Experimental Procedure

N.B: The volume of the soft drink has been reduced to exactly half of its initial volume.

Extraction

1. Ensure the stopcock of the separatory funnel is closed. Then measure out 50 ml of cola
into the funnel.

2. Add between 10 and 15 ml of ammonium hydroxide to the cola. Close the stopcock and
swirl to mix the two liquids together.

3. Pour in 10 ml of the dichloromethane solution into the separatory funnel.

4. Seal the funnel and remove it from the stand. While holding the stoppered end, turn it
upside down. Open the stopcock to release pressure.

5. Close the stopcock and rock the funnel gently from side to side for a few seconds. Do not
do this vigorously. Vent the pressure thereafter.

6. Repeat about 5 times, releasing the pressure from time to time.

7. Place the funnel in the stand once again and let the solvents separate. If an emulsion
forms, stir the contents of the flask using a stirring rod.

8. Place a beaker under the funnel and draw off the bottom organic layer. If a bubble layer
forms, ensure it doesn’t leave the funnel.

9. IMPORTANT NOTE - DON’T USE UP ALL THE DICHLOROMETHANE - Some is needed for
the drying steps. Add another 10 ml portion of dichloromethane into the separatory
funnel and repeat the steps above. Do this one more time until all the dichloromethane is
used up, each time combining all the organic extracts into one beaker.

Drying the Organic Extract

1. Weigh a clean beaker/100ml round bottom flask on the analytical balance.

Mass of Empty Beaker/Flask - ________________________ g

2. Fold a sheet of filter paper so that it becomes fluted (refer to page 147). Place the filter
paper inside of the filter funnel and place the pre-weighed beaker/flask under the stem
of the funnel.

3. Using a Pasteur Pipet, wet the paper with about 5 ml of dichloromethane. Pour the
organic extract through the funnel.
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Isolating the Crude Caffeine from the Dichloromethane

1. In a fume hood, place the flask/beaker onto a hot plate and switch it on to the lowest
setting. The boiling point of dichloromethane is around 35-40 0 c.

2. Cool the beaker/flask to room temperature and then weigh it using the analytical balance
once again.

Mass of Beaker + Crude Caffeine - ________________________ g

Melting Point Determination

1. Place the crude caffeine onto a watch glass and dip the open end of the capillary tube
into the sample. Invert the tube and tap it gently until the solid falls to the closed end. If it
doesn’t drop the capillary tube through a dropping tube.

2. Prepare another capillary tube with pure caffeine.

3. Place both the tubes into the DigiMelt apparatus at the same time and record:

- Temperature when first trace of liquid appears (Slightest change in colour from white to
brownish)

Crude Caffeine - __________ 0 c

Pure Caffeine - __________ 0 c

- Temperature when last trace of solid disappears (When the white colour completely
disappears)

Crude Caffeine - __________ 0 c

Pure Caffeine - __________ 0 c

Vacuum Sublimation to Purify the Crude Caffeine

1. By collecting crude caffeine samples from 3-5 students, place the crude caffeine into the
flask using a spatula. Seal the flask using the stopper and attached cold finger. Ensure the
cold finger is about 1 cm away from the crude caffeine.

2. Start the water pump to provide a vacuum.

3. Fill the cold finger with water and ice and turn the hot-plate onto setting 4.

4. After all the solid has sublimed, turn off the hotplate and remove it from under the flask.

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5. Leave the flask to cool for 15 minutes with the water pump still on.

6. Release the pressure from the flask by breaking the vacuum by separating the two parts
of the hose pipe. Turn off the water pump only after this.

7. Remove the cold finger and scrape off the pure caffeine onto a watch glass.

8. Measure the melting point of the purified caffeine.

- Temperature when first trace of liquid appears (Slightest change in colour from white to
brownish)

Purified Caffeine - __________ 0 c

- Temperature when last trace of solid disappear (When the white colour completely
disappears)

Purified Caffeine - __________ 0 c

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Data Tables

Isolation of Crude Caffeine from Dichloromethane

Mass of Empty Beaker / Flask (g)

Mass of Beaker + Crude Caffeine g)

Mass of Crude Caffeine (g)

Melting Point Determination of Crude Caffeine and Pure Caffeine

Sample Crude Caffeine Pure Caffeine

Temperature 1 (first trace of liquid) / 0 c

Temperature 2 (last trace of solid) / 0 c

Melting Point Determination of Purified Caffeine

Sample Purified Caffeine

Temperature 1 (first trace of liquid) / 0 c

Temperature 2 (last trace of solid) / 0 c

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