Labconco 8 Operating Manual
Cox
x
INSTRUCTION MANUAL
FREEZE DRYER 8
75040-01
S/N
(61383
>pectek
Aa:
LABCONCO CORPORATION, 8811 PROSPECT, KANSAS CITY, MO. 64132, 816—333-8811
Dear Customer:
This letter is to insure that you get the best performance from your
new Labconco product. We want to be sure you are satisfied. If damage
has occurred in shipping, the customer must file a claim with the carrier
IMMEDIATELY. DO NOT return any items to Labconco Corporation without
written authorization from the factory. Your local laboratory apparatus
dealer can assist you, and should be contacted if problems occur. If
satisfaction is not obtained, contact Labconco Corporation.
A great deal of care has gone into the engineering, production and ultimate
quality control of your Labconco product. That is why we affix this badge
to our products. Your satisfaction is of great concern to us.
ASSEMBLED BY:
DEPT. MANAGER:
О. А. ТЕСНЫ КАН:
PACHAGED EY:
We know that even the best products require service from time to time.
So if this is ever true of your Labconco product, call the service depart-
ment of the dealer from whom you purchased the unit. He is trained to
make whatever might be wrong with the unit right. If you need additional
help, call. us at (816) 333-8811 and ask for our Service Manager. We will
make sure that you get all the help you need. |
We suggest you keep all of this material together. It's nice to know you
are protected, even though you may never need it.
Sincerely,
LABCONCO CORPORATION
TABLE OF CONTENTS
Introduction to Freeze Drying ..............e_e_._e.exedonesavrererosovereorecaooedarono, 1
Freeze Drying Process ...........—..coweceoracnedarararneorararo vccrarearerecnonecno 1
Freeze Drying Rates ................eseo0envcaroxacarorereoaoorencooceroarven arar 1
Surface Area and Thickness of the Sample. ................ezcorrescreacavereaveno „1
Condenser Temperature and Vacuum Attained................_.eeoecsorcoooveoaa 2
Melting Temperature and Solute Concentration of the Sample.................... ‚2
Capacity of Freeze Dryers............_.eeere_recessceroorecocarorcorerrocaroeasvereno 3
Samples Containing Volatile Substances............_—.—e—e_corecesresrrccoccarcorerocameno. 3
Installation ..........._.eoencrrrererceesrcecorcacrcaneorrorvrerarenCarcorenracanmorvonooreooneo 4
Installation Factors. ............__.eeooororcesossersrercaoreraneorenanooravoacerara 4
Start Up and Initial Checkout .............eoeoecerc_e__r_r_r.ervoccorcccoraconarar oe 4-5
M [email protected] e175:1110), PA 5
Freeze Drying - Manifoid Drying Procedures .................e.e00ceeree00e 00 A 6
Freeze Drying - Bulk Drying Procedures .............r.e.—reeseeeccsscoroc;eocan enero 6
Defrosting................_oe..eeerecorresarcvorocerarecivasereoorereearacanrenaaooce 6-7
Routine Maintenance ..........._.e_cooreenrscoensrvoscesoccoreroresnarorereroraracvaocoaoo 7
Vacuum System Leak Detection................._corrceercercecordararascaocoaoro. 7-8
Refrigeration System Leak Detection...........—...__eocoroonrorereresseorereecace 8
Instrumentation ........... necroccocr:ear career raro roanooaoccarnavervenraavanarmaaras 8-9
Vacuum System Trouble Shooting. ..............._._eooorcceereoveccocorereacecareo 10
Refrigeration System Trouble Shooting .............eeeeeoeecararroeorarocorecora 11
Valve Diagramm... ENKEFEKEKKRRERERERRERRERKER RR KK 12
Labeled Parts Diagram...........e_e._erees0o0renaasocsoacoooerecaarorocadanearonosoroCcerevo 13
Replacement Parts List 0000000000000 eee a ae a a a a a a ae aa 14
Electrical Schematic Model 75040 .............e_eeenresscorsaeaoororororecrearcen ere: 15
Electrical Schematic Model 75040-01
Product Designs Are Subject To Change Without Notice
©1985 LABCONCO CORP.
FORM 76925 / ECO 5238 REV. E/ PRINTED IN U.S.A.
INTRODUCTION TO FREEZE DRYING
The Freeze Drying Process
Dehydration is an important process for the
preservation and storage of biologicals, pharma-
ceuticals, and foods. Of the various methods of
dehydration, freeze drying {lyophilization) is espe-
cially suited for substances that are heat sensitive,
Other than food processing (e.g., coffee, whole
dinners), freeze drying has been used extensively
in the area of pharmaceuticals (e.g., antibiotics)
and biologicals (e.qg., proteins, plasma, viruses,
and microorganisms). The nondestructive nature
of this process has been demonstrated by the
retention of viability of freeze dried viruses and
microorganisms,
Freeze Drying is a process whereby water is
removed from frozen materials by converting the
frozen water directly into its vapor without the
intermediate formation of liquid water. The basis
for this sublimation process involves (1} the absorp-
tion of heat by the frozen sample in order to
vaporize the water, (2) the use of a vacuum pump
to enhance the removal of water vapor from the
surface of the sample, (3) the transfer and deposit
of the water vapor onto a condenser, (4) the
removal of heat, due to ice formation, from the
condenser by means of a refrigeration compressor
or a dry ice solvent bath. in essence the freeze
drying process depends upon a balance between
the heat absorbed by the sample to vaporize the
water and the heat removed from the condensor
to convert the vapor into ice.
