Edwards Ef4 Modulyo Freeze Dryer Instructions Eng.pdf 45122t

Edwards

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

pS

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

c,

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

.

Pipeline attachment accessary

13 •

"

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

•

- 1 -

24

1Q-F029-19-830

General description Cover f i x i n g

screw-^^^s>

^X^JN^^^

iff I ^^

y^

Capillary line to expansion— valve phial

Hains Cable

<
V \ ^ *

Ta rmi nal ^ S . Block ^*V. > /

,

V

J \ \ ^ \ ^ ^

Refrigerant liquid receiver

Condenser chamber

^1 Refrigerator,^

Refrigerator condensar

m

TA

\

1

i

1I

Pirani

J-y

^4 ^

y^

head

1

Cover fixing screw

U

HI

!

Expansion valve ^Sy

Mains indicator lamp

-Temperature indicator .Refrigerator on/off switch

\

X

^ r ^ i ^-

Pirani vacuum gauge ^ \

^

^

Alr a

«"anc.i

-^^'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 332 mm 535 mm 622 mm

height width depth

45 kg

Weight Electrical requirements

220-24QU 50 Hz, 1 phase 60 Hz version, also available

Power consumption

3Q0W (fuse ^ amp)

Refrigerator

Prestcold

ft.

size

V 3 hp (250U) hermetrically sealed 180 k/cal/h at -35°C (at 20°G ambien-t) R502

heat extraction rate refrigerant CondBnser ice capacity in 12h ice capacity in 24h ica capacity in total minimum temperature under vacuum surface area volume average evaporation rate (manifold)

... •* •

1.2 kg 2.3 kg 4.0 kg

•• • •• * •• •

-60°C 0.15m2 7.2 litres

•• *

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 . 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.

UN

I 1 1 1 II

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.

I I

I I

|

1 1 1

I I

\

1

I I

u . ca

1 1 1 1 II

III 1 1 1 1

1Q0-

1 1 1 1 II

10-1 CD f-l

\

CD CO CD U Q.

I I1

-

10-2 HIM

N

1 1

5 4 3t-

I I

2 I-S 10-3

0

-10

-20

-40

-30

-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 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 ittance 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 ittance 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. 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 -

Do not

Shelf and stoppering accessory

Stoppering —. Mechanism

/iTfL—/iLJn <s*—

1 u—'

Top Plate

s

—1 W

^

—--SB-e-jB-es;

Shelf

^^>

— " j U l /

,[]

Shelf •L• Gaskst

\^—

~^Z-^'\\ ' '—T

Shelf •

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) 73mm (open)

37mm (closed) 57mm (-closed)

(3 shelf version) (2 shelf uersion)

Maximum number of vials

per shelf

per assembly 2 shelf 246 178 142 78

per assembly 3 shelf 369 267 213 117

14mm 16mm 18mm 24mm

od od od od

123 " 89 71 39

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. 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.

Partially stopper

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 ittance 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) 5)1 6)

Switch on the refrigerator. When the condenser reaches -45°C switch on the rotary vacuum pump and open the gas ballast valve. 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 . 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, pushfitting 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 it 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 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 ittance valve.

7)

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

8)

Slowly open the air ittance 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 . 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.

T caver

•3-cing

,3uppoct :aas

?ecaining :•/Under aaaanisly

3*tsining : i j a i i a d i n s i i s cylincac)

csncansac cnamoar fLanga

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 ittance 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.

" ' • ' • • ' •

~..*—^r\,fi.j,i;rzv.*££.Sl<j •-:•

Position 2

Position 1

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 ittance 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 ittance 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 ittance 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 ittance 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 Motor consumption Motor speed Fuse rating Number of ampoules per carrier

240V 1ph 50Hz 8 watts 780 r.p.m. 3A 96 (0.5 ml) 24 (2.5 ml) 12 (5.0 ml)

Clamping Knob Top Plate '(Single Hols) Spacer and Pin Centre Plate (Two Holes) Spacer and Pin

Ampoule Holder Assembly

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) 9)

Switch on the refrigerator. 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 ittance 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 2

Ampoule carrier supplied with accessory 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. 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,

4)

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 secure with three screws.

over the condenser chamber and

7)

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

8)

Close the air ittance 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 ittance 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 blankingoff 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) EF4 Flodulyo basic unit (110V, 60Hz, lph) Spares kit Speedivalve Diaphragm uasher for AV5 Mains switch and lamp Thermocouple Expansion value Vacuum hose Qowty seal -J- inch 0-ring 0-ring . 0-ring Process accessories Specimen dryer accessory Shelf and stoppering attachment Drum manifold accessory Rubber value (specify quantity) B24 male connexion piece (specify quantity) Vapour trap/pipeline attachment In-line manifold accessory Glass isolation valve (specify quantity) Secondary drying accessory Secondary drying header (order with above) Centrifuge accessory Heated tray accessory Acrylic bell jar 'L' gasket for use with bell jar Optional accessories Trolley Coupling kit for vacuum pump attachment Cooling bath with one bottle spinner Bottle spinner (additional) Ampoule constrictor Flamemaster hand torch Spark tester ST4ivl Oil mist filter 0F1F12 Leak detector LT10 Rotary vacuum pump Edwards ED50 (220-2401/, 50Hz, lph) Edwards ED50 (110V, 60Hz, lph) No.18 vacuum oil (l litre) Vacuum gauge Pirani 10 vacuum gauge PIrani PR10S gauge head

10-F029-19-880

- 22 -

10-F029--19-000 10-F029--20-000 10-F029--19-800 Q8-C150--00-042 08-D118--01-003 10-F023--05-027 10-F023--05-029 10-F023--10-010 08-H021- -00-005 08-H021- -04-002 08-H021- -20-027 Q8-H021-,25-116 08-H021- -25-205 10-F029--10-000 10-F023--01-110 10-F023-•03-060 1Q-F023--03-058 10-F023--03-059 10-F023--05-021 10-F029--09-000 10-F029--09-016 10-F029-•42-000 10-F023--27-000 10-F029--11-000 10-F029-•12-000 10-F023-•01-046 10-F023-•01-018 10-F023-•05-020 10-F029-•41-000 10-F029-•13-000 10-F029-•13-001 26-F041-•01-000 26-F098-•00-000 07-H020-•02-000 04-A131-•05-000 17-0137-•15-000 03-A044-03-614 Q3-A044-03-911 09-H110-05-015 07-D035-23-000 07-0024-21-000

Supplementary instructions Spesdivalve Air ittance valve AU5 •Pirani vacuum gauge Pirani gauge heads

1*108784 ["108789 1*107865 07-D024-21-880

•• • •• *

•*

Accessory instructions Edwards Edwards Edwards Edward's Edwards Edwards

ED50 rotary vacuum pump cooling bath ampoula constrictor •... spark tsster ST4C1 ... oil mist filter 0P1F12... leak detector LT10 ...

« t

•

•

*

•

1*103894 T0-F029-13-881 1*110759 1*107855 1*104628

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