Labconco FreeZone Stoppering Tray Dryers User Manual

FreeZone



Stoppering Tray Dryers

Models
79480 Series

User’s Manual

Labconco Corporation
8811 Prospect Avenue
Kansas City, MO 64132-2696
800-821-5525, 816-333-8811
FAX [phone]
E-MAIL [e-mail]
HOME PAGE www.labconco.com

Please read the User’s Manual before operating the equipment.

To receive important product updates,

complete your product registration card

online at register.labconco.com

Copyright © 2004, 2007, 2010, 2012, 2013, 2014 Labconco Corporation. All rights reserved.

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® Stoppering Tray Dryers 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.

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.

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 #7353900, Rev. F

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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

CHAPTER 2: PREREQUISITES 6

Electrical Requirements 6
Location Requirements 7
Vacuum Pump Requirements 7

CHAPTER 3: GETTING STARTED 8

Unpacking Your Stoppering Tray Dryer 8
Stoppering Tray Dryer Components 9

Setting Up Your Stoppering Tray Dryer 9
Installing the Tray Dryer on the Freeze Dry System 10
Venting the Vacuum Pump 11
Electrical Connection 11

Chemical Resistance of Freeze Dryer Components 11

Solvent Safety Precautions 13

CHAPTER 4: USING YOUR STOPPERING TRAY DRYER 14

Stoppering Tray Dryer Controls 15

Operation Checklist 16

Operating the Stoppering Tray Dryer 17
Set-Up 17

Manual Control Operation 18

Automatic Control Operation 19

Automatic Start-Up of Freeze Dryer Vacuum 20

Programming 21

Starting the Freeze Dry Cycle 21

Changing the Program Parameters in the Middle of a Run 23

Stopping the Freeze Dry Cycle 23

Monitoring the System Operation 23

Shelf Spacing Adjustment 24

Shelf Loading 24

Sample Freezing 25
Freeze Drying 25
Stoppering 25
Vacuum Break/Backfilling 26
Alarms 26
System Temperature Variations 26
Vacuum 26
System Temperature Set Point 27
Power Failure 27
Temperature Probe 27

CHAPTER 5: MAINTAINING YOUR STOPPERING TRAY

DRYER 28

CHAPTER 6: USING THE RS232 RECEPTACLE 30

Computer Connection for Computer Interface 30

CHAPTER 7: TROUBLESHOOTING 35

Vacuum Pump 35
Gaskets, Tubing, Connections, Sample Valves 36
System Components & Collection Chamber Isolation 37
Stoppering Tray Dryer 40
Refrigeration Module Operation 40
Access to Mechanical Components 40
Shelf and Stoppering System Removal 41
Filling the Fluid System 42
Heat Transfer Fluid Precautions 43
Heat Transfer Fluid First Aid Procedures 44

CHAPTER 8: MODIFYING YOUR STOPPERING TRAY
DRYER DISPLAY 45

Modifying the Display 45

APPENDIX A: STOPPERING TRAY DRYER COMPONENTS 47

APPENDIX B: STOPPERING TRAY DRYER DIMENSIONS 50

APPENDIX C: STOPPERING TRAY DRYER

SPECIFICATIONS 52

Electrical Specifications 52
Environmental Conditions 52

APPENDIX D: STOPPERING TRAY DRYER ACCESSORIES 53

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Congratulations on your purchase of a Labconco FreeZone® Stoppering Tray
Dryer, 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.

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Chapter 1: Introduction

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SAFE TEMPERATURE AND DRYING TIMES

FOR SELECTED MATERIALS

Material
10mm Thick

Safe
Temperature
°C

Collector
Temperature
°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

Table 1

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.

*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

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Chapter 1: Introduction

3

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.

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.

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Chapter 1: Introduction

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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
Stoppering Tray Dryer. Instructions for performing routine maintenance and
making minor modifications to your Stoppering Tray Dryer are also included.

Chapter 1: Introduction provides a brief overview of the freeze dry process,
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 Stoppering Tray Dryer. Electrical requirements are discussed.

Chapter 3: Getting Started contains the information you need to properly unpack,
inspect and install your Stoppering Tray Dryer.

Chapter 4: Using Your Stoppering Tray Dryer discusses the basic operation of
your Stoppering Tray Dryer. Information on how to load samples and run the
Stoppering Tray Dryer is included.

Chapter 5: Maintaining Your Stoppering Tray Dryer explains how to perform
routine maintenance on your Stoppering Tray Dryer.

Chapter 6: Using the RS-232 Receptacle describes how to connect a computer
for monitoring the operation.

Chapter 7: Troubleshooting contains information about problems you may
encounter while using your Stoppering Tray Dryer, including the probable causes
of the problems, and suggested corrective actions.

Chapter 8: Modifying Your Stoppering Tray Dryer Display describes how to
calibrate the vacuum display and restore factory settings.

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Chapter 1: Introduction

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Appendix A: Stoppering Tray Dryer Components contains labeled diagrams of the
components of the Stoppering Tray Dryer.

Appendix B: Stoppering Tray Dryer Dimensions contains comprehensive
diagrams showing the dimensions for the Stoppering Tray Dryer.

Appendix C: Stoppering Tray Dryer Specifications contains product
specifications.

Appendix D: Stoppering Tray Dryer Accessories lists the part numbers and
descriptions of all of the accessories available for your Stoppering Tray 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.

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Before you install your Stoppering Tray Dryer, you need to prepare your site for
installation. The Stoppering 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 Stoppering 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: Stoppering Tray Dryer Specifications for complete
Stoppering 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 Stoppering Tray 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 is equipped with a 20 Amp
NEMA 5-20P plug. 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.

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Chapter 2: Prerequisites

7

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 in through the front and exhausts it through the
rear. 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: Stoppering Tray Dryer Dimensions for dimensional
drawings of the Stoppering Tray Dryer.

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 Dry 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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The United
States Interstate
Commerce
Commission
rules require
that claims be
filed with the
delivery carrier
within fifteen
(15) days of
delivery.



Now that the site for your Stoppering Tray Dryer is properly prepared, you are
ready to unpack, inspect, install and test your Stoppering Tray Dryer. Read this
chapter to learn how to:

 unpack and move your Stoppering Tray Dryer.
 set up your Stoppering Tray Dryer.
 connect the electrical supply source to your Stoppering Tray Dryer.
 safely use solvents with your Stoppering Tray Dryer.

The Stoppering Tray Dryer weighs over 400 lbs. (181 Kg). The
carton allows for lifting with a mechanical lift truck or hand
truck. If you must lift the Stoppering Tray Dryer manually,
use at least four (4) persons and follow safe lifting guidelines.

Unpacking Your Stoppering Tray Dryer

Carefully unpack your Stoppering Tray Dryer and inspect it for damage that may
have occurred in transit. If your Stoppering 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.

