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Edwards U

Instructions
1C-F029-19-380
•February 1.979

pS c,

EF4 MDDULYO FREEZE DRYER

Code ia-FO29-19-OGa . 22O/24OV


1D-Fa29-2D-OOQ 11QV

Edwards High Vacuum


Part of BOC Limited
Manor Royal . Crawley . West Sussex . RH10 2LW . England
Tel: Crawley 28844 (Std Code 0293) . Telex: 8712,3 Edhivac Crawley

) Printed in England P149


Contents

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

Cover f i x i n g screw-^^^s>

^X^JN^^^ Refrigerator condensar

iff
y^ ,

V J \ \ ^ \ ^ ^ Refrigerant liquid receiver

Condenser
chamber

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valve phial I
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1I Pirani

J-y head
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1 y^ ^4 ^ 1 Cover
fixing
U screw

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Block ^*V. > / HI Mains
! indicator
lamp
Expansion valve ^Sy
-Temperature
indicator

.Refrigerator
on/off switch

Alr a
\ X ^ r ^ i ^- ^ ^ «"anc.i
Pirani vacuum gauge ^ \ -^^'Cy^-^^ Vacuum pumping Una
'«®5L^ Orain velva control
v^ Orein line nozzle
EF4 Modulyo

The Piodulyo is a freeze drying/vapour trap facility having an ice trapping


capacity of four-litres. It is capable of being bench or trolley mounted
as required.

Designed as a basic unit it is primarily intended for freeze drying


biological and pharmaceutical preparations, but is equally suitable for
use on other vacuum duties including evaporation and distillation.

The concept of Modulyo is to provide the minimum equipment nscsssary for


these duties, and the basic unit consists of a functional cabinet in which
is contained an air cooled refrigerator compressor and a stainless steel
condenser chamber.

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.

A Pirani vacuum gauge is fitted and also a thermocouple meter to indicate


the temperature of the condenser during operation. On the front of the
unit are also fitted a refrigerator fon-off switch and an indicating lamp.

Specification
Overall dimensions

height 332 mm
width 535 mm
depth 622 mm

Weight 45 kg

Electrical requirements 220-24QU 50 Hz, 1 phase


60 Hz version, also available
ft.
Power consumption 3Q0W (fuse ^ amp)

Refrigerator Prestcold

size V 3 hp (250U) hermetrically sealed


180 k/cal/h at -35°C
heat extraction rate (at 20°G ambien-t)
R502
refrigerant

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.

A two-metre length of electricity supply mains input cable is fitted to


which must be attach'ed a fused (5 amp) plug; alternatively it should be
wired into a fused, switched terminal box.

On the front left-hand of the unit is located a drain line nozzle. To


this point may be attached a suitable length of tubing running either to
a convenient drain or to a collecting receptacle.

The condenser chamber is connected to a vacuum pipeline which terminates


in a 15 mm o.d. tube located-on the front of the unit (see illustration).
To this point should be connected a suitable two-stage oil sealed rotary
vacuum pump (1O~2 to 3 x 10~2 rnbar minimum, 50 1 min~1. If such a pump
is not part of the laboratory equipment, the Edwards EDM6 or ED50 is
particularly suited for use with the Modulyo. A vacuum pump may be
simply connected by using a pump adaptor kit (08-F029-41-000).

- 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.

Clodulyo pumping line

Coupling nut Q8-C1ia-ai~331>

Campc933ian 3iseua 08-C110—32-021,

0-ring

0-cing 08-4021-20-036

Compression 3laav/9 G8~C11C—02—321

Coupling nut 08-C110—02-321

TuBa a8-r"Q2S-41-301

' Vacuum h
oa-Hozi-oo-oos

EF4 Modulyo pump adaptor kit


Q8-F029-4.1-000

Freeze drying-the basic principles


Freeze drying is a means of preserving wet substances, or solutions in
water, that are usually of biological origin. Substances treated are
living micro-organisms for preventive or curative medicine or for 'banking'
in culture collections, starters for fermentation processes, blood fractions,
biological standards, hormones, enzymes, antibiotics, vitamins and unstable
fine chemicals and pieces of tissue.

