SOP/PD/317 01 STANDARD OPERATING PROCEDURE · PDF fileSOP/PD/317_01 STANDARD OPERATING PROCEDURE ... Clean all glassware with distilled water and examine for scratches, cracks and

UNIVERSITY OF MALTA

FACULTY OF MEDICINE & SURGERY

PHARMACY DEPARTMENT Ref. No. SOP/PD/317_01

STANDARD OPERATING PROCEDURE

BIBBY STERILIN® RE-100

ROTARY EVAPORATOR

Valid for:

2 years from

approval

Page 1 of 17

Table of Contents

Page

1. Scope 2

2. Objective 2

3. Definitions 2

4. Responsibility 2

5. Procedure 3

6. Precautions 15

7. References 15

8. Appendices 15

9. Revision History 16

Original

Authorised Copy

for:

Reading Copy

Written by: Signature/Date:

Reviewed by: Signature/Date:

Approved by: Signature/Date:

UNIVERSITY OF MALTA





ROTARY EVAPORATOR

Valid for:

2 years from

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Page 2 of 17

1. Scope

This Standard Operating Procedure (SOP) applies to the staff and students

using the Bibby Sterilin®

RE-100 Rotary Evaporator in the laboratories of the

Pharmacy Department, University of Malta.

2. Objective

To describe the procedure for the installation, operation and maintenance of

the Bibby Sterilin® RE-100 Rotary Evaporator.

3. Definitions

3.1. Batch Operation: An operational process that is carried out using a

fixed amount of material and terminates when this is used up.

3.2. Chemical Etching: The formation of characteristic features on metal

or glass surfaces after exposure to a chemical reagent.

3.3. Continuous Feed Operation: An operational process that is

continuously supplied with material and only terminates when the

operator stops the supply of this material.

3.4. Evaporating / Florentine Flask: The flask that contains the liquid to

be evaporated and is continually rotated to increase the surface area of

the liquid surface.

3.5. Implosion: The inward collapse of a highly evacuated glass vessel.

3.6. Receiving Flask: A round bottomed flask in which the distillate

collects in.

3.7. Rotary Evaporator: A distillation unit that incorporates a condenser

with a rotary flask system that rotates to continually transfer a thin

layer of liquid over the entire inner surface to increase the surface area

for evaporation by heating.

4. Responsibility

4.1. The members of the Department of Pharmacy (staff and students) are

responsible for following this SOP.

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4.2. The designated Laboratory Officer or Laboratory Assistant is

responsible for ensuring that this SOP is followed.

5. Procedure

5.1. Diagram of Bibby Sterilin® Rotary Evaporator RE-100

1. Stand 12. Up/Down Lift Switch

2. Drive Motor 13. Mains On Indicator

3. Rotation Speed Control 14. Manual Lift Clamp

4. Condenser 15. Water Connections

5. Rotating / Florentine Flask 16. Vacuum Line Connections

6. Receiving Flask 17. Motor Support Bracket

(see SOP/PD/317_01/A1)

7. Vapour Tube 18. Motor Support Rod

8. Feed / Vacuum Release Adapter 19. Condenser Reatining Cap and Spring

9. Spherical Joint Clip 20. Glassware Angle Hand Clamp

10. Conical Joint Clip 21. Jack (see SOP/PD/317_01/A1)

11. Vacuum Seal Assembly

(see SOP/PD/317_01/A1)

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5.2. Installation

5.2.1. Place the stand [1] on a level surface.

5.2.2. Fit the motor bracket [17] to the top of the jack [21].

5.2.3. Check that the fitting for the support rod is facing forward.

5.2.4. Check that the bracket is angled downwards (see

SOP/PD/317_01/A1 fig1).

5.2.5. Tigthen the allen screws with an allen key.

5.2.6. Place the support rod [18] into its fitting.

5.2.7. Tigthen the accompanying allen screw.

5.2.8. Check that the end of the screw locates in the recess of the rod

(see SOP/PD/317_01/A1 fig 1).

5.2.9. Place the motor assembly [2] onto the support rod [18].

5.2.10. Tighten the hand clamp [4] to fix the motor assembly in

position.

5.2.11. Check that the speed control [3] is facing foward.

5.2.12. Check that the clamp is located on the flat side of the rod.

5.2.13. Check that the motor is located as low as possible on the

support rod.

5.2.14. Plug the electrical connection of the motor into the socket at the

rear end of the stand.

5.2.15. Pass the plain end of the vapour tube [7] through the motor

assembly.

