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Laboratory intership archer and mang por

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  • 1. Polymer Synthesis
    By: MangPor (AtimaKreemaha) and Archer (Archer Jirasirikul)
  • 2. Equipments
    3-aminophenol (NH2OH) 50g
    Ammonium persulfate ((NH4)2S2O8) 75g
    1M Sulfuric Acid (H2SO4 ) 185mL
    Magnetic bar 1bar
    Droppers 1dropper
    Flasks 2flasks
    Beaker 2beakers
    Volumetric flask 1flask
    Distilled Water 100mL
    Magnetic Stirrer 1stirrer
    Filter paper 1paper
    Litmus paper 1paper
    Incubator 1Incubator
    Weighing scale 1scale
    Labeling tags 2tags
    Stirring rod 1rod
    Vial 1vial
  • 3. Procedures
    Label the flask as PmAP (Polyaminophenol)
    Weigh 50g of NH2OH in a flask
    Put the magnetic bar in the flask
    Make a 185mL of 1M H2SO4 using a volumetric flask
    Pour the 1M H2SO4 into the flask that contains the NH2OH
    Place the flask on the magnetic stirrer
  • 4. Procedures (continue)
    Start stirring at the speed level of about 5
    Weigh 75g of (NH4)2S2O8 in a beaker
    Calibrate 100mL of distilled water using another beaker
    Add the distilled water to the beaker with (NH4)2S2O8
    Use a stirring rod to stir the solution until it completely dissolve
  • 5. Procedures (continue)
    Using a dropper, drop the (NH4)2S2O8 solution into the PmAP flask, one drop at a time until the (NH4)2S2O8 solution has all been added (do not stop stirring at this step)
    Stir for 24 hours
    Filter the solution into another flask
    Wash it until it has the pH of 7 (check this using the litmus paper)
  • 6. Procedures (continue)
    Incubate at 80 degrees Celsius for 24 hours (to make sure that all the water has evaporated)
    Store the powder in a vial
    Label the vial as PmAP
  • 7. Data
  • 8. Catalyst synthesis
  • 9. Equipments
    Poly-aminophenol (PmAP) 2.72825g
    Sodium Hydroxide (NaOH) 0.75g
    Distilled Water 150mL
    Weighing Scale 1scale
    Spatula 1spatula
    Beakers 5beakers
    Incubator 1incubator
    Labeling tags 10tags
    Magnetic bar 5bars
    Magnetic stirrer 5stirrers
    Graduated cylinder 1cylinder
    Timer 1timer
    Vial 5vials
  • 10. Procedures
    Label the beakers as 1.25, 2.5, 3.75, 5, and 6.25mmol NaOH
    Weigh out about 545.65mg of PmAPin the beaker using the electronic scale and spatula
    Repeat step 2 for the other 4 beakers
    Weigh out about 50mg of NaOH using the other side of the spatula
    Add it to the 1.25mmol NaOH beaker
    Weigh out about 100mg of NaOH
    Add it to the 2.5mmol NaOH beaker
  • 11. Procedures (continue)
    Weigh out about 150mg of NaOH
    Add it to the 3.75mmol NaOH beaker
    Weigh out about 200mg of NaOH
    Add it to the 5mmol NaOH beaker
    Weigh out about 250mg of NaOH
    Add it to the 5mmol NaOH beaker
    Use the graduated cylinder to calibrate 30mL of distilled water
    Add it to a beaker
  • 12. Procedures (continue)
    Repeat step 14 and 15 for the other 4 beakers
    Put a magnetic bar in each beaker
    Put each beakers on a magnetic stirrer
    Turn the stirrers on at the stirring speed of 5.5 - 6
    Leave it for 1 hour
    Turn the stirrer off
    Put all the beakers in the oven at the temperature of 60 degrees Celsius
  • 13. Procedures (continue)
    Leave them until they’re dry
    Label the vials as 1.25, 2.5, 3.75, 5, 6.25mmol NaOH
    Use a spatula to scratch the catalyst off of the beakers into the vial with the same label
  • 14. Data
    199.9
  • 15. Transesterification (Part I)
  • 16. Equipments
    Catalyst (from the step before) 5types
    Soybean oil 50g
    Methanol 35mL
    Timer 1timer
    Beakers 7beakers
    Graduated cylinder 1cylinder
    Magnetic bars 5bars
    Double neck flask 5flasks
    Bowl of oil 5bowls
    Hot plate with a magnetic stirrer 5plates
    Temperature probe 5probes
    Weighing Scale 1scale
    Normal Stopper 5stoppers
    Stopper with hole 5stoppers
    Parafilm 10blocks
    Funnels 5funnels
    Filter paper 5papers
    Flasks 5flasks
    Label tags 5tags
  • 17. Procedures
    Pour some soybean oil into a beaker