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Chapter 3: Getting Started

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Power Cords

Catalog #

Description

Volts

Hz

1336400

1336500

1342100

1332601

1332701

7948020

Stoppering Tray Dryer

115

60 X 7948030

Stoppering Tray Dryer

230

50 X 7948040

Stoppering Tray Dryer

230

60 X 7948060

Stoppering Tray Dryer

230

50 X 7948070

Stoppering Tray Dryer

230

50

X

Part #

Qty.

Component Description

7353900

1

User’s Manual

1880712

4

Screw ¼-20 x .75

1905621

4

Nut ¼-20

1911416

8

Washer ¼

7353403

1

Cable RS 232





IF YOUR STOPPERING 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.

DO NOT DISCARD THE CARTON OR PACKING MATERIAL
FOR YOUR STOPPERING TRAY DRYER UNTIL YOU HAVE
CHECKED ALL OF THE COMPONENTS AND INSTALLED
AND TESTED THE STOPPERING TRAY DRYER.

Stoppering Tray Dryer Components

Locate the model of Stoppering Tray Dryer you received in the following table.
Verify that the components listed are present and undamaged.

Plus the following:

If you did not receive one or more of the components listed for your Stoppering
Tray Dryer, or if any of the components are damaged, contact Labconco
Corporation immediately for further instructions.

Setting Up Your Stoppering Tray Dryer

After you verify receipt of the proper components, move your Stoppering Tray
Dryer to the location where you want to install it. Then, follow the steps listed
below.

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Chapter 3: Getting Started

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Installing the Tray Dryer on the Freeze Dry System

The following tools are required to install the Stoppering Tray Dryer onto a
FreeZone Freeze Dry System base unit: Flat blade screwdriver 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 Stoppering 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 edge of the
hose is above the lower edge of the stainless steel tube. Snug both clamps on the
hose to hold them in place.

Lift the Stoppering 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 Stoppering Tray Dryer support stand with the four holes in
the top of the Freeze Dry System.

NOTE: Do not lift the Stoppering 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.

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The Stoppering 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 Stoppering Control is in the “LOWER” position and 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.

Venting the Vacuum Pump

If any materials will be placed in the Stoppering 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 Stoppering Tray Dryer
and plug the other end into a suitable power receptacle.

DO NOT ATTEMPT TO PLUG THE STOPPERING TRAY
DRYER INTO THE FREEZONE FREEZE DRY SYSTEM.

CAUTION: When the appropriate power cord is plugged into
the power receptacle on the rear panel of the tray dryer, the
clamp on the tray dryer receptacle should be tightened to
prevent the cord from accidentally being switched with the
freeze dryer cord located underneath the tray dryer. (The
freeze dryer may require different mains A.C. voltage and
switching these power cords may cause damage).

Chemical Resistance of Freeze Dryer
Components

The FreeZone Freeze Dry System and Stoppering 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:

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Chapter 3: Getting Started

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Acids

Buffers Solvents

Component

Material

Acetic Acid 20%

Formic Acid

Trifluoroacetic Acid (TFA) Calcium Chloride

Sodium Phosphate Acetone

Acetonittirle

Carbon Tetrochloride

Cyclohexane

Dioxane

Methyl t-Butyl Ether (BTBE)

Pyridine

Valve Stem

Acetal

C D D D D

Collector*
Lid & Door

Acrylic

D D D D

Hoses,
Gaskets &
Valve
Bodies

Neoprene

C D D C C D D D C

D

Flask Top

Silicon
Rubber

C D D D D D C

D

Chamber &
Fittings

Stainless
Steel

C

* An accessory glass lid is available for the Freeze Dry Systems.
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. This is accomplished by closing all
sample valves on a clean, dry freeze dry system and turning on the vacuum
pump. If the pump is operated at an elevated vacuum level (> 10mBar), oil
may be expelled from the pump and damage could occur.

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Chapter 3: Getting Started

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!

Another way to extend the life of the vacuum pump is to install an optional
secondary trap in the line between the Freeze Dry System 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 Dry System, contact Labconco Technical Service at 1-800-821-5525 or
816-333-8811 or e-mail: [e-mail].

Solvent Safety Precautions

Solvents used in the Stoppering Tray 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 a fume hood.

Hazardous materials such as strong acids or bases, radioactive
substances and volatile organics must be handled carefully and
promptly cleaned up if spilled. If a sample is spilled in the
collector chamber it must immediately be cleaned up.

WARNING: The disposal of substances used in connection
with this equipment may be governed by various Federal, State
or local 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 to comply with such regulations.

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D

D

RRYYEERR

!

After your Stoppering Tray Dryer has been installed as detailed in Chapter 3:
Getting Started, you are ready to begin using your Stoppering Tray Dryer. Read

this chapter to learn how to:

 operate the controls.
 understand the display.
 connect samples.

Do not use the Stoppering Tray Dryer in a manner not
specified by the manufacturer (refer to Appendix C: Stoppering
Tray Dryer Specifications). The electrical protection properties
of the Stoppering Tray Dryer may be impaired if the
Stoppering Tray Dryer is used inappropriately.

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Chapter 4: Using Your Stoppering Tray Dryer

15

6

14 2

3

4

13

11

10

12

1

5 6 7 8 9

14

Stoppering Tray Dryer Controls

The control panel for the Stoppering Tray Dryer is shown with a description about
its function.

1. Display. Displays all necessary programming and operational data. Provides

prompts to aid in programming.

2. Display Selector. Changes format of display from “monitor’ to “auto” to

“manual” to “set up” screen.

3. Display Indicators. Amber lamps indicate which display “screen” is shown.

4. Alarm Indicator. Red LED indicates that a system alarm has occurred.

5. Decrease Switch. Used in programming to decrease a parameter set point.

6. Increase Switch. Used in programming to increase a parameter set point.

7. Enter Switch. Used in programming to enter a selected set point into memory.

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!

8. Mode Indicator. Amber lamp indicates whether the control is set to operate either

in the automatic or manual mode.

9. Mode Selector Switch. Selects the mode of operation – either manual or

automatic.

10. Run/Stop Switch. Initiates the start or stop of the lyophilization process.

11. Run/Stop Indicator. Amber lamp burns steadily while freeze drying is in

progress and turns off if either the programmed cycle is completed or the process

is terminated in mid cycle. The amber lamp flashes if freeze drying is in progress

and an out-of-specification condition exists.

12. Stoppering. Controls the stoppering up and down movement. The mechanism

will function only while the chamber is under vacuum. The stoppering action

should be closely monitored when operating this control.

13. Vacuum Release. Vents the chamber so the chamber door can be opened. This

control can also vent gas into the chamber when the gas is properly connected to

the backfill port.

14. Back Fill. A regulated tank of gas may be connected to the port to allow the

introduction of gas into the chamber after freeze drying. The port accepts 1/8"

tubing.

Ethylene Oxide is not recommended for use in this Tray Dryer for

decontamination because of its hazardous and corrosive properties.

15. Power Switch. Turns all power to Tray Dryer ON or OFF. Not shown. Located

on left side of cabinet.