After pre-freezing, the frozen product is exposed to vacuum and the


contained ice allowed to sublime - that is, to change directly from the
solid to the vapour state without melting. During freeze drying the ice
does not evaporate simultaneously from all parts of the material, but a
frozen interface continuously moves away from a dry outer boundary. The
resulting 'cake1 has substantially the same size and shape as the original
'frozen mass and it may usually be stored at room temperature until required
for use. When reconstitution is necessary this can be done by the addition
of a suitable quantity of water, when the properties which survived the
initial freezing are restored.

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.

Vacuum creates conditions favourable to freeze drying and sublimation only


occurs if heat is supplied to the frozen material. Room heat is usually
sufficient for manifold or small chamber freeze dryers.

Temperature/ vapour pressure -


its effect on drying times
Evolution of water vapour from the frozen product will cause the temperature
to fall to a point where heat lost due to sublimation is balanced by heat
gained from the surroundings or from applied heat.

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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0 -10 -20 -30 -40 -50 -60 -70
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).

Far most efficient drying it is therefore essential that the product


temperature is kept as high as possible without melting. In the Flodulyo
sufficient heat is normally derived from the surroundings.

Note:. Pressures given above are typical and apply to aqueous solutions.

Operation —General

I) Switch on the mains power supply to the unit. An indicator lamp on


the extreme right-hand s'ide of the front panel will light.

.2) Open the drain valve by turning the control knob anti-clockwise.
Drain completely.

3) Close the drain valve by turning the knob in a clockwise direction.

4) Switch on the refrigerator by pressing the indicator button on the


temperature indicator meter.

5) Attach accessory to the chamber.

6) Close the air admittance valve.

7) Switch on the vacuum pump.

• Note: it is generally necessary to use full gas ballast on the


vacuum pump for a freeze drying process.

8) When the process is finished, switch off the-vacuum pump.

9) Slowly open the air admittance valve.

10) Remove the product.

II) Switch off the refrigerator.

12) Open the drain valve and allow the condenser to defrost naturally or,

13) Assist defrosting as fallows:

14) Remove the accessory from over the condenser chamber.

15) Pour warm water (50°C maximum) into the condenser chamber. Do not
fill above the level of the pumping line.

16) Allow a few minutes for the ice to thaw.

17) Open the drain valve.

10-F029-19-880 -6 -
Shelf and stoppering accessory

Stoppering

/iTfL—-
/iLJn
—. Mechanism

Top Plate
s
<s*— 1 u—' —1 W
^ Shelf

—--SB-e-jB-es; ^^>

— " j U l /

,[] Shelf
•L• Gaskst

\^— ~^Z-^'\\
Shelf

' '—T
• Cylinder

Ofi ' L ' Gasket

p-

This accessory allou/s freeze drying of materials in vials of maximum


height of 52mm (including partially closed stopper). When dried,
the vials can be stoppered in situ without breaking the vacuum.
Additional spacers are included however, so that the accessory can
be adapted to-accept vials up to 73mm high on a two shelf assembly.

Vials for processing (with stoppers partially closed) are placed


on to the three trays provided and transferred to a freezing bath
or deep freeze. After freezing, the loaded shelf assembly is fitted
inside the acrylic cylinder (which is located over the chamber of
the Plodulyo) and the drying process is started.

Stoppering is carried out in situ under vacuum by turning the


stoppering handle clockwise.

— 7 — 10-F029-19-880
Technical specification

Number of shelves • ,2 or 3 " .


Height between shelves 53mm (open) 37mm (closed) (3 shelf version)
73mm (open) 57mm (-closed) (2 shelf uersion)

Maximum number of vials per shelf per assembly per assembly


2 shelf 3 shelf
14mm od 123 246 369
16mm od " 89 178 267
18mm od 71 142 213
24mm od 39 78 117
Operation

1) Fit the acrylic cylinder on to the baseplate flange of the Wodulyo,


together with the two L section gaskets.

