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Edwards EF4 Modulyo Freeze Dryer Instructions ENG PDF
Edwards EF4 Modulyo Freeze Dryer Instructions ENG PDF
Instructions
1C-F029-19-380
•February 1.979
pS c,
Page number
General description . .< 2
Specification 3
Installation 3
Freeze drying - the basic principles 4
Temperature/vapour pressure - its effect on drying times 5
Operation - general 6
Shelf and stoppering accessory 7
Drum manifold accessory 9
In-line manifold accessory 11
Bell jar accessary . 13
Pipeline attachment accessary • " 14.
Specimen dryer accessary 15
Heated tray accessory 17
Centrifuge accessary 18
Secondary drying accessary 19
Maintenance • 20
Circuit diagram 21
Ordering details 22
Supplementary instructions 23
Accessory instructions (additional) 23
Communications with Edwards • 24
- 1 - 1Q-F029-19-830
General description
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EF4 Modulyo
When used with any of the accessaries offered the flodulyo can be used for
freeze drying material in bulk, round bottomed flasks or vials. Alternatively,
the unit can be used as a convenient, low temperature vapour trap that may
be attached to an existing evaporative facility.
The condenser chamber and its associated pipework are manufactured from
stainless steel to minimise corrosion. The thermally insulated chamber
acts as a trap for water or other solvent vapour and as a container for
the resulting ice or condensate. A large flange opening enables easy
inspection, cleaning and water defrosting.
10-FQ29-19-880 - 2 -
A valued drain terminating on the front of the Modulyo is provided for
simple and quick removal of water and condensate.
Specification
Overall dimensions
height 332 mm
width 535 mm
depth 622 mm
Weight 45 kg
Refrigerator Prestcold
CondBnser
ice capacity in 12h ... 1.2 kg
ice capacity in 24h ... 2.3 kg
ica capacity in total •* • 4.0 kg
minimum temperature
under vacuum •• • -60°C
surface area •• * 0.15m2
volume •• • 7.2 litres
average evaporation
rate (manifold) •• * 95 cc/haur
Installation
The unit is designed to fit a 'standard' laboratory bench or it can ba
trolley mounted where bench space is at a premium.
- 3 - 10-F029-19-880
Mote; A condenser extension tube.is supplied. This should be fitted to
the vacuum pumping line' within the chamber when either the shelf and
•stoppering attachment, the heated tray accessory, the centrifuge accessory,
or the bell jar accessory is used. By extending the pumping line further
down the chamber an improvement in the distribution of ice will result.
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10-F029-19-880 - 4 -
Apparatus for freeze drying consists essentially of a vacuum vessel, a water
trap and a mechanical vacuum pump. The water vapour which evolves in the
process is trapped before entering the pump, which cannot deal with the
large volumes of vapour generated in the process. Methods in common use
for trapping water are desiccants (drying agents), or refrigerated
condensers as in the Modulyo. Containers of the prefrozen material are
either attached externally to a vacuum manifold or placed in a chamber
or cabinet which is then evacuated.
The amount of heat being received by the product will determine the product
temperature and vapour pressure. This in turn determines the pressure
differential between the product and the condenser or vapour trap, thus
establishing a driving force between one and the other.
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Temperature °C
Vapour pressure above ics
^ 3 *™ 10-F029-19-880
If, for example, the product temperature stabilises at -3G°C, the vapour
pressure at this temperature will bs 3.7 x 10~"l mbar (see graph). If
however, the product temperature is increased to 10°C the vapour pressure
of the product will be 2.6 mbar, an obvious increase in the driving force
between the product and the condenser tsmperature of -60°C (equivalent
to a vapour pressure 1.1 x 10~2 mbar).
Note:. Pressures given above are typical and apply to aqueous solutions.
Operation —General
.2) Open the drain valve by turning the control knob anti-clockwise.
Drain completely.
12) Open the drain valve and allow the condenser to defrost naturally or,
15) Pour warm water (50°C maximum) into the condenser chamber. Do not
fill above the level of the pumping line.
10-F029-19-880 -6 -
Shelf and stoppering accessory
Stoppering
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Top Plate
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^ Shelf
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Shelf
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— 7 — 10-F029-19-880
Technical specification
10) Switch on the rotary pump and open the gas ballast valve.
11) The drying process will now begin and the material in ths vials will
remain frozen by evaporative cooling.
13) . Stopper the vials by turning the shelf handles in a clockwise direction,
10-F029-19-880 - 8 -
Drum manifold accessory
The accessory is ideal for freeze drying bulk materials such as aqueous
solutions and slurries. It is usual to shell freeze such materials before
processing by means of a freezing bath or refrigerated cabinet.