Operation Checklist

The following checklist should be followed prior to each use of your Stoppering
Tray Dryer:

1. Wipe out the interior of the Stoppering Tray Dryer chamber with a soft cloth
or paper towel to remove any moisture or debris

2. Wipe the interior of the collector chamber of the Freeze Dry System with a
soft cloth or paper towel to remove any accumulated moisture.

3. Check the collector chamber drain hose on the Freeze Dry System to ensure
that the hose is free of moisture and that the drain plug is securely installed.

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17

TEMPERATURE UNITS:

°C °F

REFRIG TOTAL HOUR: XXXX

SERVICE HOUR: XXXX

VACUUM UNITS:

MBar Pa Torr

REFRIGERATION TOTAL HOURS: XXXX:

RESET SERVICE HOUR: ? X

4. Using a soft, lint-free cloth or paper towel, wipe the Freeze Dry System
collector chamber lid gasket and the Stoppering Tray Dryer door gasket to
remove any dirt and contaminants that could cause a vacuum leak. Vacuum
grease is not required on the door gasket or collector lid gasket to obtain a
proper vacuum seal.

Operating the Stoppering Tray Dryer

Set-Up

The display units for vacuum may be selected to be mBar, Pascal (Pa) or Torr and
the temperatures may be displayed as either °F or °C. The refrigeration operating
time may be monitored and the vacuum reading may be calibrated. To configure
your Stoppering Tray Dryer, turn the main power switch ON. Press the Display
button until the Set up LED is lit. The display will show:

 Press  or  until the desired units are flashing.
 Press ENTER.
 The display will show:

 Press  or until the desired units are flashing.
 Press ENTER
 The display will show:

 Press ENTER if you do not want to reset SERVICE HOURS.
 Press  to reset the Service Hours to 0. This allows you to keep track

of the time the refrigeration system operated since it was serviced.

 The display will show:

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Chapter 4: Using Your Stoppering Tray Dryer

18

SET POINT TEMP –30°C

 Hold  for 5 seconds.
 Press ENTER.
 At any time the DISPLAY button can be pressed to select a different

display screen.

Manual Control Operation

(1) Turn the Power switch ON. The display will become active.
(2) Push the DISPLAY button until the Manual LED lights. This will

cause the manual display screen to be shown with the previously
entered set point temperature.

The temperature units are displayed in the units (°F or °C) selected in
the Set Up.
The temperature may be set anywhere from +40°C to –40°C in 1°C
increments.

(3) If the set point needs to be changed, press the INCREASE or

DECREASE button until the desired set point temperature is
displayed.

(4) Press ENTER. If ENTER is not pressed within 10 seconds, the set

point will revert to the previously entered set point temperature.
(5) Press MODE button until the Manual LED lights.
(6) Press RUN/STOP button. The amber LED by the button will light and

the refrigeration system and/or heater will operate.
(7) To change the set point temperature in the middle of a run, repeat steps

2, 3 and 4. The system will adjust to the new temperature set point.
(8) To monitor system operation, press DISPLAY until the Monitor LED

lights. The display will simultaneously show system temperature,

vacuum and three sample temperatures if sensors were plugged into

their jacks at the front of the chamber and inserted into sample vials.

If sensors are not plugged into their jacks, the probe temperature

display will show “- - -”.

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P1

-indicates what program is selected

PRB

-shelf probes for shelf 1, 2 and 3 (If a probe
is not installed, the display shows ---)

C

-°C F -°F

TMP

-system temperature

SEG

-indicates what segment is active and
ramping or holding.

M

-manual mode

VAC

-system vacuum level

m

-mBar

P

-Pascal

T

-Torr

R

-Ramp

H

-Hold

TR

-Time remaining in hours

P1 PRB 1=XX 2=XX 3=XXc
TMP=XX SEG=M VAC=hi m

The segment number will always indicate “M” while operating in the

manual mode. Segment numbers are used only in the automatic mode to

identify portions of the programmed cycle. Temperatures and vacuum are

displayed in the units selected during the set up procedure. Above 5.0

mBar the display will show “hi” vacuum. System temperature rather than

probe temperature is the parameter that is regulated by the controller.

(9) To stop, push RUN/STOP button, which will turn off the amber LED

over the switch, the refrigeration system and the heater. To turn off

the entire system, turn the power switch off.

Automatic Control Operation

The Stoppering Tray Dryer is equipped with a microprocessor based controller
that permits temperature to be programmed using as many as five different
segments. Each segment consists of a temperature ramp function and a
temperature hold function. There are five programs of five segments each that
store the settings. One of the five may be selected by pressing the DISPLAY
switch until the AUTO LED lights. Press the UP/DOWN keys to select the

desired program, and then press “ENTER.” The display will change to show the

parameters for this program. The ramp allows the temperature of the sample to be
increased or decreased at any desired rate within the capacity of the heating and
cooling systems of the Stoppering Tray Dryer.

A Stoppering Tray Dryer without samples on shelves is capable of cooling at a
rate of approximately .5°C/minute and can heat at approximately 1.3°C/minute.
The cooling ramp rate may be slower as the temperature approaches –40°C. Hold
temperatures may be set anywhere from +40°C to –40°C in 1°C increments.

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When the desired temperature is achieved, the hold function will maintain that
temperature for the programmed length of time. The microprocessor control has a
built in memory of the last entered program to allow the identical protocol to be
repeated by simply pushing the RUN button. A typical 3 segment program is
shown in Figure 5.

Automatic Start-Up of Freeze Dryer
Vacuum

At the end of Segment 1 Hold, if the StopperingTray Dyer is connected to the
Freeze Dry System base unit, the vacuum provided by the Freeze Dryer will start
automatically. The base unit should have the refrigeration started in manual mode
to allow it to reach temperature while the Tray Dryer is processing Segment 1 of

the program. (Do not start the base unit’s refrigeration using automatic mode.

This will not allow the Tray Dryer to start the vacuum on the Freeze Dryer).
Connect the Tray Dryer to the Freeze Dryer with cable #7353403 (this cable is
shipped with the Tray Dryer). One end of the cable plugs into the 4-pin connector
(Output to Freeze Dryer) on the back of the Tray Dryer in the lower right hand
corner of the unit (when viewing the back of the unit), and the other end of the
cable plugs into the 4-pin connector (Stoppering Tray Dryer Input) on the back of
the Freeze Dryer in the upper right hand corner of the unit (when viewing the
back of the unit).

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Chapter 4: Using Your Stoppering Tray Dryer

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P1 SEG 1 RAMP 00.0°C/MN
HOLD –34°C TIME 00.0

Programming

The Tray Dryer will store up to five programs numbered 1 through 5. The five
programs, once programmed, will be retained in memory. To program a run,
select the program number that you want to use and enter the parameters as
follows.

Turn the Power switch to the ON position. Press the DISPLAY button until the
Auto LED lights.