2) Load into suitable vials the material to bs dried. Partially stopper


each vial and stack in the accessary trays. .

3) Assemble the trays in the accessory and transfer the batch to a


freezing cabinet. .

4) Prefreeze the entire assembly of accessory and vials to the desired


temperature in the freezing cabinet. Store the batch in the cabinet
until required for the drying process. .

5) Check that the Modulyo unit is completely drained by opening the


drain valve. Close the valve when satisfied that the condenser is
empty.
6.) Switch on the electricity supply to the Modulya.

7) Switch on the refrigerator.

8) When the condenser coil temperature reaches -45°C.

9) Transfer the pre-frozen assembly to the acrylic chamber on the Modulyo.

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.

12) Continue drying until the process is complete.

13) . Stopper the vials by turning the shelf handles in a clockwise direction,

14) Switch off the rotary pump.

15) Open air admittance valve.

16) When the chamber is at atmospheric pressure, remove the assembly


from the acrylic cylinder.

17) Switch off the refrigerator.

18) Open the drain valve.

10-F029-19-880 - 8 -
Drum manifold accessory

The drum manifold consists of a stainless steel chamber terminating eight


radial outlet ports to which ars fitted rubber waives. The values can
be fitted with B24 male cone connecting pieces for simple attachmenet
of spherical flasks of up to 1 litre capacity. Note: an extension tube
is supplied with this accessory but it is not required when the manifold
is used on a Modulyo unit.

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.

WARNING As a protection against the effects of a flask imploding under


vacuum, it is recommended that each flask be wrapped in domestic cling
•film before use.

Thermovac valve

A non—restricted vacuum valve manufactured from neoprene rubber and fitted


with a plunger for opening or closing. This valve allow rapid connexion
or disconnexion of flasks, etc. without disturbing the system. Each valve
has its own venting port which allows regulated breaking of vacuum in a
vessel connected to it.

- 9 - 10-F029-1Q-880
The handle of the value incorporates a pointer and in operation it is
used as follows:

Value open for drying - handle pulled out with pointer


at 3 o'clock
•Value closed - handle pushed in with pointer
at 3 o'clock
Value closed, in venting position for regulated breaking of
uacuum in a flask - handle pushed in and pointer at 12 o'clock

Note: on some values an aluminium plunger is fitted which has handles of •


unequal length. On these ualues the longer handle (fitted with a coloured
sleeue) should be regarded also as the pointer.

12 o'clock position
Handle

Vent hols

3 o'clock
position

Venting slot
Pointer

Shell freezing

(Refer also to instructions for Edwards cooling bath No. 10-F029-13-881)


Before starting the drying process a flask containing aqueous matter
should be prepared by freezing the contents as euenly as possible around
the inner surface. Rotating and rolling the flask in a refrigerated
cabinet or a freezing bath of solid carbon dioxide and methylated spirit
should achieve this; ideally the solution should be frozen to a uniform
thickness of approximately 8 mm or with a freeze drying fill of i of the
nominal capacity of the flask.

Operation

1) . Mount the drum manifold accessory in the Wodulyo condenser chamber


and secure it with the three screws supplied.
2) Close the drain ualue and the eight Thermovac valves.
3) Switch on the mains electricity supply.
4) Switch on the refrigerator.
5)1 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 connexion of a rubber valve.
7) Open the Thermouac valve to start the drying process.
8) Allow the pump time to stabilize the pressure in the chamber before
connecting each subsequent flask.

10-F029-19-880 - 10 -
In-line manifold

This accessory is an alternative design to the drum manifold, where


in-line working is more convenient to the user. Eight ports (arranged
four on either side) accept valves for flask connexion and enable freeze
drying of bulk materials, i.e., aqueous solutions and slurries.

The glass isolation valves incorporate a B24 connexion piece for


attaching glass flasks, and are for use specifically with the in-line
manifold accessary.

