Innovative Programme
Minutes
Date: 07-05-07
Venue: Applied Chemistry Lab
Aim of the day: Extraction, Purification and Distillation of 2L (1st) batch.
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Grouping and discussion of individual tasks
• Short term
• Long term
Group 1
Boon Tiong (Leader)
Siew Fang
(Production)
Jessica
(HR)
Group 2
Joshua
Ming Jing
(Leader)
(HR)
Group 3
Ee Sang
Yi Jiang
(Leader)
(Production)
Short Term (2wks)
1.
2.
3.
4.
Letter of confidentiality/contact list
Structure of organisation- Science website (Hierarchy)
Excel Production Sheet (Accounting)
Testimonial Questions
a. Introduction (Abstract)
b. Questions
Long Term (6mths)
1.
2.
3.
4.
5.
6.
7.
50% TA commitment
Recording of results
Biobiz 2007 (sep/oct)
Pharmacy Dept
9th Start Up (Jan/Feb)
Recruitment
OUR (Outstanding Undergraduate Research)
-
Familiarize with equipment and procedures
1. Separate into groups of 3. Doing cleaning of fementor, preparation of broth
solution, centrifuge, extraction, rotavap and distillation.
2. Used Diethyl ether as solvent and failed to recover during rotavap. Planned to
use Methyl-tert-butyl ether the next day.
3. Started with vacuum distillation. Learnt to decrease pressure bit by bit to
avoid mixture from being sucked back. Product will be out at temperature
around 40°C, pressure at around 10mbar.
4. Due to time constraint, we stopped at vacuum distillation. Tap water is used
for the condenser.
Problems faced
1. Limited amount of equipment: only
2 2L beakers available.
2. Diethyl ether not able to recover.
3. Pressure remained at 60mbar for
quite a long time due to large
amount of solvent remained in
mixture.
Solution/Lesson learnt
1. We try to use the next bigger
beaker. While doing centrifuge, we
will start with extraction.
2. Use methyl-tert-butyl ether as
solvent due to higher boiling point.
3. Rotavap mixture for a longer period
of time. Use ice water for the next
batch.
Innovative Programme
Minutes
Date: 08-05-07
Venue: Applied Chemistry Lab
Aim of the day: Distillation of 2L (1st) batch. Extraction, Purification and Distillation of
4L (2nd) batch.
-
Grouping for tasks
Fementor
Centrifuge
Extraction
Rotavap
Distillation
(3)
(1)
(2)
(1)
(3) & Victor
1. Carried out distillation using ice water for condenser. Use aluminium foil to
cover the glass.
2. Prepare 6L (3rd) batch broth solution.
3. Methyl-tert-butyl ether run out, stock expected to come at 3pm.
4. Watched video on proper use of equipment.
5. Used anhydrous ether in the end. Do no submerge into the basin as anhydrous
ether has very low melting point. Mixture will feel cold due to enthalpy of
vaporization.
6. GC takes around 20min for each sample.
Problems faced
Solution/Lesson learnt
1. Limited amount of solvent
available.
1. Always check for availability of
chemical.
2. Anhydrous ether not able to recover.
2. Use methyl-tert-butyl ether as
solvent.
3. Rotavap mixture for a longer period
of time.
3. Pressure remained at 60mbar for
quite a long time due to large
amount of solvent remained in
mixture.
Innovative Programme
Minutes
Date: 09-05-07
Venue: Applied Chemistry Lab
Aim of the day: Extraction, Purification and Distillation of 6L (3rd) batch. Analysis of GC
result.
-
Analyse GC results
Enantiomeric excess = (area S – area R)/total area
1st Pear shape enantiomeric excess
1st Pear shape purity
2nd Pear shape enantiomeric excess
2nd Pear shape purity
-
:
:
:
:
97.1%
89%
97.7%
96%
Grouping for tasks
Fementor
Centrifuge
Extraction
Rotavap
Distillation
(2)
(3)
(1)
(3)
(2)
1. Solvent came at 10am. People for lower level complained strong ether smell.
Production stops in the morning.
2. We were asked to dispose all used chemical (solid & liquid) into a container
and label as ‘Non-Chlorinated waste’.
3. Started production after lunch. Failed to recover methyl-tert-butyl ether.
Lowered chiller temperature to 2°C. Being using 10°C for the past few days.
90% methyl-tert-butyl ether recovered.
Chiller consists of 30% ethylene gycol/70% H2O.
Specific Heat
: 0.9
Normal Range
: 0°C -90°C
Extreme Range
: -15°C - 107°C
-
Amount of ethyl Acetoacetate used
1st Batch : 8mL (0.8mL/hr)
2nd Batch : 16mL (1.6mL/hr)
3rd Batch : 24mL (2.0mL/hr)
-
Solvent Recovery
1L of mixture: 1L of ether (Do a recovery check)
Problems faced
1. Failed to recover methyl-tert-butyl
ether. Complain of strong ether
smell
Solution/Lesson learnt
1. Lowered chiller temperature to 2°C
to maximise recovery.
Innovative Programme
Minutes
Date: 10-05-07
Venue: Applied Chemistry Lab
Aim of the day: Distillation of 4L (2nd) and 6L (3rd) batch.
-
Distillation
1. Started with pressure 300mbar.
2. When pressure reach about 12-12mbar, temperature is expected to be 100°C
(90°C for our experiment)
3. Our product theoretically should be out at 10mbar, 60°C. (Majority fall into
1st fraction at condition 10-12mbar, 70°C)
4. Product out at condition 8-9mbar & 60-62°C for our experiment.
5. Our machine can’t go below 6mbar.
6. Do not add ice immediately for condenser as solvent will condense and
remain in system. This will cause pressure to remain at around 60mbar for
quite some time. So allow solvent to come out before adding ice into basin to
condense mixture for higher purity.
7. Do no need to dismantle everything while washing. Use ethanol to wash
column with a beaker to contain the waste.
-
Rotavap
1. Water can be re-use but is not advisable.
-
Disposal of waste
1. Label container as ‘Non-Chlorinated waste’ (sticker) because we are using
only ether.
2. Write the date of disposal and venue as S8-04-04 on the sticker.
3. Disposal of waste is every Thursday, 2.45pm-3pm. Each disposal is $40.
-
Gas Chromatography
1. Go to S 6 level 4, Catalysis Laboratory.
Innovative Programme
Minutes
Date: 11-05-07
Venue: Applied Chemistry Lab
Aim of the day: Re-distillation of 6L (3rd) batch. Distill Victor’s sample.