NOTE: Values shown in this example are for reference only.

The “P” in the display will flash and the program number that will be run is

shown. To select different programs, press the UP or DOWN key to change
program number (Programs 1 through 5). When the desired program number is
displayed, press ENTER.

The display will show the parameters that were last entered for this program.

If any of the parameters are changed, the ENTER key must be pressed for the new
value to be stored. If the ENTER key is not pressed within 10 seconds after the
last parameter adjustment, the value will return to the previously stored value.
The flashing parameter name indicates the parameter that will be changed.
Pressing ENTER only will advance to the next parameter.

After the AUTO RUN cycle is started, segments with a value greater than the
segment running may have their parameters changed. Only the selected program
may be modified. To modify a different program, the system must be stopped and
the desired program selected.

Starting the Freeze Dry Cycle

After the desired cycles have been programmed, push the MODE button to
Select-AUTO. Push the RUN/STOP button to start the program running. The
RUN indicator will light. The System

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Chapter 4: Using Your Stoppering Tray Dryer

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P1

-indicates what program is
selected

PRB

-shelf probes for shelf 1, 2
and 3 (If a probe is not
installed, the display shows ---)

C

-°C F -°F

TMP

-system temperature

SEG

-indicates what segment is
active and ramping

VAC

-system vacuum level

M

-mBar

P

-Pascal

T

Torr

P1 PRB 1=28 2=29 3=28 C
TMP=30 SEG=1H VAC=.030 M

P1 PRB 1=28 2=29 3=28 C
TMP=30 TR=4.55 VAC=0033 M

TR

-indicates the amount of time
remaining in the present seg­ment. If time is 10.0 hours or
more, the time is displayed in
1/10 hours. If time is less than

10.0 hours, the time is displayed
in 1/100 hours. If the hold time
was programmed to be
indefinite, the display will show
“INDF”.

P1

-indicates what program is
selected

PBR

-shelf probes for shelf 1, 2
and 3

TMP

-system temperature

SEG

-indicates what segment is
active and holding

VAC

-system vacuum level

P1 PRB 1=28 2=29 3=28 C
TMP=30 SEG=1R VAC=.030 M

Status Display will change and the Display will change to MONITOR mode.

During the RAMP cycle of the active segment, the Status Display will be as
follows:

During the HOLD cycle of the active segment the Status Display will alternately
be as follows:

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Changing the Program Parameters in the
Middle of a Run

(1) Press DISPLAY to obtain Monitor screen. Note current operating

segment.

(2) Press DISPLAY to obtain Auto screen.

(3) Enter a segment number that will occur after the current segment that is

running.

The presently running segment cannot be modified while the system is

running.

(4) Modify as required.

(5) Press ENTER.

Stopping the Freeze Dry Cycle

1. At the end of the last programmed segment, the freeze dry system will
automatically stop. The refrigeration system and the heater will shut off.
The display will show Segment “E” (End).

2. To stop before the completion of the last programmed segment, press
RUN/STOP. The amber lamp will turn off as will the refrigeration system
and heater. The display will remain active but time functions will stop
operating.

3. The entire system can be shut off by pressing the Power Switch.

4. If the Power switch is shut off prior to stopping the cycle with the
RUN/STOP button, when the Power Switch is again turned on, the system
will resume operation and attempt to complete the programmed cycle from
the point at which it was shut off. The display mode indicator
“PROGRAM” will flash to indicate power loss during programmed run.

Monitoring the System Operation

Press the Display button until the monitor LED lights. The display will show
system temperature, system vacuum and 3 sample temperatures if sensors were
plugged into their jacks at the front of the chamber and inserted into sample vials.
If sensors are not plugged into their jacks, the probe temperature display will
show “- - -”. The temperatures and vacuum are displayed in the units selected in
Set Up. Above 5.0 mBar the display will show “HI” vacuum.

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Chapter 4: Using Your Stoppering Tray Dryer

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

If the temperature is warmer than +50°C, the display will show “HI”. If the

temperature is cooler than –50°C, the display will say “LO”.

Shelf Spacing Adjustment

Prior to loading the shelves with the product to be freeze dried, adjust the shelves
to the 3-shelf, 2-shelf or 1-shelf position. It is best to observe the shelf supporting
mechanism and practice while reading these procedures. In the 3-shelf position,
the spacing between the shelves will accommodate a serum bottle with the stopper
raised up to a maximum height of 75 mm (2.9 inches).

Minimum serum bottle height with lowered stopper for bottles on 3 shelves is 38
mm (1.5 inches).

For a 2-shelf system, grasp the top shelf and raise it until it latches in place. Then
raise the middle shelf approximately 1 inch until it latches in a position to allow a
two equally spaced shelf system. The spacing between shelves will accommodate
a bottle with the stopper raised up to a maximum height of 107 mm (4.2 inches).
Minimum serum bottle height with lowered stopper for a 2-shelf system is 56 mm
(2.2 inches).

For a single shelf system, raise both the top and middle shelves until they latch in
place in their top positions. The spacing for a single shelf system will
accommodate a bottle with raised stopper up to a maximum height of 196 mm
(7.7 inches), and the minimum height of a bottle with lowered stopper for
successful stoppering is 114 mm (4.5 inches).

To unlatch the shelves, press the latch protruding from the side of the shelf
support structure and move the latch until it clears the shelf and allows the shelf to
drop. The top shelf has one latched position, the middle shelf has two latched
positions, and the bottom shelf should not latch in any position.

Shelf Loading

The stoppering mechanism is capable of generating a very strong force, which can
damage the shelves or mechanism. Therefore, it is important to distribute the
serum bottles to be stoppered evenly across the entire surface of each shelf.

Your Stoppering Tray Dryer has a unique system for keeping the shelves level
and moving smoothly while stoppering. If a problem occurs during stoppering,
the system is designed to flex a small amount to lessen the possibility of damage
to the unit.

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Chapter 4: Using Your Stoppering Tray Dryer

25

The stoppering action should be monitored by looking through the chamber door.
Cease stoppering when all bottles appear stoppered or if a problem occurs.
Distributing the serum bottles evenly on the shelves also aids in consistent drying
of all serum bottles on each shelf.

Sample Freezing

Before the freeze dry process can occur, the products to be dried must be in a
frozen state. This can be accomplished in a freezer separate from the Stoppering
Tray Dryer or on the shelves in the Stoppering Tray Dryer. First the shelves
should be adjusted to accept the size of the selected sample containers. Next, turn
On the power switch and set the controls to cool the shelves. This is most simply
done by setting the temperature in the manual mode, although segment 1 in the
automatic mode can also be programmed to cool the shelves and start the vacuum
after the end of Segment 1. Load the samples onto the shelves after the system
temperature is below the sample eutectic temperature. If desired, place one
temperature probe in a sample vial on each shelf. The temperature can be
monitored by pressing the Display button until the Monitor LED lights.

