Milk -5 -40 10
Urea -7 -40 10
Blood Plasma -10 to -25 -40 16
Serum -25 -40 18
Vaccinia -30 to -40 -50 22
Influenza Vaccine -30 -50 24
Human Tissue -30 to -40 -50 48
Vegetable Tissue -50 -80 60
*Total sample 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 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.
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Chapter 1: Introduction
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.
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.
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CChhaapptteerr 22::
PPrreerreeqquuiissiitteess
Before you install your Bulk Tray Dryer, you need to prepare your site for
installation. The Bulk Tray Dryer will mount on top of a FreeZone 6, 12 or 18
liter Freeze Dry System. This could be either a benchtop or console model.
Carefully examine the location where you intend to install your Bulk Tray 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: Bulk Tray Dryer Specifications for complete Bulk Tray
Dryer electrical and environmental conditions, specifications and requirements.
Refer to the User’s Manual for the FreeZone Freeze Dry System for complete
electrical and environmental conditions, specifications and requirements.
Electrical Requirements
The Bulk Tray Dryer requires a dedicated electrical outlet. This outlet requires a
15 Amp circuit breaker or fuse for models rated at 115V (60 Hz). An outlet
equipped with an 8 Amp circuit breaker or fuse is required for models rated at
230V (50/60 Hz). Various power cord configurations are provided with 230V
models. If this does not match with 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. A minimum of
3" must be allowed between the rear and both sides of the Freeze Dryer and
adjacent wall surfaces. Restriction of airflow during operation could adversely
affect performance. Refer to Appendix B: Bulk Tray Dryer Dimensions for
dimensional drawings of the Bulk Tray Dryer.
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Chapter 2: Prerequisites
Vacuum Pump Requirements
A vacuum pump must be provided by the user. A vacuum pump with a
displacement of 144 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 with the FreeZone Freeze
Dry System. 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 system. 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 an 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 Dry System. Refer to the User’s Manual for the FreeZone Freeze
Dry System for vacuum pumps available from Labconco.
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CChhaapptteerr 33::
GGeettttiinngg SSttaarrtteedd
Now that the site for your Bulk Tray Dryer is properly prepared, you are ready to
unpack, inspect, install and test your Bulk Tray Dryer. Read this chapter to learn
how to:
• Unpack and move your Bulk Tray Dryer.
• Set up your Bulk Tray Dryer.
• Connect the electrical supply source to your Bulk Tray Dryer.
• Safely use solvents with your Bulk Tray Dryer.
The Bulk Tray Dryer weighs over 202 lbs. (92 Kg). The carton allows for
lifting with a mechanical lift truck or hand truck. If you must lift the Bulk
Tray Dryer manually, use at least two (2) persons and follow safe lifting
guidelines.
Unpacking Your Bulk Tray Dryer
Carefully unpack your Bulk Tray Dryer and inspect it for damage that may have
occurred in transit. If your Bulk Tray Dryer is damaged, notify the delivery
carrier immediately and retain the entire shipment intact for inspection by the
carrier.
Do not return goods without the prior authorization of Labconco. Unauthorized
returns will not be accepted.
If your Bulk Tray 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.
The United States Interstate Commerce Commission rules require that claims be
filed with the delivery carrier within fifteen (15) days of delivery.
Do not discard the carton or packing material for your Bulk Tray Dryer until you
have checked all of the components and installed and tested the bulk tray dryer.
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Chapter 3: Getting Started
Bulk Tray Dryer Components
Locate the model of Bulk Tray Dryer you received in the following table. Verify
that the components listed are present and undamaged.
