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Laboratory intership   archer and mang por
 

Laboratory intership archer and mang por

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    Laboratory intership   archer and mang por Laboratory intership archer and mang por Presentation Transcript

    • Polymer Synthesis
      By: MangPor (AtimaKreemaha) and Archer (Archer Jirasirikul)
    • 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
    • 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
    • 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
    • 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)
    • 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
    • Data
    • Catalyst synthesis
    • 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
    • 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
    • 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
    • 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
    • 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
    • Data
      199.9
    • Transesterification (Part I)
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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)
    • 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
    • Transesterification (Part II)
    • 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
    • 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
    • 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
    • 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
    • Data
    • Data NaOH +
      1.3505 × 2
      ___________
      = 90.03%
      1.0000 × 3
    • 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.
    • 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 (>_<“)