Freeze Drying

Turn on the FreeZone Freeze Dry System base unit. Following the instructions
for the unit, this may be accomplished in either the automatic or manual mode.

When the collector temperature is less than –40°C and the vacuum is less than

0.133 mBar, the manual mode set point temperature may be adjusted or the

automatic mode program may be initiated. At no time during the primary drying
phase should the product temperature be allowed to rise higher than the eutectic
temperature.

The ice collecting coil temperature and the vacuum level should be monitored.
Higher than desired collector coil temperature or vacuum levels will inhibit or
ruin the freeze dry process.

Stoppering

The stoppering operation (when desired) is performed after the freeze dry process

is complete. To stopper, move the Stoppering control toward the “RAISE”

position. This action allows the actuator beneath the bottom shelf to inflate
causing the bottom shelf to rise. The vials on the shelf will then contact the
middle shelf causing it to rise and the top shelf will eventually be contacted and
rise. When all three shelves have raised and made contact with each other,
stoppers will be pressed into the vials. Monitor the stoppering process by looking
through the chamber door.

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When all of the vials appear to be stoppered, move the Stoppering control to the
“LOWER” position. This opens the diaphragm to the vacuum pump, which
deflates the diaphragm. Opening the vacuum release control also deflates the

stoppering diaphragm. The Stoppering control should be left in the “LOWER”

position when not stoppering.

Vacuum Break/Backfilling

To open the chamber door, the vacuum must be released. To release the vacuum,

move the Vacuum Release control to the “OPEN” position and shut off the

vacuum pump using the switch on the base unit.

Air enters the vacuum chamber through the Back Fill port. When the sound of air
through the Back Fill port is no longer audible, the chamber door is ready to open.

To backfill the chamber with a gas, connect a cylinder of the desired gas to the
Back Fill port. The port will accept 1/8" tubing. The bottle must be equipped
with a regulator set to 15 psi maximum. The gas can be metered with the
Vacuum Release control and chamber pressure monitored with the freeze dry

system’s vacuum gauge. Allow the vacuum pump to run for a few minutes while

the gas enters to permit the back fill gas to surround the freeze dried sample.
When the vacuum pump is turned off, air will enter the system through the
vacuum break valve located between the vacuum pump and the collector
chamber.

Alarms

A number of unusual events may occur during a lyophilization procedure that can
adversely effect the operation of the Stoppering Tray Dryer. If an event occurs,
the alarm indicator will flash and the beeper will sound.

The beeper will automatically mute itself after one minute. The specific alarm

can be identified observing the display. The following “out of specification”

conditions will initiate an alarm:

System Temperature Variations

Once the system temperature has stabilized for 20 minutes, if the manual set point
temperature or automatic hold temperature varies more than ±2°C as measured by

the system temperature sensor, the Red Alarm indicator and the word “TMP” on

the display will flash. Pressing Run/Stop or turning off the power switch cancels
the flashing warning.

Vacuum

Once the system vacuum is low and stabilized at a point where it changes less
than 0.020 mBar in 5 minutes, if the vacuum changes more than 0.500 mBar, the
Red Alarm indicator and the word “VAC” on the display will flash. Pressing
Run/Stop or turning off the power switch cancels the flashing warning.

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TEMPERATURE SENSOR X

CALIBRATION ERROR

System Temperature Set Point

If during a Ramp mode the system temperature stabilizes without reaching the set
point temperature, the control will enter the next Hold mode. The Red Alarm
indicator will flash and the program indicator “Px” on the display will flash.
Pressing Run/Stop or turning off the power switch cancels the flashing warning.

Power Failure

If a power failure occurs while a run is in progress, the Red Alarm indicator and
Run/Stop Indicator will flash when the power is restored. Once power is restored,
the process will continue as programmed until completion. Pressing Run/Stop or
turning off the power switch cancels the flashing warning.

Temperature Probe

When the power is turned on, the Stoppering Tray Dryer automatically checks the
calibration of all four temperature probes. If a probe is out of calibration, the
alarm LED will flash and the display will show:

Where X is:

S for the system probe
1 for sample probe 1
2 for sample probe 2
3 for sample probe 3

If this alarm occurs, the faulty probe must be replaced. If any of the sample
probes are faulty, it may be unplugged and the Stoppering Tray Dryer may be
used. The sample temperature display will show “- - - .” If the system probe is
faulty, it must be replaced before the Stoppering Tray Dryer can be used.

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C

C

HHAAPPTTEERR

5

5

M

M

AAIINNTTAAIINNIINNG

G

Y

Y

OOUURR

S

S

TTOOPPPPEERRIINNG

G

T

T

RRAAY

Y

D

D

RRYYEERR

Under normal operation, the Stoppering Tray Dryer requires little maintenance.
The following maintenance schedule is recommended:

As needed:

1. The user has the responsibility for carrying out appropriate decontamination if

2. Clean up all spills; remove liquids from the chamber.

3. Clean door and gasket using soft cloth, sponge or chamois and a mild, non-

4. Check oil level of the vacuum pump. It should be between MIN and MAX. If

5. If oil shows cloudiness, particles or discoloration, drain the pump and replace

6. Utilization of acids requires immediate cleaning and neutralization after

Monthly:

1. The rubber components on the Stoppering Tray Dryer may eventually

hazardous material is spilled on or inside the equipment. This may be done by
wiping the contaminated surfaces with a soft cloth dampened with alcohol.
Alcohol may craze the acrylic door. Before using any cleaning or
decontamination method except those recommended by Labconco, users
should check with Labconco that the proposed method will not damage the
equipment.

abrasive soap or detergent.

the oil level is less than an inch (25.4 mm) above MIN, add oil to proper level.

with fresh oil.

a run or physical damage will result.

deteriorate and require replacement. The effective life of rubber parts depends
upon both their usage and the surrounding environment. Check all rubber
hoses and gaskets and replace any that show signs of hardening, permanent set
or deterioration.

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2. Using a soft cloth, sponge or chamois and a mild, non-abrasive soap or

detergent, clean the acrylic door.

3. Using a soft cloth, sponge, or chamois and a mild, non-abrasive soap or

detergent, clean the exterior surfaces of the unit. Liquid spray cleaners 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 Stoppering Tray 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 performance.

Decontamination

When freeze drying biological substances, it may be necessary to decontaminate
the system. A surface decontaminant should be used to clean the accessible
surfaces. The use of ethylene oxide is not recommended because of its hazardous
and corrosive nature. Contact Labconco for additional information.

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30

C

C

HHAAPPTTEERR

6

6

U

U

SSIINNGG

T

T

HHEE

R

R

S

S

2

2

3

3

2

2

R

R

EECCEEPPTTAACCLLE

E

The operation of the Stoppering Tray Dryer and the FreeZone Freeze Dry System
can be monitored using a computer when the Stoppering Tray Dryer is connected
to the RS232 receptacle on the rear panel of the Freeze Dry System base unit.
The computer cannot control the operation of the Freeze Dry System.

