Innovative Programme

Minutes

Date: 07-05-07

Venue: Applied Chemistry Lab

Aim of the day: Extraction, Purification and Distillation of 2L (1st) batch.

-Grouping and discussion of individual tasks

•Short term

•Long term

Group 1

Boon Tiong(Leader)

Siew Fang(Production)

Jessica (HR)

Group 2

Joshua(Leader)

Ming Jing(HR)

Group 3

Ee Sang(Leader)

Yi Jiang(Production)

Short Term (2wks)

  1. Letter of confidentiality/contact list
  2. Structure of organisation- Science website (Hierarchy)
  3. Excel Production Sheet (Accounting)
  4. Testimonial Questions
  5. Introduction (Abstract)
  6. Questions

Long Term (6mths)

  1. 50% TA commitment
  2. Recording of results
  3. Biobiz 2007 (sep/oct)
  4. Pharmacy Dept
  5. 9th Start Up (Jan/Feb)
  6. Recruitment
  7. 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 / Solution/Lesson learnt
  1. Limited amount of equipment: only 2 2L beakers available.
  1. Diethyl ether not able to recover.
  1. Pressure remained at 60mbar for quite a long time due to large amount of solvent remained in mixture.
/
  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(3)

Centrifuge(1)

Extraction(2)

Rotavap(1)

Distillation(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. Anhydrous ether not able to recover.
  1. Pressure remained at 60mbar for quite a long time due to large amount of solvent remained in mixture.
/
  1. Always check for availability of chemical.
  1. Use methyl-tert-butyl ether as solvent.
  2. Rotavap mixture for a longer period of time.

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:97.1%

1st Pear shape purity :89%

2nd Pear shape enantiomeric excess:97.7%

2nd Pear shape purity :96%

-Grouping for tasks

Fementor(2)

Centrifuge(3)

Extraction(1)

Rotavap(3)

Distillation(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

NormalRange: 0°C -90°C

ExtremeRange: -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 / Solution/Lesson learnt
  1. Failed to recover methyl-tert-butyl ether. Complain of strong ether smell
/
  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.