WARNING As a protection against the effects of a flask imploding under


vacuum, it is recommended that each flask be wrapped in domestic cling
film before use.

Shell freezing (refer also to instructions for Edwards cooling bath


No. 10-F029-13-881)

Before starting the drying process a flask containing aqueous matter


should be prepared by freezing the contents as evsnly as possible around
the inner surface. Rotating and rolling the flask in a refrigerated
cabinet or a freezing bath of solid carbon dioxide and methylated spirit
should achieve this; ideally the solution should be frozen to a uniform
thickness of approximately" 8 mm or with a freeze drying fill of 1/4 °f
the nominal capacity of the flask.

- 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;

a) to evacuate flasks turn the valve handle to place the


aperture towards the manifold. ,
b) to admit air to a flask, turn the valve handle to place
the aperture towards the venting port. ,... .
c) to seal off a flask from the vacuum system and atmosphere,
position aperture mid-way between the ports.-

;
Operation .
1) Mount the manifold accessory in the Modulyo condenser chamber
and secure it with the three screws supplied,

2) Close the drain valve and the eight glass valves.

3) Switch on the mains electricity supply.

4) Switch on the refrigerator.

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

1) Close the drain valve.

2) Switch on the electricity supply.

3-) Switch on the refrigerator.

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.

6) Close the air admittance valve.

7) At the and of the process, switch off the pump, the refrigerator
and the electricity supply.

8) Slowly open the air admittance valve.

9) Remove bell jar and treated material.

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

1) Place the accessory in position over the chamber of the Madulyo

unit and secure it with the three screws supplied.

2) Connect to the accessary a pipeline from the system to be evacuated.

3) Close the drain valve on the Modulyo.

4) Switch on the electricity supply.


5) Switch on the refrigerator.

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.

8) Open the drain valve.

9) Remove the accessory.

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

1) Pre-freeze the specimen, if possible, before placing in the container.

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.

4) Switch on the mains electricity supply to the Wodulyo. •

5) Switch on the refrigerator by pressing the indicator button on .the


temperature indicator meter.

6) If freezing of the specimen is to be carried out in the Modulyo,


the vacuum pump must NOT be started until the specimen is completely
frozen ( 2 - 3 hours).

- 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

Motor 240V 1ph 50Hz


Motor consumption 8 watts
Motor speed 780 r.p.m.
Fuse rating 3A
Number of ampoules per carrier 96 (0.5 ml)
24 (2.5 ml)
12 (5.0 ml)

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.

2) Charge the ampoules with the material to be dried.

3) Load the ampoule carrier with the prepared ampoules.

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.

Secondary drying accessory


The manifold supplied"has a total capacity of 48 ampoules. When the full
load of 96 ampoules of 0.5ml capacity is to be secondary dried it is
necessary to fit an additional secondary drying manifold (as shown) which
is available complete with the coupling as an optional extra..
Two GRP P2Q5 trays are supplied for containing the dBsiccant within the
condenser chamber of the flodulyo.

1 Ampoule carrier supplied with accessory


2 Coupling on top of chamber
Position of ampoule carrier already
supplied with unit

- 19 - 1Q-F029-19-8S0
Operation
1) Switch off the rotary pump and refrigerator.

2) Defrost the condenser by pouring in water at a temperature not


greater than 50°C. Leave the chamber immersed until all the ice
has malted. Open the drain value; wipe the condenser dry and then
close the drain valve.

3) While the condenser is being defrosted, fit the secondary drying


header to the coupling on the acrylic cover plate.
4) With an Edwards Ampoule Constrictor, constrict the ampoules as
described in the instruction HI 0759 and load onto the secondary
drying header; fill vacant positions with empty ampoules if necessary,
5) Carefully load desiccant into tha trays provided and_ place the tray
assembly inside the condenser.

Note: If it is not desirable to use a chemical desiccant to achieve


secondary drying omit step 5 ) . The refrigerated condenser is capable
of secondary drying but will take slightly longer than when a desiccant
is used.
6) Fit the secondary drying header over the condenser chamber and
secure with three screws.

