Labconco FreeZone 7750000 Manual de usuario

FreeZone® Benchtop and Console

Freeze Dry Systems

Models

7750000 7751000

7750001 7751001

7750003 7751003

7750004 7751004

User’s Manual

LABCONCO CORPORATION

8811 PROSPECT AVENUE

KANSAS CITY, MO 64132-2696

800-821-5525, 816-333-8811

FAX 816-363-0130

E-MAIL [email protected]

HOME PAGE www.labconco.com

Labconco’s Mascot,

Labby the LABster

www.labconco.com/productreg.html

or return the attached card and

receive FREE LabbyWear™!

Product designs are subject to change without notice

Printed in U.S.A.

Labconco Corporation

8811 Prospect Avenue

Kansas City, Missouri 64132

The information contained in this manual and the accompanying product are copyrighted and all rights are

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.

FreeZone® is a registered trademark of Labconco Corporation.

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® Delta® Series Biological Safety Cabinets carry a three-year warranty from date of

installation or four years from date of shipment from Labconco, whichever is sooner.

• 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 also not covered.

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.

Visit Labconco’s web site at: http://www.labconco.com or email Labconco at: labconco@labconco.com.

Part #7519800

REV C/ECO B176

☞

CHAPTER 1: INTRODUCTION 1

FreezeDryProcess 1

FreezeDryRates 2

FreezeDryCapacity 4

Samples Containing Volatile Substances 5

About This Manual 5

Typographical Conventions 7

YourNextStep 7

CHAPTER 2: PREREQUISITES 9

ElectricalRequirements 10

Location Requirements 10

Vacuum Pump Requirements 10

Space Requirements 11

YourNextStep 11

CHAPTER 3: GETTING STARTED 13

UnpackingYourFreezeDryer 14

Freeze Dryer Components 14

Setting Up Your Freeze Dryer 15

Component Orientation 15

Vacuum Pump Connection 16

ElectricalConnection 16

Solvent Safety Precautions 16

YourNextStep 18

CHAPTER 4: USING YOUR FREEZE DRYER 19

FreezeDryerControls 20

OperationChecklist 22

Vacuum Pump Ballast Setting 22

Operating the Freeze Dryer 23

AutomaticStart-Up 23

ManualStart-Up 23

AddingSample 24

Alarms&InformationalMessages 26

ShutDown 27

Defrosting 28

CHAPTER 5: MAINTAINING YOUR FREEZE DRYER 29

CHAPTER 6: USING THE RECORDER JACK 31

Recorder Jack Pin Configuration 31

Computer Connection 32

CHAPTER 7: TROUBLESHOOTING 37

VacuumPump 37

Gaskets, Tubing, Connections, Sample Valves 38

System Components & Collection Chamber Isolation 40

Refrigeration Module Operation 42

APPENDIX A: FREEZE DRYER COMPONENTS 43

APPENDIX B: FREEZE DRYER DIMENSIONS 49

APPENDIX C: FREEZE DRYER SPECIFICATIONS 51

Electrical Specifications 51

Environmental Conditions 52

Wiring Diagram (115V) 53

Wiring Diagram (230V) 54

APPENDIX D: FREEZE DRYER ACCESSORIES 55

DECLARATION OF CONFORMITY 65

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Congratulations on your purchase of a Labconco Freeze

Dry System. Benchtop and console models are

available for operation on 115V or 230V.

The Labconco FreeZone® 4.5 Liter Freeze Dry System

is designed for laboratory lyophilization procedures. It

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

Dehydration is an important process 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

microorganisms). 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 is removed

from frozen materials by converting the frozen water

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Chapter 1: Introduction

directly into its 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 three 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.

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

*Total sample quantities are contingent on various freeze dryer capacities.

Table 1

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Chapter 1: Introduction

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 ice 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 10 to 15°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 most applications, the maintenance of

a vacuum of 133 x 10-3 mBar or less is required for

freeze drying to occur.

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 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 at 0°C. Although the

eutectic temperature is not dependent upon the

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

Chapter 1: Introduction

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 to less than 133 x 10-3 mBar,

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

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Chapter 1: Introduction

cascade type refrigeration so that the collector

temperature can be cooled to below –75°C, or a dry

ice/solvent trap can 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 acetic

acid, formic acid or pyridine. In addition to these

substances having an effect on the eutectic temperature,

they may enhance 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, freeze drying samples that contain volatile

substances will have a greater tendency to melt,

particularly when placed in flasks or exposed to room

temperature. If a sample containing a volatile

substance tends to melt when placed on a freeze dry

system, dilution of the sample with more water will

help keep the sample frozen. For example, a 0.2M

solution of acetic acid is much easier to freeze dry than

a 0.5M solution.

About This Manual

This manual is designed to help you learn how to

install, use, and maintain your Freeze Dryer.

Instructions for performing routine maintenance and

making minor modifications to your Freeze Dryer are

also included.

Chapter 1: Introduction provides a brief overview of

the Freeze Dryer, explains the organization of the

manual, and defines the typographical conventions used

in the manual.

Chapter 2: Prerequisites explains what you need to do

to prepare your site before you install your Freeze

Dryer. Electrical requirements are discussed.

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