Freeze Drying Rates
The efficiency of the freeze drying process is
depended upon (1) the surface area and thickness
of the sample, (2) the condensor temperature
and vacuum obtained, and (3) the melting tempera-
ture and solute concentration of the sample.
These factors will be helpful in the efficient
utilization of your freeze dryer unit. A listing of
selected materials and their drying times are
shown below for your reference.
SAFE TEMPERATURE AND DRYING TIMES |
FOR SELECTED MATERIALS
1OMM THICK TEMPERATURE TEMPERATURE (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
Vegeiable
Tissue —50 —80 60
*Total sample quantities are contingent on various freeze dryer capacities.
Surface Area and Thickness
Of the Sample
Up to the point of overioading the system, the
greater the surface area of the sample, the greater
the rate of freeze drying. By contrast for a given
surface area, the thicker the sample the slower
the rate of lyophilization. This is based upon the
fact that the heat of sublimation is usually absorbed
on one side of the frozen sampie and must travel
through the frozen layer to vaporize water at the
other surface. in addition, if the sample is lyophilized
the water vapor must travel through the layer of
dried material. The thicker the sample, the greater
the chance that the dried layer can collapse
which would cause an additional decrease in the
rate of freeze drying.
The surface areaandthickness of the sample can
usually be ignored when each sample only
contains 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. Sample volume of the
lyophilizer flask should be two times the volume of
the sample.
Condenser Temperature and
Vacuum Attained
In order for lyophilization to occu I, the water vapr at
the surface of the frozen sample must be removed.
This is accomplished by a condenser and the
vacuum pump. The condenser which should be at
least 10 to 15 degrees C. colder that the eutectic
temperature (meiting temperature) of the sample,
serves to trap the water vapor as ice. Since the
vapor pressure at the condenser is less than that of
the sample, the net flow of water vapor is from the
sample tothe condenser. While this vapor diffusional
process could occur very slowly in air, a good
vacuum is essential to maintain a sufficient diffusionat
rate. In most applications the maintenance of a
vacuum of 100 microns or less is required for
freeze drying to occur: in general, a vacuum of 20-
30 microns will be obtained.
— DRY CAKE
FROZEN
CAUTION: Since most but not all of the vapors
will be trapped by the condenser, the vacuum
pump ballast must always be open a small amount
in order to allow the vapors to be removed from
the pump oil.
SAMPLE
INTERFACE
Melting Temperature and
Solute Concentration of the Sample
The rate of lyophilization is directly proportional to
the vapor pressure and the vapor pressure is
dependent upon both the eutectic temperature
and solute concentration of the sample. For example,
a solution of sodium chloride would lyophilize 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 of pure water
is about 1/16 that 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 genera! most solutions or biological samples
will have a eutectic temperature of -10 to -25
degrees C. However, ifthere is 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.
Capacity of Freeze Dryers
The volume of a sample (capacity) thai can be
freeze dried at one time is related to the factors
discussed previously and the size and design of
the freeze dryer. With any given instrument, the
capacity is based upon (1) the surface area ofthe
frozen sample, (2) the eutectic temperature of
the sample, (3) the concentration of the sample,
and (4) the rate and amount of heat transferred to
the frozen sample. Of these factors, the eutectic
temperature is the most important in determining
the amount of sample that can be lyophilized at
one time, particularly when flasks are used. This
is because, as the eutectic temperature decreases,
the vapor pressure decreases whereas the rate
of the heat absorption by the sample does not
decrease. This tends to promote melting of the
sample which leads to a marked increase in
vapor pressure and ultimately overloads the
condenser and vacuum pump. Samples that
have eutectic temperatures of -20° C. or lower
should be placed onthe freeze dryer one flask at
a time so as to allow the vacuum of the system to
recover before placing another sample on the
machine. If the vacuum does not recover to less
than 100 microns, the capacity of the freeze
dryer has been exceeded and the sample should
be removed. Ifthere is a probiem with a particular
type of sample melting when placed on the
freeze dryer, dilution of the sample with more
water or providing some insulation around the
flask to decrease the rate of heat absorption by
the flask may help. Hf the eutectictemperature of
the sample is-40 to-60° C., the freeze dryer must
be equipped with a cascade type of refrigeration
system so that the condenser temperature can
be cooled to below -80° C.
SAMPLE PRE-FROZEN rp
TO -10°C 3 a
SUBLIMATION
TAKING O:
E
REFRIGERANT
E
REFRIGERATION COMPRESSOR
oy
sé
AIR BEING REMOVED
> ts
> a ES
NN
NA
A
/] } FROM SYSTEM
VACUUM PUMP
Samples Contain Additional
Volatile Substances
in certain cases the solvent used for freeze
drying a sample, in addition towater, may contain
another volatile component; (e.g., acidic 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 all require the absorption of less
heat for sublimation to occur. Hence, freeze
drying samples that involve the sublimation of an
additional substance will have a greater tendency
to meit, particularly when placed in flasks or
exposed to room temperature. If a sample
containing an additiona! volatile substance tends to
melt when placed on a freeze dryer, dilution of
the sample with more water may help keep a
sample frozen; for example, a 0.2 M solution of
acidic acid is much easier to lyophitize thana0.5 M
solution.
Installation
Your laboratory freeze dryer unit has been
shipped toyouinone carton {optional equipment
has been packaged separately).
Q
Installation Factors
Once you have completed the unpackaging of
your Labconco Freeze Dryer unit, check for any
internal freight damage that may have occurred
during transit. Once this is completed, you
should also check the refrigeration components
prior to installation and operation.
