DEPARTMENT OF CHEMISTRY

FACULTY OF SCIENCE AND MATHEMATICS

EXPERIMENT 2
SKA 3013 ANALYTICAL CHEMISTRY

NAMA & MATRIC NO. 1. RONALD DECK YAMI (D20171078135)

2. NORAINI SHAHIRA BINTI WARIANTO
(D20181083306)
EXPERIMENT NO 2
TITLE EXTRACTION OF ANALYTICAL CHEMISTRY
GROUP B
LECTURER PROF. MADYA DR. AZLAN BIN KAMARI
INTRODUCTION

The technique used to separate an organic compound from a mixture of compounds is called
Extraction. Extraction process selectively dissolves one or more of the mixture compounds into
a suitable solvent. The solution of these dissolved compounds is referred to as the Extract. Here
the organic solvent dichloromethane is used to extract caffeine from an aqueous extract of tea
leaves because caffeine is more soluble in dichloromethane (140 mg/ml) than it is in water (22
mg/ml).
Liquid–liquid extraction, also known as partitioning, is a separation process consisting of
the transfer of a solute from one solvent to another, the two solvents being immiscible or
partially miscible with each other. Frequently, one of the solvents is water or an aqueous
mixture and the other is a non-polar organic liquid. As in all extraction processes, liquid–liquid
extraction comprises a step of mixing (contacting), followed by a step of phase separation. It
is important to consider both steps in the selection of solvents and modes of operation.
Beverages cover a vast variety of addictive drinks out of which
Tea and Coffee are the most popular acceptable drinks. Tea powder is
extracted from tea leaves which contain tannins, which are acidic in
nature, a number of colored compounds and a small amount of
unrecompensed chlorophyll and an important stimulant called
Caffeine. Because of the presence of Caffeine, tea and coffee are
gaining popularity as an addictive stimulant. An average 30g of tea
can contain 20-ll0 mg of caffeine thereby making tea a significant source of caffeine compared
to other beverages. Caffeine can stimulate nervous system and can cause relaxation of
respiratory and cardiac muscles.
Caffeine is well known to increase both the alertness level and attention span. But like all
other addictive, tea also shows withdrawal symptoms like headache, nervousness and insomnia
for a regular consuming person. Caffeine, 1,3,7 - trimethylxanthine, belongs to a wide class of
compounds known as alkaloids. These are plant derived compounds with complex structure
containing nitrogen, and usually have roles in physiological activity. The melting point of
Caffeine is 238°C.
OBJECTIVE

1. To extract caffeine from beverages using liquid–liquid extraction technique.

2. To determine amount of caffeine present in beverages.
3. To determine the KD of caffeine between water and dichloromethane solvent.

PROCEDURE
*refer jotter

RESULT

1.1 Filter the caffeine solution

Sample (g) A B C
- -
Mass of petri dish 34.719

Filtration of solution
 1.2 Collect the white crystal

Sample A B C
Mass of petri dish + white 34.721 - -
crystal (g)
0.002 - -
Mass of white crystal (g)
217.5 - -
o
Melting point ( C)

1.3 Collect the white crystal

white crystal

1) Why Na2CO3 and Na2SO4 were added into the beverage solution during the experiment?
Sodium carbonate is added to the extraction medium to ensure that the acidic components
in the tea leaves remain water soluble and that caffeine is the free base. Sodium carbonate
is basic. It is also to remove excess water so that a pure sample of caffeine could be obtained
after the solvent evaporated at room temperature.

2) Estimate the purity of your caffeine based on its melting point and color of the sample.
𝑚𝑒𝑙𝑡𝑖𝑛𝑔 𝑝𝑜𝑖𝑛𝑡 𝑜𝑓 𝑐𝑎𝑓𝑓𝑒𝑖𝑛𝑒 𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑
𝑇ℎ𝑒 𝑝𝑢𝑟𝑖𝑡𝑦 𝑜𝑓 𝑐𝑎𝑓𝑓𝑒𝑖𝑛𝑒 = × 100%
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑒𝑙𝑡𝑖𝑛𝑔 𝑝𝑜𝑖𝑛𝑡 𝑜𝑓 𝑐𝑎𝑓𝑓𝑒𝑖𝑛𝑒
The purity of the caffeine based on the melting point is
= (217.5 / 238.0) x 100% = 91.39%.
The colour of the sample is dark purple.
3) Calculate the percentage of caffeine in each of sample and determine the average.

Percentage of the caffeine = 0.002 x 100%

0.500

= 0.4 %
The average is not calculated since we only do 1 sample.

4) Assume that the percentage of caffeine in your original beverage samples is 5%.
Calculate the KD of caffeine.

𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑜𝑓 𝑐𝑎𝑓𝑓𝑒𝑖𝑛𝑒 𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑

1
Volₐ
=[ ] × 𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑜𝑓 𝑐𝑎𝑓𝑓𝑒𝑖𝑛𝑒 𝑖𝑛 𝑠𝑎𝑚𝑝𝑙𝑒
(Kᴅ × Volₒ) + Volₐ

1
30 ml
0.0040 = [ ] × 0.05
(Kᴅ × 20 ml) + 30 ml
Kᴅ= 17.25

5) Do you think the amount of caffeine acquired is similar to the real amount of caffeine
that found in your beverage sample? Give reasons for your answer.

Yes, I think the amount of caffeine acquired is not similar to the amount of caffeine that
found in the beverage’s samples. This is due to the percentage of the caffeine that we
only get is 0.4%.
Several organic solvents can be used to extract organic materials from aqueous solutions.
The most common solvents are as follows:
a) Chloroform
b) Toluene
c) Ethyl acetate
d ) Diethyl ether

Draw the molecular structure of the solvents and determine which solvent will be on top
or bottom layer if the extraction occur from aqueous medium. Discuss.

1. Chloroform

2. Toluene

3. Ethyl acetate
 4. Diethyl ether

Based on the solvents given, only chloroform will be at the bottom during the extraction
meanwhile toluene, diethyl ether and ethyl acetate will be at the top if the extraction occurred.
This is due to the density of the chloroform which is denser than the aqueous solution. For this
aqueous solution, the density is 0.998 g/cm3. The density of the chloroform is 1.483 g/cm3
while for the toluene, ethyl acetate and diethyl ether are 0.867 g/cm3. 0.900 g/cm3 and 0.714
g/cm3 respectively. Hence, the denser will be at the bottom.

CONCLUSION

For this experiment, we use tea leaves as our caffeine extraction sources. Dichloromethane is
used our organic solvent to extract the caffeine from the aqueous solution. This is because the
caffeine is more soluble in Dichloromethane. By having a different density, we can have two
separable solutions which is organic solvent and the aqueous solution. The amount of caffeine
that we extracted is 0.4% and the melting point of the caffeine is 217.5°c.

REFERENCE

Othmer, D., & Tobias, P. (1942). Liquid-liquid extraction data-the line correlation. Industrial
& Engineering Chemistry, 34(6), 693-696.

Shashi, Pradeep & Ashoka, Hadgali & Gn, Rameshaiah. (2015). CAFFEINE EXTRAVTION
AND CHARACTERIZATION.
Mumin, A., Akhter, K. F., Abedin, Z., & Hossain, Z. (2006). Determination and
characterization of caffeine in tea, coffee and soft drinks by solid phase extraction and high
performance liquid chromatography (SPE–HPLC). Malaysian Journal of Chemistry, 8(1),
045-051.

McCusker, R. R., Goldberger, B. A., & Cone, E. J. (2006). Caffeine content of energy drinks,
carbonated sodas, and other beverages. Journal of Analytical Toxicology, 30(2), 112-114.