Thermovac valve
- 9 - 10-F029-1Q-880
The handle of the value incorporates a pointer and in operation it is
used as follows:
12 o'clock position
Handle
Vent hols
3 o'clock
position
Venting slot
Pointer
Shell freezing
Operation
10-F029-19-880 - 10 -
In-line manifold
- 11 - 10-F029-19-880
Glass isolation valves
•—^———~—————————______ 'tO,!-^i
Each valve is connected to a manifold port by means of a
short piece of vacuum hose. Flasks are connected by, push-
fitting onto a ground taper. The aperture can be seen
through the glass body and should be positioned as .follows;
;
Operation .
1) Mount the manifold accessory in the Modulyo condenser chamber
and secure it with the three screws supplied,
5) When the condenser reaches -45°C switch on the rotary vacuum pump
and open the gas ballast valve.
6) Attach a prepared flask to the cone connexion of a glass valve.
7) Open the glass valve to start the drying process.
8) Allow the pump time to stabilize the pressure in the chamber before
connecting each subsequent flask.
9) Remove flasks as required by closing the valve and turning the
handle to the venting position.
1Q-FQ29-19-880 - 12 -
Bell jar accessory
A cylindrical acrylic bell jar designed to sit over the chamber of the
Modulyo in an I section gasket. An elevated baseplate is supplied with
the basic unit, to support material for processing away from the
refrigerated environment of the chamber. Materials to be processed
myst be pre-frozen before loading into the bell jar. In the case of
spherical flasks pre-freeze as described in the shell freezing section.
In the case of beaksrs, a maximum fill of between 12-15 mm should be
pre-frozen in the beaker.
Operation
4.) Whan the condenser temperature reaches -45°C, load the material
into the bell jar.
5) Switch on the rotary pump and open the gas ballast valve.
7) At the and of the process, switch off the pump, the refrigerator
and the electricity supply.
10) Pour warm water (50°C Max) into the chamber to assist defrosting.
Open the drain valve. Drain completely and wipe dry.
- 13 - 10-FQ29-19-880
Pipeline attachment accessory
This accessory which fits directly onto the flange of the condenser, is
designed for the removal of vapours from other processes. Manufactured
from stainless steel,to,minimise corrosion, it accepts.a rubber or :
plastics tube of between .20-25 mm id, or alternatively, an Edwards .
coupling system. • , .. . ,. .
Operation
6) When the condenser coil reaches -45°C Switch on the rotary pump
and open the gas ballast valve.
7) At the end of the process, switch off the pump, the refrigerator
and the electricity supply.
10) Pour warm water (50°C max.) into the chamber to assist in defrosting
the condenser.
10-FQ29-19-880 - 14--
Specimen dryer accessory
The accessory comprises a cylindrical stainless steel container 123 mm
dia x 280 dsep, an acrylic cover plate and a tripod support. It is
designed to be positioned within the condenser of the Plodulyo unit, at
a selected height, for initial freezing or subsequent drying of specimens,
such as small mammals, insects and vegetable materials etc.
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Operation
2) Load the specimen into the accessory and mount the specimen dryer
onto the condenser chamber of the flodulyo (See position 1)
3) Close the condensate drain value on the Modulyo and also the air
admittance valve.
- 15 - 10-F029-19-880
7) When the freezing state is complete, start the vacuum pump, and
open the gas ballast value. Water vapour given off from the specimen
will be removed through the gauze base of the accessory and.trapped
on the inside surface of the Modulyo condenser.
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Position 1 Position 2
Freezing of small mammals may take as long as three or four days and it
is recommended that after tuio days the specimen be removed and test
weighed. Open the air admittance valve and allow the vessel to achieve
atmospheric pressure in order to remove the specimen.
This process can then be repeated daily until no further weight loss is
observed.
For the final stages of drying the specimen accessory may be moved to the
raised position (Position 2 ) . This will raise the temperature of the
specimen, thereby preventing the risk of condensate forming on the surface
of the specimen when it is finally removed from the freeze dryer. Release
the vacuum by opening the air admittance valve before attempting to raise
the container.
10-F029-19-880 - 16 -
Heated tray accessory
Designed to permit the addition of heat into the vacuum system during a
freeze drying process which enables more rapid drying of liquids or
semi-solids. Each tray is fitted with a thermostatically controlled
65 watt heater at 50 volts. -Three 30mm deep trays are supplied, each
of 150 ml capacity, giving a total capacity of 450 ml. The thermostats
fitted to the shelves are preset at +40°C. Product temperatures can
be controlled by adjustment of the energy regulator on the control box.