Check the refrigeration components as follows:
1. inspect all refrigeration components for
visible damage and check the condenser
fan to insure unobstructed operation.
Observe pre-rotation on the fan blade when
the refrigeration side is switched on.
Be sure to inspect the freeze dryer thoroughly prior
to installation. Report any damage that may have
occurred in transit.
3. A vacuum pump with a rated capacity of at
least 100 liters per minute is required to
operate your freeze dryer unit properly. The
unit itself is provided with a 3" 1.D. heavy wall
vacuum hose for connection between your
vacuum pump and the freeze dryer unit
refrigeration system. Place the vacuum
pump itself on the movable shelf internal to
the freeze dry cabinet and secure to the
vacuum hose with the enclosed hose clamp.
WARNING: Do not allow the vacuum hose to kink
when it is installed. If the hose is too long for the
vacuum pump that you have selected, cut the
hose down to a suitable length prior to installation.
WARNING: Disconnect the freeze dryer unit
from the main power supply connection before
inspection and maintenance procedures are
performed on the unit.
o Locate the freeze dryer unit in an area that
provides an unobstructed flow of air around
the cabinet. This air acts as cooling airto the
refrigeration system. The refrigeration system
draws the air through the grill on the front
panel and exhausts it out through the back. A
minimum of 3” must be allowed between the
freeze dryer unit and the wall surface, of the
openings on the cabinet while the unit is in
operation, as the performance will be adverse-
ly affected. Periodically remove any dust
from the front grili and condenser to maintain
optimum performance.
Start Up An Initial Check-Out
Before nominal everyday usage of your freeze
dry unit begins, a functional check of the refrig-
eration system should be performed to insure
proper operation of the machine.
The check list of steps required for this procedure
are as follows:
4. Clean the rubber gasket onthe clear, acrylic
condenser chamber closure to remove dirt
and other contaminants that could be a source
of vacuum leakage. As arule, vacuum grease is
NOT required to obtain a vacuum. if vacuum
grease is used, the procedure should be as
follows:
A. Clean both surfaces witha soft cloth or
paper towel to remove old vacuum
grease and/or dirt that may have
accumulated.
B. Apply a very thin film to one surface
only,
C. Use a soft cloth or paper towel to wipe
off all excess grease.
Wipe the interior of the condenser chamber
with a soft cloth or paper towel to remove any
moisture that may have accumulated during
transit. Reposition the acrylic cover on the
unit, when this is complete.
Checkthe drain line of the condenser chamber
toinsure that the line has its plug in place and is
free of moisture.
Install accessories, (ie. manifold and/or
chamber), to the base unit as required.
Connect your freeze dryer to a power supply.
Locate the control switch marked REF, on
the front of the cabinet. Turnthe switchtothe
on position. Allow the condenser unit to
reach a temperature of -40° C. or lower.
5. Locatethe control switch marked VAC on the
front of the cabinet. Turn the switch tothe on
position and wait until the vacuum pump
pulls a system pressure of 25 microns or
lower to assertain that there are no vacuum
leaks in your system.
NOTE: All performance ratings represented in
this manual are given for an ambient condition
of 21° C/70° F at the rated voltage and 60 Hz
electrical service.
Normal Operation
Once you have gone through the initial installation
and check list for your freeze dry unit and have
ascertained that it is in proper working condition,
you are now ready to proceed with the actual
operation of the equipment.
The operating instructions for the unit are printed
on the freeze dryer switch plate located on the
front panel of the cabinet and also here for your
review,
Follow the steps as listed on the switch plate
each time you use the unit for overall optimum
performance.
O.
OPERATEMG EASTALICTEGNS
с TURIN ON RES МАДАМ Рая,
ON 50 NOT; FAOCFEO UALESS TEMPERATURE KG a ON
OA LOWER,
VAC, on CHECA YACLEAS Poio CL CIMA OFF
AND CUANTITY ECFORE STARTIGO FLA,
CHANGE OL WHEN DEITY OF CLOUÈPE
OFF DEF.
Ex) MONTI Ly SEMPLES LATE, 50 LCD Y ALLA RS
5 RECACIAS DA LESS.
tx OPERATE YALA РОМ №; me OPEN TO
PLRGE DHL GF ANT ACCMNATED TE
De TERM OFF MACHIRE IN POLL CARO SECUENDE
ELIA,
FREEZE DRYER 8
Freeze Drying-
Manifold Drying Procedures
1.
Pre-freeze samples. Appropriate containers
for freeze drying include ampules, serum
bottles, and wide-mouth freeze drying flasks.
Proper sample container size should always
be no more than two times the sample size.
Examples: 150 ml samples should be prepared
in a 300 m! container, a one liter sample
should be prepared in a two liter container,
etc. Shell-freezing of samples is recom-
mended. Shell-freezing is accomplished by
rotating or swelling the liquid sample during
the pre-freezing process. Rotating or swelling
action distributes the frozen sample into a
thin shell over the internal surface of the
container.
Connect the pre-frozen samples one at a
time to a vacuum valve on your manifold
assembly. Although samples can be connect-
ed to any size valve, a small (2) vacuum
valve is generally used for samples less than
150 ml. The large (3) valve can be used for
either small or large samples. After connecting
pre-frozen samples to a vacuum valve, turn
the plastic valve knobto the “VAC” position to
open the valve (Figure B), shown on page 15.
Allow the system pressure to return to a
vacuum of approximately 100 microns orless
before adding additional samples to the unit.
