sop/pd/317 02 standard operating procedure€¦ · 3.1. batch operation: ... release adapter [8] to...
TRANSCRIPT
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
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
5.1. Diagram of Bibby Sterilin® Rotary Evaporator RE-100 3
5.2. Installation 4
5.3. Operation 5
5.4. Maintenance 7
5.5. Troubleshooting 8
5.6. Flow Charts 9
6. Precautions 15
7. References 15
8. Appendices 15
9. Revision History 16
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
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.
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 3 of 17
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_02/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_02/A1)
11. Vacuum Seal Assembly
(see SOP/PD/317_02/A1)
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 4 of 17
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_02/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_02/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_02/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_02/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_02/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_02/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_02/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.
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 5 of 17
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_02/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_02/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.
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 6 of 17
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.
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 7 of 17
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.
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 8 of 17
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
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 9 of 17
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
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 10 of 17
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
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 11 of 17
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
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 12 of 17
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
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 13 of 17
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
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 14 of 17
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
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 15 of 17
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_02/A1 – Accompanying Installation Diagrams
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 16 of 17
9. Revision History
Version Number Amendments/ Reasons for change
01 Initial Release
02 Inclusion of subheading titles of
Procedure section in Table of Contents
Update of entire SOP to Version 2
UNIVERSITY OF MALTA
FACULTY OF MEDICINE & SURGERY
PHARMACY DEPARTMENT Ref. No. SOP/PD/317_02
STANDARD OPERATING PROCEDURE
BIBBY STERILIN® RE-100
ROTARY EVAPORATOR
Valid for:
2 years from
approval
Page 17 of 17
SOP/PD/317_02/A1 – Accompanying Installation Diagrams
Figure 1 Figure 2
Figure 3 Figure 4
Figure 5