5.2.16. Push this vapour tube firmly into position until it locates firmly

behind the spring clip.

5.2.17. Check that the conical joint is on the right of the motor when

viewed from the front (see SOP/PD/317_01/A1 fig 2).

5.2.18. Place the defender, main vacuum seal and subseal onto the

vapour tube.

5.2.19. Slide these components of the vacuum seal down until they

locate in the bearing housing (see SOP/PD/317_01/A1 fig 2).

5.2.20. Check that all 3 elements of the vacuum seal are fitted in the

correct sequence (see SOP/PD/317_01/A1 fig 2).

5.2.21. Check that the spring loaded slide of the main seal is facing the

bearing housing (see SOP/PD/317_01/A1 fig 2).

5.2.22. Place the retaining cap [19] over the wide end of the condenser

with the screw thread facing outwards.

5.2.23. Retain cap in position with the circular spring (see

SOP/PD/317_01/A1 fig 3).

5.2.24. Place the condenser over the vapour tube so that the wide end

of the condenser squeezes up to the vacuum seal.

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5.2.25. Check that the spherical joint is pointing downwards.

5.2.26. Screw the retaining cap onto the bearing housing to secure

tightly.

5.2.27. To set the condenser to the required angle:

5.2.27.1. Support condenser while loosening the hand clamp

[20].

5.2.27.2. Position the condenser at the required angle.

5.2.27.3. Hold it in place while re-tightening the hand clamp.

5.2.28. Hold the receiving flask [6] in position and secure using the

spherical joint clip [9].

5.2.29. Place the rotating flask [5] onto the end of the vapour tube and

secure using the conical joint clip [10].

5.2.30. Remove plastic safety connectors from the condenser and fit

into the hose.

5.2.31. Secure the hose using a Jubilee clip.

5.2.32. Fit the connectors and the hose to the water inlet and outlet

connections on the condenser respectively (see

SOP/PD/317_01/A1 fig 4).

5.2.33. Remove the grey plastic screwcap that is attaching the feed

vacuum release adapter to the condenser.

5.2.34. Assemble the screw cap onto the feed/vacuum release adapter

(see SOP/PD/317_01/A1 fig 5).

5.2.35. Pass the tube that is attached to the feed/vacuum release adapter

through the condenser and vapour tube.

5.2.36. Check that the end of this tube is inside the rotating flask.

5.2.37. Tigthen the grey screwcap onto the screw thread of the

condenser.

5.3. Operation

5.3.1. Batch Operation

5.3.1.1. Remove the rotating flask [5] from the vapour tube

[7].

5.3.1.2. Fill the rotating flask with the liquid to be evaporated

ensuring that it is not more than half full.

5.3.1.3. Check that both the stop cock and vacuum release

screwcaps are closed.

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5.3.1.4. Check that water is flowing through the condenser at

approximately 60L/hr.

5.3.1.5. Check that the speed control [3] is set to 0.

5.3.1.6. Switch on the electricity supply. The green “mains

on indicator” will light up.

5.3.1.7. Press and hold the [UP] switch until the glassware

stops moving to raise the glassware assembly to the

highest position.

5.3.1.8. Place a suitable water bath directly below the

rotating flask.

5.3.1.9. Press and Hold the [DOWN] switch until the rotating

flask is partially immersed in the water of the water

bath.

5.3.1.10. Set the speed control [3] to the required setting. A

yellow lamp will light up on the speed control.

5.3.1.11. Attach a vacuum line to the side arm of the

condenser [16] if evaporation at reduced pressure is

desired.

5.3.1.12. Set the temperature of the water bath to the desired

temperature.

5.3.1.13. Wait for the evaporation process to be complete.

5.3.1.14. Unscrew the vacuum release screwcap.

5.3.1.15. Set the rotation speed control to 0.

5.3.1.16. Press and hold the [UP] switch to raise the glassware

out of the water bath.

5.3.2. Continuous Feed Operation

5.3.2.1. Attach a length of flexible tubing to the sidearm of

the feed/vacuum release adaptor [8].

5.3.2.2. Repeat steps 5.3.1.3 to 5.3.1.9.

5.3.2.3. Immerse the free end of the flexible tubing into the

container holding the liquid to be evaporated.

5.3.2.4. Attach a vacuum line to the side-arm of the

condenser [16].

5.3.2.5. Slowly open the stopcock on the feed/vacuum

release adapter [8] to draw liquid into the rotating

flask by the created vacuum.

5.3.2.6. Close the stopcock when sufficient liquid has entered

the flask.

