Abstract:

Caffeine (𝐶8𝐻10𝑂2𝑁4) is founded in the cola drink. Crude caffeine is obtained through selective
extraction, filtration, and solvent removal. By comparing the obtained caffeine's melting point to
the given pure caffeine, one can assess the purity of caffeine crude. Using the aforementioned
techniques and dichloromethane (DCM), it was discovered that the amount of times DCM
utilised (same total volume) has an impact on the purity of the caffeine.
Introduction:
Caffeine was first discovered in 1819. It acts as a central nerve stimulant, preventing sleepiness
and boosting alertness for a short period of time (1). Also, it can be found in certain types of
drinks like coffee, tea, energy drinks, and cola beverages. They determined the caffeine crude
from a variety of sources and then by using the developed method - High performance liquid
chromatography (1) to obtain the caffeine, they have shown how effective this method was.
This study was conducted to determine the effect of the number of times DCM utilised (same
total volume) on caffeine purity. The extraction method is used to separate an organic
compound from a mixture compound (diet cola drinks). The filtering and solvent removal are
used later to obtain crude caffeine. To determine caffeine purity, compare the melting point of
received caffeine to the melting range of pure caffeine which is 234 - 239 ℃ (1). Also, DCM (
𝐶𝐻2𝐶𝑙2) has boiling point of 39. 6 °C, and it is used for caffeine extraction because caffeine is
sparingly soluble in most polar solvents but is highly soluble in less polar solvents (1). As the
result, the more time washing DCM to the extraction, the higher of caffeine purity.
Experimental Section: (Method)
(Working under fume hood) To extract the caffeine from diet cola drink, mix 50 mL of sample,
10-15 mL ammonium hydroxide (10% concentration), and 15 mL of DCM in the separatory
funnel. When it was fully separated, allow organic layer (clear color) to run into the 50 mL
beaker. Repeat the process with another 15 mL DCM. Weight a dry clean 100 mL round bottom
flask (RBF). Pour all extracted compounds into a folded filter-paper (pre-wet with DCM).
Eventually, all the caffeine product is contained in the RBF. To isolate crude caffeine: connect
the RBF (contain caffeine) to rotator; open green tab; adjust the RBF to hot bath, turn on rotator
and the crude will finally be on the RBF. Then connect RBF to vacuum pump to make sure it
dries completely. Weigh the RBF to determine the weight of crude caffeine is formed. Add a few
drops of DCM into the RBF, and use the pasteur pipette to transfer all mixture into a small test
tube, leave the tube inside a 10 mL beaker (already have water), which is placed on the hot
plate (turned to 3). After a while, use spatula to take all the caffeine to the watch glass.
To determine melting point, insert about 3 mm of caffeine into capillary tube, when the melting
point apparatus is ready, place both obtained caffeine tube and pure caffeine tube into channels.
Observe and record the melting range for both. For purification: add crude to the flask and fully
add ice into the cold finger, connect vacuum line and turn on pump, leave about 10 mins, pure
caffeine is deposited outside of cold finger.
Result:
Table 1: Crude caffeine obtained of teammate: (2x15 mL of DCM) - Group 1
Member 1 Member 2 Member 3 Member 4

Weight 0.0239 g 0.0297 g 0.0210 g 0.0182 g

Table 2: Crude caffeine obtained by another group: (3x10 mL of DCM) - Group 2

Weight 0.0280 g 0.0161 g 0.0669 g 0.0257 g 0.0263 g

Average 0.0326 g
weight
- Determined weight of caffeine = 0.0297 g ⇒ The yield per cent: 74.25%
- Melting range for obtained caffeine: 233.3 - 236.9℃
- Melting range for pure caffeine: 234.1 - 239.2℃
- Melting range for sublimated caffeine: 231.8 - 232.9℃
Discussion:
The average weight yield amount of caffeine in group 2 is higher than group 1 which is similar to
the hypothesis. The reason for this difference is group 2 performed more washing time with
DCM than group 1. DCM is used because caffeine is more stable in DCM than water as the
solvent is much denser than the water and is insoluble in it. The more time washed with DCM,
the fewer impurities in the mixture. However, there were some errors since the amount of
member 3 in group 2 was significantly high. This error can result if the initial volume of diet cola
is larger than required or perform the techniques wrongfully which lead to the impurities instrude
into the mixture. Based on the result, the melting range for obtained caffeine is similar to the
melting range for pure caffeine. However, regard the melting range for sublimated caffeine, it is
a little lower than the standard range, which is the result of some errors as mentioned while
performing the crude caffeine but it is still within + or - 5℃. Therefore, it is accepted.
To improve the result, instead of using the melting point apparatus, it is suggested to use the
High performance liquid chromatography (1). There could be some experimental errors while
observing the melting point of the caffeine because we determine just by looking when it started
to melt and when the process was done. Meanwhile, High performance liquid chromatography
is a very sensitive technique as it incorporates a wide range of detection methods. Moreover, it
would be more precise if the given equipments is more accurate (i.e. using the pump to pump
out the dcm, the set value of the pump could be changed a little bit after many time of uses; the
dark compound could flow into the beaker if the performer mistakenly did it during the
extraction. Ultimately, the result is similar to the hypothesis since the average weight of formed
caffeine in group 2 is higher than group 1 so the yield per cent in group 2 is higher than group
1.
Conclusion:
There are more caffeine is form when perform more time of the extraction with DCM, which is
align to the hypothesis.
Bibliography:
(1) Pradeep, S. International journal of current research and review. 2015, 2231-2196.