Any combination of valves and sample sizes
may be used at one time. Provided the
system vacuum remains sufficiently low to
prevent meltback and the condenser temp-
erature remains below -40° C.
Ambient temperature plus water vaporin the
room condensing on the outer surface of a
sample container will usually supply sufficient
heat for rapid sublimation of your material.
Samples containing salts and/or sugars with
depressed freezing points may tend to melt-
back, and require insulation from room heat.
When all the frost has disappeared from the
outer surface of the sample containerand no
cold spots can be detected by handling the
container, the sample is nearly dry. To be
certain of low final moisture content, dry the
sample for several more hours past this point.
To remove a flask after drying is complete,
turn the plastic knob on the vacuum valve, to
the closed position (“VENT”). Should you
desire to backfill with nitrogen gas or other
types of material, this can now be accom-
plished at this time by connecting through
the vent port on the valve as shown in Figure
B.
7. Ampules may be flame sealed while connected
to a vacuum valve by using a sealing torch.
The oxygen/natural gas torch is recommended
for the borosilicate glass ampules.
For ampules with short stems, it will be
necessary to place an insulation material
between the vacuum valve and the torch
flame to prevent any damage to the rubber
valve structure.
Freeze Drying - Bulk Drying Procedures
The inside area of the combination, bulk, and/or
other drying chambers (see Labconco catalog)
may be used to bulk freeze dry large pre-frozen
volumes of material in trays, or for processing
samples in containers such as serum bottles,
Petri dishes and/or beakers.
Defrosting
Frequent defrosting of the condenser on your
freeze dry unit is recommended to keep the
defrost times short and your unit's efficiency at
its peak. The following steps shouid be used in
defrosting your freeze dry unit.
WARNING: If acid has been used as part of
the sample, flush out condenser with cold water
before defrosting. This will keep acid(s) from
attacking the materials used in the condenser
chamber,
1. Release the vacuum inside the condensor
chamber by using either a valve or the drain
line connection.
2. Turn off refrigerator system and the vacuum
pump.
3. Place the condenser drain hose in a suitable
container for the accumauition fo the moisture
that will be removed from the condenser.
4, For rapid defrost, turn the REF./OFF/DEF.
switch to the defrost position. Allow the con-
denser to defrost a minimum of 30 minutes.
After the bond between the ice and the
condenser is broken, remove the ice intact
and turn the switch to the “OFF” position.
WARNING: Do not attempt to chip ice off the
condenser, as serious damage to the refrigeration
system may result.
5. If the rapid ice removal is not desired, the
frozen condensate may be allowed to meit
and drain out through the drain line at room
temperature.
6. The condenser chamber should be flushed
with water after each defrosting. This flushing
cleans out any material that may have collected
on the walls of the condenser chamber and
should be wiped dry prior to going back into
normal operation again.
7. Replace the drainline plugwhen the draining
of the condenser chamber has been com-
pleted.
Routine Maintenance
Cabinet Maintenance
1. Moisture in the vacuum pump and insufficient
pump oil are major causes of poor performance
of freeze drying equipment. Frequently check
the pump oil for signs of water or low oil level.
To expel small amounts of water which may
accumulate in the pump oil, it is advisable to
occasionally operate the pump against a dry,
tight system with the gas ballast open.
WARNING: Evidence of mercury or other contami-
nants in the vacuum pump will void warranty.
1. If the oil in your vacuum pump contains
excessive moisture, it will be necessary 10
change the oil. For further information in
regard to exact procedures of changing the
vacuum pump oil, refer to the vacuum pump
manufacturers instructions.
o Ali rubber parts on your freeze dryer unit will
eventually deteriorate and will require replace-
ment. The effective life of rubber parts will
depend upon both their usage and the
surrounding environment. ltis recommended
that allrubber hoses and gaskets be checked
frequentiy and replaced when signs of
hardness, permanent set, or deterioration
occur.
3, To clean the acrylic cover, wash with a non-
abrasive soap or detergent and water, using
the bare hand to feel and dislodge any dirt. A
soft grit-free cloth, sponge, or chamois may
be used. The cloth or chamois may be kept
free of grit by rinsing frequently in clean
water. Dry with a clean, damp chamois prior
to reinstallation. Hard, rough cloths will scratch.
Where water cannot be used freely, dust very
lightly with a soft cloth or feather duster.
4. To clean the exterior of your freese dryer
cabinet, wash with a non-abrasive soap or
detergent and water. Liquid spray cleaners
and polishes may be used. Do hot use solvents
to remove the stains from the cabinet finish
as the finish may be damaged.
Vacuum System Leak Detection
The Labconco Freeze Dryer can achieve an
ultimate vacuum of 25 microns of mercury (10 x
103 Torr.) or lower under a no-load condition. in
order to achieve sufficent vacuum, it is necessary
that afl joints and connections be tight, that the
vacuum pump is operating properly and that the
condenser refrigeration temperature is -40° C or
lower. If the Freeze Dryer does not obtain a
satisfactory vacuum, the following procedure
should be used to locate and correct vacuum
system problems:
1. General Connections
A. Make sure vacuum gauge is working proper-
ly, that there are no leaks in the connecting
line, and that the system is dry.
B. Check vacuum pump oil sight gauge for oil
condition. Replace the oil if it is dirty or
cloudy. Add oil to the pump if the ¡eve! is
low. Close the pump gas ballast valve. -
(See vacuum pump manufacturers instruc-
tions for additional information.)