    Weigh out about 10g of oil from the beaker into a double neck flask using a weighing scale
    Repeat step 2 for 4 other flasks
    Put a bowl of oil on each of the heat plate
    Attach each double neck flask to the heat plate with magnetic stirrer
  • 18. Procedures (continue)
    Move it so the flask is dipped in the oil
    Turn the machine on to heat up the oil
    Pour some methanol into a beaker
    Weigh out about 0.3g of all 5 types of catalyst into 5 different beakers
    Use a graduated cylinder to measure about 7mL of methanol
    Add it to a beaker
  • 19. Procedures (continue)
    Repeat step 10&11 to the other 4 beakers
    Wait for 5 minutes
    Pour each substance in the beakers in each double neck flask that’s being heated
    Put a magnetic bar in each flask
    Start stirring at about level 5
    Put a normal stopper in one of the neck of each flask
    Put a stopper with hole on the other neck of each flask
  • 20. Procedures (continue)
    Put a temperature probe in each flask through the stopper with hole so that the probe just slightly touch the solution
    Use 2 blocks of a parafilm to cover the gap of the stopper with hole
    Do the same for the other 4 flasks
    Wait for one hour but come check the temperature probe every once in a while to make sure that the temp. is about 60~70 degrees C
  • 21. Procedures (continue)
    Turn off the hot plate and stirrer
    Fold 5 filter papers in a way that will maximize the area used for filtering
    Put each filter paper on each funnel
    Put each funnel in each flask
    Label the flasks using the label tags (label it the same as the vials)
  • 22. Procedures (continue)
    Pour the substance from the double neck flask that uses the catalyst from the vial to the flask with the same label (through the filter paper)
    Wait until it finish filtering
    Take a small sample of each filtered solution
    Run it through NMR
  • 23. Transesterification (Part II)
  • 24. Equipments
    Sodium Hydroxide (NaOH) 0.2g
    Polyaminophenol (PmAP) 0.21g
    Soybean oil 10g
    Methanol 2.5mL
    Timer 1timer
    Graduated cylinder 1cylinder
    Magnetic bars 1bar
    Double neck flask 1flask
    Bowl of oil 1bowl
    Hot plate with a magnetic stirrer 1plate
    Temperature probe 1probe
    Weighing Scale 1scale
    Normal Stopper 1stopper
    Stopper with hole 1stopper
    Parafilm 2blocks
    Beakers 1beaker
  • 25. Procedures
    Weigh 10g of Soybean oil to a double neck flask
    Calibrate 2.5mL of methanol in a beaker
    Weigh out 0.2g of NaOH
    Add the NaOH to the beaker
    Add the substance in the beaker into the double neck flask
    Attach it to a hot plate with magnetic stirrer
  • 26. Procedures (continue)
    Turn on the heat at 60~65 degrees Celcius and the stirring level of about 5
    Put a normal stopper in one of the neck
    Put a stopper with hole into the other neck
    Stick the temperature probe inside so that it barely touches the solution
    Use 2 blocks of parafilm to close the gap between the probe and stopper
    Wait for 1 hour
  • 27. Procedures (continue)
    Turn off the machine
    Take a sample of the solution
    Weigh out 0.21g of PmAP
    Add the PmAP to the solution
    After had completely dissolved, take another sample of it
    Run it through NMR
  • 28. Data
  • 29. Data NaOH +
    1.3505 × 2
    ___________
    = 90.03%
    1.0000 × 3
  • 30. Conclusion
    We have confirmed that PmAP-Na catalyst isn’t a good heterogeneous catalyst for the transesterification due to the fact that the catalyst can dissolves in methanol. There could be many human errors. For example, the amount of substance added is wrong, the calculation is wrong, etc.
    As shown in the result, the higher the amount of NaOH, the more yield the substance tends to have. Although the fact that the catalyst “5mmol of NaOH + 5mmol of PmAP” gain lower yield than the catalyst “3.75mmol of NaOH + 5mmol of PmAP” could be the result from the human errors we had done.
  • 31. Thank You
    Thank You makmaknakub P’ Ing and P’ Suai for helping us during the internship (^_^)/
    P.S. We forgot to take pictures with you two (>_<“)