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5.3.2.7. Set the speed control [3] to the required setting. A

yellow lamp will light up on the speed control.

5.3.2.8. Set the temperature of the water bath to the desired

temperature.

5.3.2.9. Re-open the stopcock when further quantities of

liquid will need to be added during the evaporation.

5.3.2.10. If receiving flask requires emptying during the

operation:

5.3.2.10.1. Raise glassware out of the water bath.

5.3.2.10.2. Wait until boiling ceases and distillate

stops dripping into the receiver flask.

5.3.2.10.3. Stop rotation and release the vacuum.

5.3.2.10.4. Remove the receiving flask.

5.3.2.10.5. Empty the receiving flask.

5.3.2.10.6. Re-attach the receiving flask.

5.3.2.10.7. Lower the glassware into water bath.

5.3.2.10.8. Set the speed control to the required

Setting to continue the process.

5.3.2.11. Repeat steps 5.3.1.14 to 5.3.1.16 when evaporation

process is complete.

5.4. Maintenance

5.4.1. Isolate unit from the mains electricity, water and vacuum

supplies before commencing with any maintenance procedures.

5.4.2. Wash the vacuum seal with distilled water and allow to dry

naturally.

5.4.3. Clean all glassware with distilled water and examine for

scratches, cracks and signs of chemical etching.

5.4.4. Replace any damaged parts before further use.

5.4.5. Clean the main stand and the motor with a mild cleaning agent.

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5.5. Troubleshooting

Fault Cause/s Solution/s

Poor Vacuum

- Faulty vacuum pump

- Vacuum seal inserted wrong

way round

- Dirty vacuum seal

- Worn vacuum seal

- Loose condenser screw cap

- Dirty Quickfit joints

- Scratched Quickfit joints

- Loose vacuum connection

- Split „O‟ ring vacuum

connector

- Check that stopcock and

vacuum release screwcap are

closed

- Check vacuum pump

- Arrange accordingly

- Remove and clean

- Replace

- Check and fasten tightly

- Clean

- Check and replace

- Check and tighten

- Check and replace

Noisy Operation N/A

Remove vapour tube and apply

vacuum grease to the inner ground

surface

Inoperative drive

motor N/A

Check plug fuse and the fuses in the

rear of the stand

Inoperative lift N/A Check fuse in plug and the fuses in

the rear of the stand

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5.6. Flow Charts

5.6.1. Installation

Start

Place stand [1] on level surface

Fit motor bracket [17] to top of jacket [21]

Check that fitting for support

rod is facing downwards

Check that bracket is angled downwards

Tighten allen screws with allen key

Place support rod [18] into its fittings

Check that end of screw locates in recess of rod

Place motor assembly [2]

onto support rod [18]

Tighten hand clamp [4]

to fix motor in position

Check that speed control [3]

is facing forwards

Check that clamp is located on flat side of rod

Check that motor is located as low

as possible on support rod

1

Plug electrical connection of motor into

socket at rear end of stand

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1

Pass plain end of vapour tube [7]

through motor assembly

Push vapour tube firmly into position until it

locates firmly behind spring clip

Check that conical joint is on the right of

motor when viewed from front

Place defender, main vacuum seal

and subseal onto vapour tube

Slide these components down until

they locate in bearing housing

Check that all 3 components are

fitted in the correct sequence

Check that spring loaded slide of main

seal is facing the bearing housing

Place retaining cap [19] over wide end of

condenser with screw thread facing outwards

Retain cap in position with circular spring

Place condenser over vapour tube so that wide

end of condenser squeezes up to vacuum seal

Check that spherical joint

is pointing downwards

Screw retaining cap onto bearing

housing to secure tightly

2

Need to set condenser

to a required angle 3

Yes

No

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2

Support condenser while

loosening hand clamp [20]

Position condenser at required angle

Hold in place while re-tightening hand clamp

Hold receiving flask [6] in position and secure

using spherical joint clip [9]

Place rotating flask [5] onto end of vapour

tube and secure using conical joint clip [10]

Remove plastic safety connectors from

condenser and fit into the hose

Secure hose using Jubilee clip

Fit connectors and hose to water inlet and

outlet connections on the condenser

Remove grey plastic screw cap that is

connecting the feed vacuum release adapter to the condenser

Assemble screw cap onto

feed/vacuum release adapter

Pass tube that is attached to feed/vacuum release adapter

through condenser and vapour tube

Check that end of tube is inside rotating flask

Tighten grey screw cap onto screw thread of condenser

End

3

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5.6.2. Operation

Start

Perform batch

operation

Remove rotating flask [5] from vapour tube [7]