C. Remove or isolate the drying chamber
from the vacuum connection. Where appli-
cable, plug or stopper the 3" vacuum
connection using a rubber gasket with a
back-up plate of metal or plastic. (A
convenient acrylic plug is available for this
purpose--Labconco Part No. 76426.)
D. Turn on vacuum pump. If the vacuum
pump is less than 25 microns, the leak was
in the drying chamber. Clean and lightly
grease gasket of drying chamber and
check all valves and make sure they are
clean, and fully closed. Reconnect the
chamber to the Freeze Dryer and turn on
the vacuum pump. If unable to achieve
sufficient vacuum, contact your dealer
representative or if satisfaction is not
obtained there, contact Labconco Corp.
directly. If vacuum leak was not in the
drying chamber, proceed to the next step.
Plug the vacuum line that connects the
vacuum pump to the condenser chamber.
The plug isolates the vacuum pump and
connecting hose from the condenser
chamber.
Turn on the vacuum pump and observe the
vacuum gauge. The pressure should drop
to approximately 5 microns immediately. If
the vacuum is sufficient, the vacuum pump
and hose connection is not the source of
the leak, the leak is therefore located inthe
condenser chamber, and you should pro-
ceed to Step W. If the vacuum is not
sufficient, the leak is in the vacuum pump
or connecting hoses and you should pro-
ceed to Step 2.
2. Vacuum Pump Connection
A. Turn off the vacuum pump and vent the
vacuum.
B. Disconnect the vacuum hose connection
at the pump and connect the vacuum
gauge directly to the pump inlet. A gauge-
to-pump connection can be made by boring
a small rubber stopper to accept a gauge
connection {usually 3" or Va" metal or glass
tubing), and inserting the stopper in the
pump inlet. Grease lightly alt connections
with silicone vacuum grease at this time.
Turn on the vacuum pump. The pressure
should drop to approximately 5 microns or
lower immediately. if not, the pump is
defective. If the vacuum is sufficient then
the leak is not in the pump itself, but is in
the hose connections between the pump
and the condenser chamber.
Disconnect the vacuum hose and vacuum
gauge connections inside the cabinet and
lightly regrease the joints with silicone
vacuum grease. Reconnect the joints
themselves using the hose clamps and
retest.
3. Condenser Chamber
A. Check the seal on the condenser chamber
closure gasket. Wipe seal clean with a soft
cloth and inspect the gasket for cracks,
tears, or indentations. If the gasket is
found to be in good condition, regrease
seal with a very thin, stiicone vacuum
grease and reinsert on the closure lid itself.
inspect the vacuum lines for cracks and
tighten all clamps. Check tightness of all
nuts and screws on the condenser chamber
area and check all welded connections for
cracks or leaks.
B. Turn the refrigeration system on and allow
the unitto reach temperature (-40°) C. Turn
on the vacuum pump. The vacuum should
drop to 25 microns or lower within 20
minutes if the leak has been corrected. For
additional assistance, contact your dealer
service representative or if satisfaction is
not obtained, contact Labconco Corp.
directly.
Refrigeration System Leak Detection
Should repair of any refrigeration component be
required, contact a laboratory supply dealer
immediately. If satisfaction is not obtained
through the dealer service network, please contact
Labconco Corp. directly. Repairs should only be
undertaken by a competent refrigeration tech-
nician or through an authorized Labconco service
agency.
1. Performance
Under a no-load condition (dry, water vapor
condenser without ice and a vacuum of 25
microns or lower) the water vapor condenser
temperature will reach -40% C or lower
depending upon ambient temperature and
humidity. Ifthe temperature does not reach -
-AO° C. within 20 minutes, the system is not
functioning properly.
Should you detect that your system is not
functioning properly, refer to the trouble
shooting chart, refrigeration system and
electrical schematic for problem solving and
construction details on your specific Freeze
Dry unit.
Instrumentation
The instrumentation on your Freeze Dry unit
consists of a thermocouple temperature indicator
for the water vapor condenser and a vacuum
gauge forvacuum indicationon the total system.
Repair and maintenance suggestions on both of
these two indicators are as follows:
4. Thermocoupie Temperature Gauge
The thermocouple is iron constantan and is
located on the water vapor condenser coils.
The gauge is a dual-scale CF and °C) in-
dicating meter. Erratic temperature indic-
ation, high temperature indication, or fiuct-
uation of the indicating needle is possibly
due to a loose connection in the thermo-
couple circuit.
CAUTION: Prior to checking loose connections
on your thermocouple gauge, disconnect the
main power to the Freeze Dryer unit. Check to
see that the lead connections on the back of the
meter are clean and tight. Also checktoseeifthe
thermocouple is making positive contact on the
refrigeration coil. Failure of the meter to show
any change in temperature is an indication of a
damaged meter.
Repairofa damaged meteris not feasibleandthe
meter must be replaced. Continuous indication
of a temperature at or near room temperature is
an indication of either an open or short circuit in
the thermocouple wire.
2. Electronic Vacuum Gauge
The electronic vacuum gauge Figure A does
not require mercury for operation. This
vacuum gauge operates ona thermal principle
and because of this, it is effected differently
by different gases, therefore any particular
reading wit! depend upon the gas components
being measured. The gauge itself will measure
condensables as weil as non-condensable
gases. The principie advantage of the
electronic vacuum gauge is its ability to give
a continuous indication of the relative vacuum
conditions. The gauge is not as absolute as
the mercury McLeod gauge, and therefore a
difference in indication between those two
measuring devices is to be expected and
should not be construed as an inaccuracy on
the part of either, but merely a normal difference
hetween two types of measuring systems.
