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 (>_<“)