Fill rotating flask ensuring

that it is not > half full

Check that both stop cock and vacuum

release screwcaps are closed

Check that water is flowing through

condenser at approx 60L/hr

Check that speed control [3] is set to 0

Switch on electricity supply

Press and hold [UP] switch

until glassware stops moving

Place a suitable water bath

directly below rotating flask

Press and hold [DOWN] switch until rotating

flask is partially immersed in water bath

Set speed control [3] to required setting

Evaporation at reduced pressure is

desired

2

3

Attach a length of flexible tubing to sidearm of feed/vacuum release adapter [8]

Immerse free end of flexible tubing into

container holding liquid to be evaporated

Check that both stop cock and vacuum

release screwcaps are closed

Check that water is flowing through

condenser at approx 60L/hr

Check that speed control [3] is set to 0

Switch on electricity supply

Press and hold [UP] switch

until glassware stops moving

Place a suitable water bath

directly below rotating flask

Press and hold [DOWN] switch until rotating

flask is partially immersed in water bath

Attach vacuum line to

side-arm of condenser [16]

Slowly open stopcock on feed/vacuum release adapter [8] to draw liquid into the rotating flask

4 Yes

Yes

No

No

Perform continuous

feed operation 1

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Attach vacuum line to the

side arm of condenser [16]

2

Set T of water bath to the desired T

Unscrew vacuum release screwcap

when evaporation is complete

Set rotation speed control [3] to 0

Press and hold [UP] switch to

raise glassware out of water bath

3

Close stopcock when sufficient

liquid has entered the flask

Set speed control [3] to desired setting

End

4

Set T of water bath to the desired T

Re-open stopcock when further

quantities of liquid need to be added

Raise glassware out of water bath

Receiving flask

requires emptying

Wait until boiling ceases and distillate

stops dripping into receiver flask

Stop rotation and release vacuum

Remove receiving flask

Empty receiving flask

Re-attach receiving flask

Lower glassware into water bath

Set speed control to required setting to continue the process

5

5

Yes

No

1

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5.6.3. Maintenance

Start

Isolate unit from mains electricity, water

and vacuum supplies before commencing with any maintenance procedures

Wash with distilled water and

allow to dry naturally

Clean with distilled water and examine for

scratches, cracks and signs of chemical etching

Replace before further use

Clean using a mild cleaning agent

End

Vacuum seal

needs cleaning

Glassware needs

cleaning

Any damaged parts

Main stand and/or

motor needs cleaning

Yes

Yes

Yes

Yes

No

No

No

No

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6. Precautions

6.1. Examine all glassware for any signs of scratches or chemical etching

before operating the apparatus under vacuum due to the risk of

implosion.

6.2. Take special care when using the evaporator with flammable solvents.

6.3. Never fill the rotating flask by more than half of its capacity i.e.

approximately 500ml.

6.4. When lowering the glassware into the water bath, ensure that the

glassware does not make contact with any part of the bath and that the

water does not overflow as the flask is immersed.

6.5. When setting the desired speed of rotation, ensure that the rotation is

not so fast that the water is splashed out of the bath.

6.6. In the event of a power failure, the glassware may be raised manually

in the following manner:

6.6.1. Disconnect from the electricity supply.

6.6.2. Set the speed control to 0.

6.6.3. Loosen the hand clamp [14].

6.6.4. Lift the drive motor and glassware assembly up the support rod

[19].

6.6.5. Tighten the hand clamp [14].

6.6.6. Re-position accordingly to the normal operating position at the

bottom of the support rod before further use.

6.7. Ensure that no strain is applied to the feed/vacuum release adapter

during a continuous feed operation.

6.8. Ensure that, each time liquid is added to the rotating flask during a

continuous feed operation, there is sufficient capacity in it to cope with

this addition.

6.9. Any servicing or repair should only be undertaken by suitably qualified

personnel.

7. References

Bibby Sterilin. Rotary Evaporator RE-100 Assembly and Operating

Instructions.

8. Appendices

SOP/PD/317_01/A1 – Accompanying Installation Diagrams

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9. Revision History

Version Number Amendments/ Reasons for change

01 Initial Release

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SOP/PD/317_01/A1 – Accompanying Installation Diagrams

Figure 1 Figure 2

Figure 3 Figure 4

Figure 5

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SOP/PD/317 01 STANDARD OPERATING PROCEDURE · PDF fileSOP/PD/317_01 STANDARD OPERATING PROCEDURE ... Clean all glassware with distilled water and examine for scratches, cracks and