Although the electronic vacuum gauge res
quires no routine maintenance, should ad-
justment for calibration become necessary,
please consult Figure A for instructions.
NEEDLE y _ $ SWITCH
== ace POT
O
AO JUSTMENT ADJUSTMENT
| |
| 7 1000 |
| All) om
г | я YELLOW i
MICRONS Hg
VACUUM
NEEDLE
ADJUSTMENT
Electronic Gauge
Figure A
Method Of Adjustment Is As Follows
1. With power OFF and unit under atmospheric
conditions, turn the needle adjustment screw
so needle is on line with atmosphere mark.
9. Turn power to gauge “ON.”
3, The switch is a TWO position switch, Positioning
the switch will cause the needle to be in
either the “zero” or the “atmos” side of the
meter.
4. Adjust the pot on the side TOWARD which
the switch is positioned to achieve “zero” or
“atmos” reading.
5, Place switch in alternate position and adjust
the other pot for “atmos” or “zero” reading.
6. Repeat steps 4 and 5 for fine adjustment.
7. If last adjustment was for “atmos” reading,
unit is ready to use. If adjustment was for
“zero” reading, place switch #1 in alternate
position to obtain “atmos” reading. Unit is
now ready to use.
NOTE: Switch must be in “atmos” adjustment
position for normal operation.
Vacuum System Trouble Shooting
PROBLEM
1. No Vacuum
. Very poorvacuum (pressure of
200 microns .2 Torr or higher)
CAUSE
a. Pump not on
b. Pump not connected to vacuum
system
с. Water vapor condenser drain
open
d. Break or opening in vacuum
lines
e. Vacuum valve open
a. Vacuum pump oil leve! low
b. Excessive moistureinvacuum
pump oil
c. Vacuum leaks in line
Vacuum leaks in condenser
and drying chamber gaskets
10
CORRECTIVE ACTION
a. Turn on pump
b. Connect vacuum connection
to pump outiet.
c. Install plug in open end of
drain line
d. Locate and correct
e. Close all valves (“vent” up
position)
a. Add vacuum pump oil to proper
level
b. Replace pump oil
с; Locate andrepairieaks. Apply
siticone vacuum grease to
connections and secure with
hose clamps.
d. Locate andrepairieaks. Apply
silicone vacuum grease to
gaskets.
Refrigeration System Touble Shooting
PROBLEM
1. Refrigeration system does not
start.
2. Refrigeration system starts
but shuts off,
3, Shelf temperature too high.
CAUSE
a. Unit not plugged in.
bh. Fuse blown,
c. Defective off/on switch.
d. Defective internal wiring.
a. Low voltage to unit.
b. Defective voltage to unit.
с. Excessive suction.
System low in refrigerant.
po
bh. Excessive load.
c. Restrictions in cooling air.
d. Excessive ambient
temperature.
41
CORRECTIVE ACTION
a.
Plug into 115 V, 60 Hz,
20 amp service, or 220 V,
50 Hz, 15 amp service,
depending on specific model.
Replace defective fuse.
Replace switch.
Locate and replace
defective wire.
Determine reason and correct.
Replace protector.
Determine reason and correct.
Locate and repair leak,
evacuate, recharge.
Reduce load.
Locate and remove
obstruction, clean
refrigerant condenser.
Reduce ambient temperature.
With valve in VAC position, freeze dry containers
are directly connected to the vacuum S
ysiem.
12
Turn to VENT position and
disconnected from the vacuum system and
automatically connected to the vent port which
your container IS
gently bleeds air to release the vacuum in the
container. The vent port may also be used in
conjunction with glass or poiypropyiene drying
tubes to introduce sterile air or dry nitrogen.
LO-070SZ T3A0N
070SZ TICIÓON
NYHOVIO S1HYd di139V1 67)
UY IIS
Y OLLYW:HOS
OIFEENEES
E
"OANI did
"OVA 438
13
'pajou a1suym ¡deoxe “OVOSZ SPO 10} UMOUS SE
gwes 34) ele |0-0Y0SZ [9POW JO] sed jusuoduroo [Y LON
1496) 101091044 a1!M-BuiUSNE v9 oval Suly O. 25
6589. [SUB [8011199/3-19A07 £9 SEL 1aqqnu-egni LE
59161 agn| ueid-diio 29 69961 dwejo eso 05
£869. Guijdno9 sant L9 OLLGZ ajeld Joydepy 62
9269. Jaquiey) wnnoeA 09 8589. Buin! WINNOBA 87
LZ124 A¡quiessy 1ejeeH 65 2549! бы „О, Le
8189. pnosus es 9E-+6061 INN 9e
AA jeueg U810 LS peal Jaqggny-sqn1 Se
69271 1099UL107 98 LLIZZ soi #2
£6.21 Qclel 34617 Old GS evel 18qgny-sgnL EC
8269. pnoiyg-jaued ле PS PPTL -- mess 1BQANY-OQN L 20
oveel WNNDEA-YONMS eS LO-EOLZZ A8A07 |8UVEUD Le
6625! UORBISÔULOY-YOUMS 2s 10-201 LL ¡9UUBYO IM 02
50-90144 10-90104 ejejd LONINSUl LS vegr dusejo esoH 61
PELLL iojeiodeal 0S ¿OLLZ jeNno-19de7 8!
