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CHEM123 Experiment 10 Caffeine Extraction and Purification From Cola

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65 views

CHEM123 Experiment 10 Caffeine Extraction and Purification From Cola

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anonstudent415
Copyright
© © All Rights Reserved
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CHEM123 Experiment 10: Caffeine Extraction and Purification from Cola

Research Question:
How does the yield of 3 washes of 10mL DCM compare to 2 washes of 15mL DCM in the
extraction of caffeine from a 50mL cola sample?

Hypothesis:
If the caffeine is rinsed with 3 washes of 10mL of DCM, the yield will be higher than if the caffeine
is rinsed with 2 washes of 15mL of DCM.

Note: the cola we used had to be pre-heated to half its original volume. Amount cola found in given
volume is actually present in twice the given volume.

Glassware:
25mL graduated cylinder: for measuring out NH4OH
250mL beaker: for collecting organic extract from cola
Fume hood: to whisk away volatile fumes
Separatory funnel: for separating cola into organic and aqueous layers and extracting the
organic layer
Round bottom flask with plastic holder: for collecting dried organic extract during drying of
caffeine
Filter paper: for filtering out water residue from extracted caffeine
Glass funnel: for filtering out water from organic extract
Rotary evaporator: for removing DCM from dried product
Capillary tube: to fill up with caffeine and be inserted in the melting point apparatus
Melting point apparatus: shake caffeine to the closed end of the capillary tube, to determine
the melting point of caffeine
Vacuum sublimation apparatus: to purify caffeine
Vacuum outlet adapter: for secondary drying of caffeine

Chemicals:
Cola
NH4OH
Dichloromethane
caffeine
CHEM123 Experiment 10: Caffeine Extraction and Purification from Cola

Procedure:
Extracting crude caffeine from cola
1. Using a 25mL graduated cylinder, add 10-15 mL of ammonium hydroxide (NH4OH) to the
given 50mL cola sample and swirl to mix liquids. NH4OH is added because caffeine is
basic and will not react with it. The unwanted acids in the cola will react with NH4OH,
forming ammonium salts and remaining in a distinct aqueous layer, thus making caffeine
extraction more effective.
2. Making sure your solution is at room temperature, pour it into a separatory funnel, making
sure the stopcock is closed (horizontal).
3. In the fume hood, add 10mL of dichloromethane (DCM) to the mixture in a separatory
funnel (given 30mL for all the separations you will perform)
4. Making sure the funnel vent is pointed away from people, open stopcock to release gas
5. Close the stopcock, shake the funnel gently
6. Vent the pressure. Repeat this process 5 times.
7. Let the funnel sit for a few minutes for distinct layers to form. Record observations of layers,
how they form.
8. Place a beaker under the stopcock, remove the stopper and drain the organic layer into a
250mL beaker
9. Repeat steps 3-8 for 2 more washes with 10mL DCM each

Drying the Organic Extract


1. Weigh a clean dry 100mL round bottom flask on analytical balance, record mass
2. Flute your filter paper and place it in the dry funnel (see figures 1 and 2)
3. Wet the filter paper using a dropper full of DCM (DCM and water have different polarities,
thus water will not pass through filtration)
4. Pour organic extract through filter paper into the pre-weighed round bottom flask
5. Stopper the flask in the fume hood before taking sample back to lab bench

Note: the cola we used had to be pre-heated to half its original volume. Amount cola found in given
volume is actually present in twice the given volume.
Solvent Removal: Isolation of the Product
1. Remove the DCM from the round bottom flask using a rotary evaporator
2. Once DCM is removed, wait for RBF to cool to room temperature. Then, quantitatively
weigh the crude caffeine using the analytical balance. Record mass to 4 decimal places.
3. [the following steps were added on during the lab]
4. In the fume hood, drop a few drops of DCM into RBF, redissolve the product
5. Using a Pasteur pipet, transfer the dissolved product into a clean dry test tube
6. Place the test tube into a beaker containing some water. Heat the water using a hotplate
set to 4 until the DCM evaporates and you are left with a solid white powder

Use this mass of crude caffeine to compare the amount of caffeine in sample

Determine the melting point of caffeine


1. Transfer some of the dry solid sample onto a watch glass
2. Using a capillary tube, tap some of the caffeine into the tube. There should be around 3mm
of caffeine
3. Fill another capillary tube with pure caffeine obtained from the TA.
4. Use the tube tapper function on the melting point apparatus to shake the caffeine to the
closed end of the tube
5. Place both tubes into the melting point apparatus at the same time to conduct a melting
point analysis.
6. Once have green LED lights for READY and STOP, insert capillary tubes in the melting
oven and press START button.
7. When RAMP green and MELT red, keep eyes on view finder and fingers on buttons 1 and 2
always. At slightest hint of brown color, click the sample number’s button. Once sample
completely brown, click again.
8. Once test is done, click STOP. Click number button associated with your sample to see
starting temperature, click again to see ending temperature
9. Observe and record the melting point range of both crude and pure samples. Colour
transparency, state. How do your results compare to the literature value? Is your sample
relatively pure (+/- 2°C of literature value, 40°C)

Purification of Caffeine
1. The crude caffeine will be purified using vacuum sublimation. The apparatus must be dry so
that no additional liquid condenses outside the cold finger, thus rendering the caffeine
deposits impure
2. Flask should be in a clamp, on a hotplate
3. Using a spatula, scoop crude caffeine into the flask
4. Pack the stopper test tube with ice, making sure the outside is dry
5. Stopper flask, connect vacuum line to flask. Turn on pump, then turn on green tap.
6. Turn hotplate onto setting 3. Heat for 15 minutes, or until all caffeine has sublimed
7. Break vacuum connection first, then turn off tap
8. Turn off hotplate, move it away from flask. Allow apparatus to cool.
9. Remove test tube. Pure caffeine is deposited on the outside of the cold-finger during
evaporation.
10. Are the crude sample and the sublimate the same colour? Record observations
11. Conduct a melting point analysis of the purified caffeine and record the value

Note: if the sample was wet during sublimation or the technique not performed correctly, can
increase temperature range and drop melting point compared to crude sample

CRC Handbook of Chemistry and Physics. Dichloromethane.


http://wwwhbcpnetbase.com (accessed February 11, 2023)

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