Computer Connection for Computer
Interface

Check your computer to see which type of serial port is provided, then use 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 Dry System.

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 Dry System.

The purpose of the RS232 interface is to send data to a data logging computer to
monitor the state and activity of the Freeze Dry System This data is half duplex
data. The data properties are as follows:

1. Data Rate 2400 Baud

2. 8 Bit word length

3. 1 Start bit, 1 Stop bit

4. No parity is transmitted

5. Standard ASCII character set

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B

= Base Unit

T

= Collector Temperature

-48

= Collector Temperature in °Celsius

V

= Vacuum

18

=Vacuum Level in Micro Bars

SF

= Shell Freezer Temperature (if so equipped)

-41

= Shell Freezer Temperature in °C

C

=Vacuum Chamber Temperature (if so equipped)

9

=Feature not installed or out of range

PG

= Purge (if so equipped)

1

= ON

0

= OFF

TD

= Tray Dryer

PR

= Program

1

= Program 1 is selected

S

= Segment

3

= Segment 3 is operating

R

= Segment is in Ramp Mode

H

= Segment is in Hold Mode

TR

= Time Remaining of the current Hold Segment

5678

= Time Remaining in Hours

ST

= System Temperature

-40

= System Temperature in °C

P1

= Probe 1 Temperature

-39

= Probe 1 Temperature in °C

P2

= Probe 2 Temperature

999

= Probe not connected or temperature is out of range

P3

= Probe 3 Temperature

-37

= Probe 3 Temperature in °C

V

= Vacuum at Stoppering Tray Dryer

537

= Vacuum in Micro Bars

RS-232 TRANSMISSION RATE

10 SECONDS

B<T= -48 V= 18 SF = -41 C=999 PG=1 > TD<PR=1S=3R TR = 5678 ST= -40 P1 = -39 P2 = 999 P3 = -37 V = 0537>

The time between data transmissions may be varied by the user to occur at 10, 30,
60, 300 or 600 second intervals. Press the MENU button on the Freeze Dryer
base unit until the RS232 screen appears on the display.

Press select until the desired time interval is shown.

The format of the transmitted message with typical values is as follows:

Where:

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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 use an IBM compatible computer with Hyper

Terminal™ software (included with Windows® 95, 98, XP or 2000 operating

systems) to collect the RS232 data from your Freeze Dryer:

1. Make sure that the Freeze Dryer is properly connected to the communication
port on the computer.

2. Open Hyper Terminal™ software.

i)Windows® 95 or 98 use:

START/PROGRAMS/ACCESSORIES.

ii) Windows® 2000 or XP use:

START/PROGRAMS/ACCESSORIES/COMMUNICATIONS

The first time Hyper Terminal™ is opened a dialogue box requesting an area

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.”

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Chapter 6: Using The RS232 Receptacle

33

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 Properties” dialogue box will open. Enter the appropriate data
properties and press “OK.”

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Chapter 6: Using The RS232 Receptacle

34

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.

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35

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Refer to the following if your Freeze Dry System fails to operate properly. If the
suggested corrective actions do not solve your problem, contact Labconco for
additional assistance.

FreeZone Freeze Dry Systems that are clean and dry and without samples
attached should reach a vacuum of 0.133 mBar within 30 minutes and should
achieve an ultimate vacuum of 0.040 mBar within 18 hours when the refrigeration
is operating. If the Freeze Dry System does not obtain a satisfactory vacuum,
perform the following maintenance tests.

Vacuum Pump

First make sure that the vacuum pump operates. If it fails to operate, check the
electrical connections of the Freeze Dry System to the power source and then
check the electrical connection of the vacuum pump to the Freeze Dry System. 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 oil several times. To flush the pump, run the
pump 5 to 10 minutes to allow the oil to warm up. Drain the oil and refill
with clean oil. Repeat as necessary.

2. Check the oil level in the pump. Ensure it is filled to the correct level.

3. Check vacuum hose connections from the pump to the Freeze Dryer and

try running the unit.

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Chapter 7: Troubleshooting

36

If vacuum problems continue, consider obtaining a second vacuum gauge capable
of reading a vacuum of 0.010 mBar. It is often useful in determining if the
vacuum pump is operating properly and the vacuum sensor reading is accurate.

4. Isolate the pump by disconnecting the vacuum hose from the Freeze Dry

System. Deadhead the pump by inserting the vacuum sensor from a
secondary vacuum gauge into the end of the vacuum hose and observe the
vacuum reading obtained. Confirm that the pump is capable of achieving
an ultimate vacuum less than 0.010 mBar or approximately 10 microns. If
an inadequate vacuum reading is obtained, the pump has most likely failed
and may need to be replaced or rebuilt.

Gaskets, Tubing, Connections, Sample
Valves

1. Check all sample valves on the optional 6 port manifold shelf (if it is

installed) and ensure all valves are closed or in the vent position.

2. Check the drain line on the Freeze Dry System and ensure the drain plug is

installed and the tube appears to be in good condition.

3. Check all rubber vacuum tubing for signs of deterioration or cracking.

4. Check all connections and make sure they are secure and leak tight.

5. Check the Freeze Dry System collector lid gasket and the Stoppering Tray

Dryer door gasket for indentations, cracks or tears. Clean gaskets using a
soft, lint free cloth or paper towel.

6. The Stoppering Tray Dryer chamber and base unit collector chamber must

be dry.

7. When checking the sample valves, (if the system is so equipped), 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 indicate a potential vacuum leak. If the valve seems to be in good
condition, remove the valve and apply a thin coat of vacuum grease to the
stem and the outside sealing surface of the valve body, and reinstall the
valve. If the valve still seems to be the source of the problem, remove the
valve and stopper the hole with a rubber stopper. Continue checking the
other valves.

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Chapter 7: Troubleshooting

37

Knob & Stem

Assembly

Valve Body

Trim Ring

Manifold Assembly

The illustration below shows how the sample valve installs on a manifold.

System Components and Collection
Chamber Isolation

The following test allows you to check the pump and the connections from the
pump to the vacuum tube.

1. Place a rubber stopper in the vacuum port in the left side of the collector

chamber and another in the drain port in the bottom.

2. Restart the vacuum system and check your vacuum indication.

Insufficient vacuum indicates a bad pump or a leak in the connections
from the pump to the side of the chamber.

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Chapter 7: Troubleshooting

38

Areas for

Potential Leaks

Collector
Chamber

The following test is used to check the integrity at the Freeze Dry System
collection chamber. The figure below points out potential areas to locate a leak:

1. Remove the stopper from the side of the chamber and place a flat gasket

and a freeze dry flask over the connection port.

2. Fill the collection chamber with approximately 2 inches of water, enough

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 begin to boil and
the test will not be effective). Look inside the chamber for any bubbling
while the pump is running and after you shut the pump off.