EFBOL 4000] 6$ 2182 + LIBEL ejoedaosy ZW
17892 e|pueH 97 9.961 dwe|Q asoH ol
£9.61 1SED J00Q-SA1SSUpYy Ly 21481 эрчиен Si
EVOL jexser 1000 af 96941 Gori 1055944000) pl
GE89L GqOUM 5$ L90ZL 85021 10)0WN ued el
89661 UOJAN-JOUSEM vr BEVEL 1OJOW UBJ-1049219 el
КОДА Buo-189eds sql op 0ESY 1 8cstL epelg ued LL
25661 Bunds A £689. aseg-%oelL Ot
9L-0L 161 ¡eJO/N-1GUSEM Ly $589. 9US-49B4L 6
gyizz dwe|d 100 ov 989. H9US 8
LO-LOLZZ HOoUS-189eds agn 6€ Ok£pl 1109 10SUSPUOY L
12-6906 INN 85 0989. SINE OL 9
6269. doy, LE £eerl бла Lules 5
6086! sbneo ainjeiadwa |, 95 rLr6L 191520 $
c189/ sônes UNNDEA GE LPZOZ aqn L ule 5
СОДА дело 1094309 ve chil [SUB 1U0JA с
2512. ÁAjquessy 101981)20 ce £ch£l эшеа ен) |
"ON LYHYd ‘ON LHvd "ON LHYd "ON LHvd
10-09054 | 09054 "ON T3GOW NOildidosaa — L0-0v0SZ | OvOSZ "ON T30OW NOLidiHOS3C qu
H3LI7 8 LO-OtOSZ ON LYVd
Ot0SZ ON LäVd
SiIYUVd LN3W3OVid3Yd
YALIT 8
14
THERMOCOUPLE RED
WHITE
TEMPARTURE
GAUGE
DEFROST HEATER
FAN DEFROST
À, SWITCH
REFRIGERATION
SWITCH
LIGHT COMPRESSOR
VACUUM
GAUGE
—
+
£3
RECEPTACLE (À
VACUUM
PUMP
SWITCH
"CAUTION:
Equipment must be disconnected from
electrical source before servicing.
115V - 60 Hz - 1 Phase
(3 CONDUCTOR GROUNDED) Volts 115
NOTE: ANY REPLACEMENT Ref. A 9
WIRING MUST BE SAME SIZE el. Amps |
AND TYPE AS ORIGINAL. Max. Amps
Recept 9
M=MOTOR Total 18
Max. Amps
ELECTRICAL SCHEMATIC - FREEZE DRYER - 8
15
THERMOCOUPLE RED
WHITE |
TEMPARTURE
GAUGE
DEFROST HEATER
TRANSFORMER
DEF LANNY DEF
RECEPTACLE CODI Y ACUUM
GAUGE
WGB
220 VOLTS 50 HZ
NOTE: ANY REPLACEMENT Volts 220
WIRING MUST BE SAME SIZE |
AND TYPE AS ORIGINAL. Ref. Amps 45
Max. Amps
CAUTION: Recept 9
Equipment must be disconnected from Total )
electrical source before servicing. Max. Amps 13.5
ELECTRICAL SCHEMATIC - FREEZE DRYER - 8 - 220 У /50 HZ
16
— EVAPORATOR
CAPILLARY
TUBE
COMPRESSOR
/
—
DRIER |
AT
ACCUMULATOR
WITH CAP TUBE
PROCESS
OIL DRAIN
4 TUBE
FAN \L |
Y | NOE /
| y
« | CONDENSER
{
REFRIGERATION SCHEMATIC — FREEZE DRYER - 8
FOR REFRIGERATION SYSTEM CHARGING INSTRUCTIONS, SEE LABEL ON CABINET BACK
17
Freeze Dryer 8 (Model 75040)
(Model 75040-01)
Cabinet: 30-34" wide, 28” deep, 36%" high
27" DIA. VAC. PORT. Casters: (Four) 3” diameter, hard rubber
Work Surface: Chemical resistant with 27" dia.
| vacuum connection in the top for
connection of drying chambers or
accessories,
16.82"
(427.9mm) Cabinet Panels: Front and side panels are epoxy
coated steel. The front panel
O | also features an expanded
NA metal grili for cooling air.
À ]
NY
Condenser: Capacity, up to 8 liters of ice before”
| defrosting. Condensing coil itself,
fabricated out of stainiess steel.
Instrument
и Controls: Condenser temperature continuously
TOP VIEW 11.18" * indicated on thermocouple gauge in
(284.42mm both degrees F and degrees C.
Electronic vacuum gauge monitors on
a range from 5 microns to 5mm (TOR).
Electrical el 75040
Requirements 115 volt, single phase, 20 amp.,
60 Hz.
ode! 75040-01
220 volt, single phase, 15 amp.,
50 Hz.
- 30.75" > LL — 28.00"
(781.mm) (711.2mm) |
11.18"
— (ватт
{OF VAC PORT)
36.12"
(917.45mm)
Y Y
FRONT VIEW SIDE VIEW
18
INSTRUCTION SHEET
LABCONCO FREEZE DRY FLASK
CAUTION: Glassware is subject to breakage. Care should be
exercised during use. Avoid rough handling and shock.
Safety glasses should be worn when glassware 15 under
vacuum.
TOP «(№ grease required)
i
BOTTOM
Filter
ADAPTER \ FAST FREEZE
| Washer |
Light Grease
LIGHT |
GREASE TOP
ADAPTER
UJ
LIGHT
ADAPTER Y GREASE
BOTTOM
STANDARD FLASK
«No Grease Required
M BOTTOM
| | LYPH-LOK
TOP | | |
LYPH-LOK SEAL
Either Shell Freeze or angle the flask as shown to avoid breakage due to expansion
of liquid. Do not freeze in vertical position.