Supply voltage required is 220/240V 50Hz 1 phase fused externally at
3 amps.
Operation
1) Load the material to be dried into the trays and insert.the thermocouple
into the material.
2) Pre—freeze the tray assembly and contents in a freezing bath or cabinet.
3) Fit the base of the accessary, with the gasket, to the basplate.
4) Switch on the electricity supply to the freeze dryer.
5) Close the condenser drain valve.
S) Switch on the refrigerator.
7) When the condenser temperature reaches -45°C.
8) Transfer the pre-frozen assembly to the accessory base on the freaze
dryer.
9) Switch on the rotary pump.
10) Connect the three heater plugs into the sockets of the trays.
11) Locate the acrylic cylinder in position over the tray assembly.
12) Check that the air admittance valve is closed.
13) When the temperature has stabilised (usually after about 30 minutes),
switch on the tray heaters,
14) Adjust the energy regulator to give the required product temperature.
15) Continue drying until the process is completed - this is usually when
the pressure is at or'below 1.3 x 10""'' mbar.
15) Turn off the shelf heaters.
17) Switch off the rotary pump.
18) Switch off the refrigerator.
19)' Slowly open the air admittance valve.
20) Unload the product.
- 17 - 10-F029-19-6S0
Centrifuge accessory
To prevent frothing and possible breakages when evaporative freezing
wet substances contained in ampoules. After freezing under centrifuge
action the material may be dried without further handling.
The accessory comprises a bell jar, upon which is mounted a 1/8 hp drive
motor, and a mounting assembly with three sizes of ampoule carriers.
Freeze drying ampoules are available from Edwards High Vacuum.
Data
Clamping Knob
Top Plate
'(Single
Register
Hols)
Spacer and Pin
Ampoule
Centre Plate Holder
(Two
Assembly
Register
Holes)
Spacer and Pin
Base Flange
Operation
1) Ensure that all valves are closed and all switches are in the off
position.
4) Mount the ampoule carrier over the condenser chamber of the Modulyo
and onto the bearing plate, which must be screwed to the condenser
top flange.
1Q-F029-19-880 - 18 -
5) Place the bell jar and csntrifuge motor assembly over the ampoule
carrier. Carefully locate the drive shaft into the carrier.
6) Switch on the mains electricity supply to the Modulyo.
7) Open the gas ballast valve on the vacuum pump and then switch on
the pump.
8) Switch on the refrigerator.
9) Allow the condenser to reach a temperature of -45°C.
10) Switch on the centrifuge motor.
11) After approximately 5 to 10 minutes (or when the Pirani gauge shows
a pressure of approximately 6.7 mbar) the material contained in the
ampoules will be frozen. Switch off the centrifuge motor as continuous
centrifuging is generally not required.
12) Continue freeze drying until a pressure of 1.3 x 10~ 1 mbar or below
is achieved, at which stage primary drying can be regarded as complete.
13) Switch off the vacuum pump.
14.) Open the air admittance valve and remove the accessory.
15) If secondary drying is required fit secondary drying header accessory.
- 19 - 1Q-F029-19-8S0
Operation
1) Switch off the rotary pump and refrigerator.
7) Switch on the rotary vacuum pump and close the gas ballast valve.
13) Test the vacuum in each ampoule with an.Edwards S T ^ spark tester to
check for air leaks.
Maintenance
1) Always wipe clean the chamber seal ring before attaching an accessory.
4) Wipe the exposed surfaces and the chamber mating flange free from
dust and spillage. To enhance the appearance of the stainless steel
top cover, it may be treated with wax polish applied by means of a
domestic aerosol spray. For difficult finger marks, etc., clean
with a bleach solution.
10-F029-19-830 - 20 -
5) If a fuse ruptures it should be replaced only by a fuse of the same
type and rating (5 amp). Do not change a fuss more than once for
the same fault. If a fuse ruptures immediately after replacement,
check the unit for electrical faults.
6) A suspected leak in the vacuum system may be found by checking with
a detector around obvious connexion points; check that the suspected
leak is in the flodulyo unit by removing any accessory and blanking-
off the chamber aperture whilst testing.
Circuit: diagram
Refrigerator
motor
6 0 0
Pirani gauge
Thermocouple
- 21 - 10-F029-19-88Q
Ordering details
Code number
10-F029-19-880 - 22 -
Supplementary instructions
Spesdivalve 1*108784
Air admittance valve AU5 •• •
["108789
•Pirani vacuum gauge •* •• * 1*107865
Pirani gauge heads 07-D024-21-880
Accessory instructions
Please specify.: •
Damage in transit.
- 23 - 10-F029-19-38Q