Power Cords
6 Port
Catalog # Description Volts Hz
7806020 Bulk Tray Dryer 115 50/60 X
7806021 Bulk Tray Dryer 115 50/60 X X
7806030 Bulk Tray Dryer 230 50/60 X
7806031 Bulk Tray Dryer 230 50/60 X X
7806040 Bulk Tray Dryer 230 50/60 X
7806041 Bulk Tray Dryer 230 50/60 X X
7806060 Bulk Tray Dryer 230 50/60 X
7806061 Bulk Tray Dryer 230 50/60 X X
7806070 Bulk Tray Dryer 230 50/60 X
7806071 Bulk Tray Dryer 230 50/60 X X
Manifold
1334500
1336100
1338000
1332600
Plus the following:
Part # Qty. Component Description
7594900 1 User’s Manual
1880712 4 Screw ¼-20 x .75
1905621 4 Nut ¼-20
1911416 8 Washer ¼
If you did not receive one or more of the components listed for your Bulk Tray
Dryer, or if any of the components are damaged, contact Labconco Corporation
immediately for further instructions.
1332700
Setting Up Your Bulk Tray Dryer
After you verify receipt of the proper components, move your Bulk Tray Dryer to
the location where you want to install it. Then, follow the steps listed below.
Installing the Tray Dryer on the Freeze Dry System
The following tools are required to install the Bulk Tray Dryer onto a FreeZone
Freeze Dry System: Flat blade screw driver or 5/16" socket and a 7/16" wrench
or socket.
Remove the four plastic hole plugs from the top of the Freeze Dry System on
which the Bulk Tray Dryer is to be mounted. If the Freeze Dry System has a flat
gasket around the 3.0 inch vacuum port, remove it. Loosen both clamps on the
lower connection hose and slide the hose upward so the bottom of the hose is
above the lower edge of the stainless steel tube. Snug both clamps on the hose to
hold them in place.
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Chapter 3: Getting Started
Lift the Bulk Tray Dryer into place on your Freeze Dry System while centering
the vacuum coupling over the vacuum connection port. Align the four mounting
holes in the Bulk Tray Dryer support stand with the four holes in the top of the
Freeze Dry System.
NOTE: Do not lift the Bulk Tray Dryer by the door or disturb it.
Install the four bolts, nuts, and washers provided. Loosen the clamps and slide
the lower hose down over the vacuum connection port. Orient the clamps to gain
access and tighten the clamps to provide a leak-free connection.
The Bulk Tray Dryer is now installed and must be tested to make certain the
system is free of leaks. To test, turn on the Freeze Dry System refrigeration and
allow the temperature to reach –40° or lower. Close the door of the Tray Dryer
and make sure the Vac Release control is in the “CLOSED” position. Start the
vacuum pump and monitor the vacuum gauge. The vacuum on the Freeze Dry
System should reach 0.133 mBar within 30 minutes and should achieve an
ultimate vacuum of 0.040 mBar or lower within 18 hours.
If 0.040 mBar cannot be achieved, consult the troubleshooting section of this
manual and of the manual supplied with the Freeze Dry System.
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Chapter 3: Getting Started
Venting the Vacuum Pump
If any materials will be placed in the Bulk Tray Dryer that can liberate
hazardous gases when heated, the vacuum pump exhaust must be vented to a
fume hood or other ventilation device.
Electrical Connection
Plug the power cord into the receptacle on the back of the Bulk Tray Dryer and
plug the other end into a suitable power receptacle.
DO NOT ATTEMPT TO CONNECT THE BULK TRAY DRYER INTO THE
FREEZONE FREEZE DRY SYSTEM.
Chemical Resistance of Freeze Dryer Components
The FreeZone Freeze Dry System and Bulk Tray Dryer are 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:
Acids Buffers Solvents
Acetic Acid 20%
Formic Acid
Component Material
Valve Stem Acetal C D D D D
Collector*
Lid & Door
Hoses,
Gaskets &
Valve Bodies
Flask Top Silicon
Chamber &
Fittings
* An accessory glass lid is available for the Freeze Dry base units.
C – Moderate degradation; Limited use.
D – Severe degradation; infrequent use recommended; immediate
Acrylic D D D D
Neoprene C D D C C D D D C D
C D D D D D C D
Rubber
Stainless Steel C
Trifluoroacetic Acid (TFA)
Calcium Chloride
Sodium Phosphate
Acetone
Acetonittirle
Carbon Tetrochloride
Cyclohexane
Dioxane
Methyl t-Butyl Ether (BTBE)
Pyridine
thorough cleaning
required.
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