LABIONIG CORPORATION
THSTRUCTION SHEET S311 Prospect
TT “ansas tity, Mo, 64132
816-333-8811
LABCONCO VALVES 1/2" AND 3/4"
LABCONCO valves are new and different. Their unique snar-fit design
places the valves all the way into the drying chamber through pre-
cision-cut manifold openings for a direct compression seal. So
leaks due to defective welds or corrosion are eliminated. Just snap
it in for a leak-proof high vacuum seal, You can even rotate the valve
a full 3609 during operation with no loss of vacuum.
A vent port provides a convenient connection for glass or polypro-
ylene drying tubes, so you can release the vacuum with dry sterile
air or dry nitrogen. For combination bulk and manifold drying chambers,
one or more valves may be removed to provide access ports for electronic
product temperature indicators, controllers, or recorders.
LABCONCO valves accommodate flasks, ampules and serum bottles. The
LABCONCO Adapter #75934 increases the capacity of the 1/2" valves
by reducing the inlet diameter of the valve to accommodate the com-
plete line of ampules.
(1/8") 3 MM (1/4") 6 MM
To install the valve, coat the stem lightly with vacuum grease.
in addition, coat the end of the valve body and the port hole into
which the valve will fit. Insert the valve body with a twisting
rotating movement until it is seated in the groove as shown. Next
install the lubricated stem into the valve body with a rotating
motion until it is seated as shown. The valve is now ready for
use. To remove valve reverse installation procedure,
ECO 4844 . (1) INSTRUCTION SHEET P/N 76580 - А
Apply silicone grease all
around full length of stem.
Apply silicone
grease all around
as indicated.
Valve Stem
Turn to "vent" position and your con- With valve in "vac" position,
tainer is disconnected from the vacuum freeze dry containers are directly
system and automatically connected to connected to the vacuum system.
the vent port which gently bleeds air’
to release the vacuum in the container.
The vent port may also be used in con-
junction with glass or polyprooylene
drying tubes to introduce sterile air
or dry nitrogen. -
PARTS LIST |
Valve | Complete Polypropylene Buna-N
Size Valve Stem Only Body Only
1/2" 75900 76000 76001
3/4" 75910 76002 76903
(2) Instruction Sheet P/N 76580 - A
LABCONCO CORPORATION
INSTRUCTION SIEET 8811 Prospect
Kansas City, Mo. 64132
816-333-8811
LABCONCO DRYING CHAMBERS & HEAT RACKS
Part Number Ports
75100 16 Chamber
75102 12 Chamber
75104 18 Chamber
75106 39 Chamber
75210 Bulk Chamber
75130 | 10" Diameter Heat Rack
75132 6" Diameter Heat Rack
The LABCONCO drying chambers are used to facilitate visibility
during lyophyilization even when bulk drying. The chambers are
fabricated of 304 stainless steel and have a clear acrylic top.
The ported chambers come complete with the unique LABCONCO valve
that provides a leak-proof vacuum seal. The 75132 heat rack may
be used with all of the drying chambers while the 75130 heat
rack is primarily for the 75210 bulk chamber and the 75104 and
75106 chambers. The heat racks come with a built-in high limit
thermostat (110°F), a 24 volt power transformer and a power feed
through cord. The 75210 chamber includes the 75130 rack and
transformer. The three-shelf product heaters are black anodized
for more efficient heat transfer.
The LABCONCO valves used in the drying chambers are of a unique
snap-fit design that places the valve into the drying chamber
through a precision-cut manifold opening which compresses the
valve body for a seal. The valve may be rotated 360° during
operation with no loss of vacuum,
A vent port provides a convenient connection for glass or
polypropylene drying tubes to backfill with dry sterile air
or nitrogen.
7 he
; f
ECO 4822 INSTRUCTION SHEET P/N 76583 D
Sht. 1 of 2
~~ LABCONCO DRYING CHAMBERS & HEAT RACKS
VE PARTS LIST
EN FOR POT ASSY, ONLY
fassemeur] 0168671] ®
NO. a POT BOTTOM TOP PLEX.
Le 16 GASKET | GASKET| TOP
[78100 |16 PoR 76054! 76908] 76898
75102 [12 PORT| 76139] 76885 76 884
|.75104 |18 PORT 76054 | 76908 76898
75106 [39 PORT [76961 | 76508 76907
75210 | BULK |76139 | 76885 76885
PARTS LIST
FOR HEAT RACK ASSY ONLY
| |
ASSEMBLY] HEAT WD ат © >
о NO, RACK CLIPS XFMR CORD, 2 4v
75130 10" | 19 15 в | 76554 76542
| 75132 6" 19158 | 76554 76542
PARTS LIST
FOR VALVE ASSY ONLY
ASSEMBLY VALVE STEM BODY
NO. ONLY ONLY
75900 | 1/2" | 76000 | 76001
75910 3/4" | 76002 | 76003
-PLUG INTO
INSERT IN
1/2 VALVE PORT.
— FOR FEED THRU
PLUG INTO P32
VENT OR MAIN PORT
BACKFILL PORT
FOR 3 LITER UNITS USE GASKET ON EXISTING LID ON PART NO. 77076.
P/N 76583 Sht. 2 of 2 | | | ____ ECO 4822
Was this manual useful for you? yes no
Thank you for your participation!

* Your assessment is very important for improving the work of artificial intelligence, which forms the content of this project

Download PDF

advertisement