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Chapter 7: Troubleshooting

39

3. If bubbling is observed around the bulkhead fittings, access the bottom of

the chamber and remove the insulation. Tighten the appropriate fitting by
placing a wrench on the fitting inside the chamber and use 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 test again. Should the
bubbling still be present, loosen the bulkhead fittings and apply vacuum
grease to the O-rings, then reassemble and test.

4. If bubbling was observed on the chamber surface, the chamber must be

replaced. This type of leak cannot be successfully repaired. The leading
cause of a chamber surface leak is corrosive residue left in the chamber
after use.

This test verifies that the vacuum leak is in the Stoppering Tray Dryer.

1. Remove the Stoppering Tray Dryer.

2. Position a flat gasket over the 3.0 inch diameter vacuum port 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 Stoppering Tray Dryer and
you should proceed to Section IV, Stoppering Tray Dryer.

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Chapter 7: Troubleshooting

40

Stoppering Tray Dryer

 Inspect the door and door gasket.
 Inspect the coupling between the freeze dryer and the Stoppering Tray Dryer.
 Remove the top left hand cover panel and inspect the valve and hose

connections to the chamber.

 Remove the top right hand cover and inspect the electrical pass through and

gasket on the top of the chamber.

Refrigeration Module Operation

Under a no-load condition and depending on the ambient temperature, the
Stoppering Tray Dryer refrigeration system can achieve a system temperature of –
40°C or lower within 4 hours when the vacuum pump is running.

If any repairs are required on the refrigeration module, contact your local
laboratory supply dealer. If your laboratory supply dealer is unable to provide
assistance, please call Labconco. Repairs should only be undertaken by a
competent refrigeration technician or through an authorized Labconco service
agency.

Access to Mechanical Components

(1) To gain access to the refrigeration system, pump, tank, and the controller

and control panel components, it is necessary to remove the cover on the
left side.

(2) Remove the stainless steel front panel and control panel. Disconnect the

wires to the power switch. Remove the left cover.

(3) Additional access is available by removing the remaining screws, which

hold the rear panel in place, and lifting it off the unit.

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Chapter 7: Troubleshooting

41

Shelf and Stoppering System Removal

(1) The shelf and stoppering system may be removed from the chamber as an

assembly for repairs if needed.

(2) Remove the acrylic door by taking out the two hex socket head screws

located on the right hand end of the cross bar.

(3) Remove the door gasket. Carefully pull loose all of the plastic fasteners

(located around the periphery of the chamber) from the chamber. Leave
the spacer blocks behind the gasket attached to the gasket.

(4) Place a support in front of the chamber and slide the shelf and stoppering

system out approximately 2 inches.

(5) Loosen the clamp securing the stoppering diaphragm tube (located in the

lower center at the back of the chamber) and remove the tube. Slide the
assembly out of the chamber and onto the support.

(6) The assembly is now ready for repairs. Whenever possible, do not break

the fluid system.

(7) Reverse the removal procedures for installation of the shelf and stoppering

system. Make sure the fluid inlet and outlet tubes are routed on top of the
assembly.

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Chapter 7: Troubleshooting

42

Filling the Fluid System

1. Fluid Circulation Valve

2. Fluid Reservoir and Cap

3. Electrical Junction Block

4. Flexible Tubing

(1) Make sure the Power Switch is in the OFF position.
(2) Remove the left cover.
(3) Remove the insulation and both caps from the fluid circulation valve,

which is located directly behind the fluid reservoir (Item 1).

(4) Attach a flexible tube to the exposed port (service port). The port is 3/8" x

45° male flare (Item 4).

(5) Remove the fluid reservoir cover (Item 2) and place the opposite end of

the tubing into the fluid reservoir.

(6) Fill the reservoir slowly allowing the fluid to drain through the system.

When the system appears full, prepare to start the circulation pump.

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Chapter 7: Troubleshooting

43

Name:

Lexol 542

Manufacturer:

Santa Barbara Chemical Co.
927 Indio Muerto
Santa Barbara, CA 93140
805-963-7793

!

(7) Open the fluid circulation valve by completely “down-seating” (turn top

valve stem completely clockwise) to direct fluid to by-pass through tubing
to fluid reservoir.

(8) Attach the power wires to the power switch. Activate the pump by

moving the Power switch to the ON position. The control panel does not
need to be installed. If it is installed, the RUN/STOP switch must be off.
The fluid system will circulate with the fluid going through the add-on
tubing, purging itself of air. Add fluid when needed to keep fluid in the
reservoir. After the fluid stream is established, tilt the stoppering system
up and down. Observe the fluid stream and repeat the tilt procedure if it is
not free of bubbles.

(9) After the system is free of air, “up-seat” fluid circulation valve (turn valve

stem completely counter-clockwise, closing the fluid/tubing by-pass).

(10) Set the controller to operate at 24°C (75°F) in the manual mode. Push the

“Run/Stop” switch to start the system.

(11) When the system temperature stabilizes, add or remove fluid from the

reservoir to the level indicated by the label.

(12) Apply vacuum to the unit, and when the system is

0.133 mBar or less install the cap on the tank.

(13) Remove the tubing. Replace the caps on the valve and replace insulation

and covers.

Heat Transfer Fluid Precautions

The fluid’s name and manufacturer are:

WARNING: The fluid used for heat transfer in this system is
combustible and hazardous. Leaks and spills should be
attended to immediately.

Handling and Storage Precautions – Dirty Solvent: Store in

accordance with all applicable regulations. Tighten caps and store in a
cool area.

Precautions if Material is Released or Spilled: Spills should be
contained immediately. Spills may be soaked up with absorbent materials,
placed in closed containers, labeled, stored and disposed of properly.
Persons performing this work should wear adequate personal protective
equipment and clothing.

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Chapter 7: Troubleshooting

44

Disposal of Non-Recyclable Solvents: Dispose of in accordance with all
federal, state, and local health and pollution regulations. Follow same
guidelines as used when disposing kerosene.

Heat Transfer Fluid First Aid Procedures

Eye Contact: Immediately flush eyes with fresh water for at least 15
minutes. If irritation persists, get medical attention.

Skin Contact: Wash contaminated areas with soap and water. Remove
contaminated clothing and footwear. Wash clothing before reuse. Discard
footwear, which cannot be decontaminated. Medical attention may be
required.

Inhalation: Remove patient to fresh air. If breathing stops, give artificial
respiration. Get medical attention immediately, if required.

Ingestion: Get medical attention immediately. Do not induce vomiting.

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45

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PRODUCTION MENU
MASTER RESET?

Your Stoppering Tray Dryer has been carefully calibrated and tested before
shipping, however under certain circumstances it may be necessary to adjust the
calibration of the vacuum display or to reset factory settings. These adjustments
may be necessary if the Stoppering Tray Dryer requires service.

An offset may be added to the vacuum display. Use an accurate traceable
reference to compare the readings.

Vacuum offset may be varied ±0.010 mBar in 0.001 mBar increments.

Modifying the Display

To enter an offset or to restore all factory settings, perform the following steps:

 Press the DISPLAY button until the Set Up LED is lit.
 Press and hold DISPLAY button for 10 seconds.