7) Switch on the rotary vacuum pump and close the gas ballast valve.

8) Close the air admittance valve.

9) Continue pumping until the product is dried to'satisfaction.


10) Using a Flamemaster hand torch flame seal each ampoule, whilst
in situ on the header, at the point of constriction. This operation
will separate the ampoules from the header.

11) Switch off the vacuum pump.

12) Open the air admittance 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.

2) Check seal rings for cracking or perishing and replace if necessary.


Do not lubricate.

3) Clean the chamber regularly.

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.

7) Refer also to separate instructions for ancillary equipment.

Circuit: diagram

Refrigerator
motor

6 0 0
Pirani gauge

Thermocouple

- 21 - 10-F029-19-88Q
Ordering details

Code number

EF4 Wodulyo basic unit (220-240V, 50 or 60Hz, lph) 10-F029--19-000


EF4 Flodulyo basic unit (110V, 60Hz, lph) 10-F029--20-000
Spares kit 10-F029--19-800
Speedivalve Q8-C150--00-042
Diaphragm uasher for AV5 08-D118--01-003
Mains switch and lamp 10-F023--05-027
Thermocouple 10-F023--05-029
Expansion value 10-F023--10-010
Vacuum hose 08-H021- -00-005
Qowty seal -J- inch 08-H021- -04-002
0-ring 08-H021- -20-027
0-ring Q8-H021-,25-116
. 0-ring 08-H021- -25-205
Process accessories
Specimen dryer accessory 10-F029--10-000
Shelf and stoppering attachment 10-F023--01-110
Drum manifold accessory 10-F023-•03-060
Rubber value (specify quantity) 1Q-F023--03-058
B24 male connexion piece (specify quantity) 10-F023--03-059
Vapour trap/pipeline attachment 10-F023--05-021
In-line manifold accessory 10-F029--09-000
Glass isolation valve (specify quantity) 10-F029--09-016
Secondary drying accessory 10-F029-•42-000
Secondary drying header (order with above) 10-F023--27-000
Centrifuge accessory 10-F029--11-000
Heated tray accessory 10-F029-•12-000
Acrylic bell jar 10-F023-•01-046
'L' gasket for use with bell jar 10-F023-•01-018
Optional accessories
Trolley 10-F023-•05-020
Coupling kit for vacuum pump attachment 10-F029-•41-000
Cooling bath with one bottle spinner 10-F029-•13-000
Bottle spinner (additional) 10-F029-•13-001
Ampoule constrictor 26-F041-•01-000
Flamemaster hand torch 26-F098-•00-000
Spark tester ST4ivl 07-H020-•02-000
Oil mist filter 0F1F12 04-A131-•05-000
Leak detector LT10 17-0137-•15-000
Rotary vacuum pump
Edwards ED50 (220-2401/, 50Hz, lph) 03-A044-03-614
Edwards ED50 (110V, 60Hz, lph) Q3-A044-03-911
No.18 vacuum oil (l litre) 09-H110-05-015
Vacuum gauge
Pirani 10 vacuum gauge 07-D035-23-000
PIrani PR10S gauge head 07-0024-21-000

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

Edwards ED50 rotary vacuum pump 1*103894


Edwards cooling bath T0-F029-13-881
Edwards ampoula constrictor •... « t • 1*110759
Edward's spark tsster ST4C1 ... • • * 1*107855
Edwards oil mist filter 0P1F12... 1*104628
Edwards leak detector LT10 ... 17-D137-17-890

Communication with Edwards


Any communication relating to the subject of this instructions should bs
addressed to Edwards High Vacuum or to the supplier from whom it was
purchased.

Please specify.: •

1) The model, serial number and code etc.

2) The date of purchase.

3) Your order number and the suppliers sales reference.

Equipment should not be returned to the supplier without prior


arrangement.

Damage in transit.

If any damage has occurred in transit, it is important to inform both


the carrier and the supplier within three days of delivery.

- 23 - 10-F029-19-38Q

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