The display will first show the screen used for setting Auto mode
parameters and then will show:

Product Service 1-800-522-7658

Chapter 8: Modifying Your Stoppering Tray Dryer Display

46

VACUUM OFFSET:
0 mBar

PRODUCTION MENU:
MASTER RESET?

If you want to restore all factory settings hold ENTER approximately 5 seconds.

This will reset:

Vacuum units to mBar
Temperature units to °C
Refrigeration service hours to 0
Refrigeration total hours to 0
RS232 transmission rate to 10 seconds
Vacuum offset to 0 mBar

At the completion of Master Reset, the display will show operational parameters.

If you do not want to restore all factory settings, but want to adjust the vacuum
offset, press DISPLAY briefly and the display will show:

Press  or  until the appropriate offset is shown. Each number
represents an offset of 0.001 mBar

Press DISPLAY and the display will show

Wait approximately 10 seconds and the display will default to show operational.

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The following pages list components that are available for your Stoppering Tray
Dryer. The parts shown are the most common replacement parts. If other parts
are required, contact Product Service.

Product Service 1-800-522-7658

Appendix A: Stoppering Tray Dryer Components

48

Item

Part No.

Qty

Description

1

7592002

1

Compressor 115V – 60 Hz

7592001

1

Compressor 230V – 50 Hz

7592000

1

Compressor 230V – 60 Hz

2

7501900

1

Lexsol Pump 115V

7501901

1

Lexsol Pump 230V

3

7510900

1

Heater 115V

7510901

1

Heater 230V

4

7529500

1

Bulkhead Harness

5

7353300

1

Temperature Sensor - System

6

7353301

3

Temperature Sensor – Sample

7

7765500

1

Diaphragm

8

7590600

1

Door Gasket

9

1926201

20

Clip - Door Gasket

10

7766801

2 Gal.

Heat Transfer Fluid (Not Shown)

11

7353500

1

Printed Circuit Board Control

12

7448000

1

Printed Circuit Board RS232

13

7684200

2

Coupling – Vacuum

14

1966900

4

Clamp Coupling

15

7769402

1

Door Assembly

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Appendix A: Stoppering Tray Dryer Components

49

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Appendix B: Stoppering Tray Dryer Dimensions

51

Size Labconco No.

Shelf Capacity

No. of Shelves

Total

Capacity

2 ml 7575010

430 3 1290

3 ml 7575210

483 3 1449

5 ml 7573010

255 3 765

10 ml 7573210

195 3 585

20 ml 7573410

132 3 396

30 ml 7573610

86 3 258

50 ml 7573810

72 2 144

100 ml 7574010

42 2 84

125 ml 7574210

36 1 36

Serum Bottle Capacity of the Stoppering Tray Dryer

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Voltage

Catalog

Number

Description

Nominal

Operating

Range

Frequency

Phase

Amperage

7948020

Stoppering Tray Dryer

115

103-127

60 1 16.0

100

98-110

50 1 16.0

7948030

Stoppering Tray Dryer

230

208-254

50 1 9.0

7948040

Stoppering Tray Dryer

230

187-253

60 1 9.0

7948060

Stoppering Tray Dryer

230

208-254

50 1 9.0

7948070

Stoppering Tray Dryer

230

208-254

50 1 9.0

This Appendix contains technical information about the Freeze Dryer including
electrical specifications and environmental operating conditions.

Electrical Specifications

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 over voltages according to Installation Categories II (Over

voltage Categories per IEC 1010). Temporary voltage spikes on the AC
input line that may be as high as 1500V for 115V models and 2500V for
230V models are allowed.

 Used in an environment of Pollution degrees 2 (i.e., where normally only

non-conductive atmospheres are present). Occasionally, however, a
temporary conductivity caused by condensation must be expected, in
accordance with IEC 664.

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PART #

DESCRIPTION

7726500

6 Port Manifold for use with Stoppering Tray Dryer

Mounts between the Stoppering Tray Dryer and the base unit and
provides 6 freeze dry valves.

7537800

Cable

Connect the RS232 output from the Freeze Dryer (or Freeze Dryer/Tray
Dryer combination) to an IBM compatible computer with a 9-pin serial
data port.

7537801

Cable

Connects the RS232 output from the Freeze Dryer (or Freeze Dryer/Tray
Dryer combination) to an IBM compatible computer with a 25-pin serial
data port.

7761500

Isolation Valve

Mounts between the Stoppering Tray Dryer and the base unit, which
provides a way to isolate the base unit vacuum system from the
Stoppering Tray Dryer vacuum system.

7756100

Tray with Slide-Out Bottom

14" wide x 12" deep. Stainless steel tray has separate bottom, which
slides out allowing serum bottles, and ampules direct contact with the
shelf to facilitate the drying process.

7756200

Bulk Tray

15" wide x 11-1/2" deep. Stainless steel tray will contain liquids for
bulk drying.

7756300

Shelf Spacers

2-1/2" high x 9" wide x 13" deep. Two stainless steel spacers placed on
one or two empty shelves assist stoppering of partial loads of small vials
or bottles.

7516200

Support Grid

7" wide x 7" deep. Stainless steel tray with removable plastic grid
provides support for stoppering ampules and other small specimen
containers while stoppering under vacuum. Grid holds 144 ampules of
12 mm diameter.

The following accessories are available for the Freeze Dryer.

Product Service 1-800-522-7658

Appendix D: Stoppering Tray Dryer Accessories

54

Size

Vials with

Screw Caps

Stoppers

5 ml

7762300

7762200

10 ml

7762600

7762200

Size

20 mm

Corkage

13 mm

Corkage

Split

Stoppers

Aluminum

Seals

Sleeve-Type

Stoppers

2 ml 7575010

7576010

7577010

3 ml 7575210

7576010

7577010

5 ml

7573010

7576210

7577110

757710

10 ml

7573210

7576210

7577110

7577510

20 ml

7573410

7576210

7577110

7577510

30 ml

7573610

7576210

7577110

7577510

50 ml

7573810

7576210

7577110

7577510

100 ml

7574010

7576210

7577110

7577510

125 ml

7574210

7576210

7577110

7577510

Threaded Vials

Stoppers and threaded vials with Screw
Caps are supplied in packages of 200.

Perfect for long term storage of freeze
dried samples. Labconco Serum
Bottles and Treaded Vials are
specifically designed for lyophilization
applications. Their uniform thin 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 and manifolds.

Serum Bottles

Serum Bottles, Stoppers and seals
are supplied in packages of 100.

Seal Crimper

Secures tear-away Aluminum Seals.

7578000 Seal Crimper for 13 mm corkage.
Shipping weight 3 lbs. (1.4 kg)
7578100 Seal Crimper for 20 mm corkage.
Shipping weight 3 lbs. (1.4 kg)

Serum Bottles and Vials

Product Service 1-800-522-7658