STKM 2211 FOOD ANALYSIS LABORATORY

PRACTICAL 8:
ISOLATION OF CAFFEINE FROM TEA BAG

LECTURER: ASSOC. PROF. Ts. DR LIM SENG JOE

NAME: NOR AFIFAH BINTI MOHD AKHIAR

MATRIC NUMBER: A192577

GROUP: 1
OBJECTIVES:

1. To extract caffeine from tea powder using polar – nonpolar solvent.

2. To understand three methods of isolation of caffeine from tea bag by extraction,
recrystallization, and melting point determination.
3. To obtain purity of the extracted caffeine using weight of crystal and melting point.

INTRODUCTION:
Caffeine (C8H10N4O2) is the common name for trimethylxanthine (systematic name is 1,3,7-
trimethylxanthine or 3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione). Caffeine is naturally
produced by several plants, including coffee beans, guarana, yerba maté, cacao beans, and tea.
Caffeine is a stimulant. It acts by reversibly blocking adenosine from binding a receptor that causes
drowsiness.
In pure form, caffeine is a bitter, white, crystalline powder. Plants produce caffeine to deter pests
and to prevent nearby seeds from germinating. Caffeine is the most widely used drug in the world.
When purified, caffeine is an intensely bitter white crystalline powder. It is added to colas and
other soft drinks to impart a pleasing bitter note.
Caffeine is a minor constituent of tea, coffee, and other natural plant materials. The major
constituent of tea is cellulose which is not water soluble. Caffeine is water soluble but so are some
tannins and gallic acid which is formed in the process of boiling tea leaves. The latter two
components can be converted to their calcium salts which are insoluble in water. The caffeine can
then be extracted from the water by methylene chloride in almost pure form.
Extraction is the physical process by which a compound (or mixture of compounds) is transferred
from one phase to another. An extraction takes place each time coffee or tea is made. Water-soluble
components in the tea leaves or coffee beans are being transferred from a solid phase, the leaves,
or beans, into a liquid phase, the hot water. This is an example of solid liquid extraction.
Using the proper extraction methods, the caffeine within a tea bag could potentially be isolated to
yield a pure solid; the mass of this solid would reflect the actual yield of caffeine in the tea. To
do so, caffeine is soluble in hot water and is extracted from coffee grounds or tea leaves when
these products are brewed.
The product that is collected after extraction still has many impurities. Sublimation is one way to
purify the sample, because caffeine has the ability to pass directly from the solid to vapor and
reverse to form a solid without undergoing the liquid phase. Caffeine has the ability to undergo
sublimation under different conditions than the impurities and can thus be isolated.
RESULTS:
Melting point ( ̊C )
Weight of caffeine from set A = 0.0224g 222.7
Weight of caffeine from set B = 0.0262g 226.2

DISCUSSION:
Based on the experiment, the weight of caffeine from set B is higher than weight of caffeine
from set A which is 0.0262g and 0.0224g. Also, the melting point of set B is higher 226.2 ̊C than
set B 222.7 ̊C, respectively.
This is because extraction from set B was repeated three times compared to set A. Repeated
extractions will increase the extraction yield. This means, partition coefficient is high. To
conclude, the higher the number of extraction steps, the higher the extraction yields. The
efficiency of the extraction needs to be taken into consideration. The solubility of the
components in aqueous or organic solvents and the ability to separate the solvent after extraction.
The partition coefficient is the equilibrium constant for the distribution of a solute between two
immiscible layers. A partition coefficient can be estimated as the ratio of solubilities of the
compound in both solvents.
In this case, caffeine is water soluble, it is much more soluble in the organic solvent methylene
chloride (CH2Cl2) or known as dichloromethane. Methylene chloride is immiscible with water
and when mixed separates from water to form a two-layer mixture. Because methylene chloride is
denser than water it usually comprises the lower layer in the two-part mixture. By mixing brewed
tea with methylene chloride, caffeine can be extracted into the organic layer. Since the organic
layer is immiscible with water, it can be removed after it separates from the water, and the solvent
evaporated to give nearly pure caffeine.
However, during the experiment, only a small amount of crystalline was produced in the test tube.
It happened because during boiling from the process purification of caffeine by sublimation, the
substance splashed out from the test tube due to huge amount of dichloromethane used to dissolve
and rinse the caffeine crystal. The amount of dichloromethane use should be few drops only
because the size of the test tube is small, that is why the substance splashed out and produced small
amount of crystal only.
Since the crystal produced in a small amount, we scrapped out the whole bottom of the test tube
to weight and measured the melting point. Pure caffeine (trimethylxanthine) occurs as a white
powder or as silky needles, which melt at 238 °C (460 °F). However, from this experiment
obtained were 222-226 ̊C. It can be concluded that the substance produced contains impurities that
can alter the purity of the extracted caffeine.
Hence, this experiment is important because extraction is a principal method for isolating
compounds from plant materials. Also, for product refining and customers satisfaction because
caffeine affects human psychology health and behaviors.
Next, there are a few safety precaution steps taken in this practical. DCM is a possible carcinogen
so it should be handled in fume hoods. During extractions, we need to release the pressure, so point
the separatory funnel stem away from face into the fume hoods.

CONCLUSION:
In this study, the weight and melting point of pure extracted crystal caffeine can be determined.
The results obtained from set B produced higher weight 0.0262g than set B 0.0224g and higher
melting point 226.2 ̊C than set A 222.7 ̊C. As conclusion, this experiment has been carried out
successfully.

QUESTIONS:
1. Explain why the amount of caffeine in set B is more than set A?

The amount of caffeine in Set B is more than set A because it was repeated three times of
extraction process. Repeated extractions will increase the extraction yield which
increases the partition coefficient value (the ratio of solubilities of the compound in both
solvents). The larger the value of partition coefficient, the more of the solute we have
extracted or partitioned into the organic phase.

2. Give one example each of industrial application of solid/liquid and liquid/liquid

extractions.

Solid liquid extractions in industrial application of food industry are widely used. Solid–
liquid extraction is a unit operation with diverse applications in the food industry.
Supercritical Fluid extraction (SFE) involves the separating of a mixture, in solid or liquid
state or in solid and liquid state, by contacting it with a fluid maintained under conditions
of temperature and pressure above its critical point.
As an example, extraction of sugar from sugar cane or sugar beet; isolation of vegetables
oils from different seeds.

Liquid–liquid extraction, sometimes also called solvent extraction. Examples of extraction

are found in the edible oil industry in which oil is extracted from natural products such as
peanuts, soya beans, rapeseeds, sunflower seeds and so on.
 3. Twenty milliliters of an aqueous solution of 0.10M butyric acid was shaken with
10mL of ether. After the layers are separated, it is determined by titration that 0.5M
of butyric acid remains in the aqueous layer. What is the distribution ratio and what
is the percentage of butyric acid extracted?

Initial mole of butyric acid:

20mL × 0.10 M = 2 mol

Mole butyric acid extracted:

2 – 0.5M = 1.5 mole

1.5 0.5
initial ∶ = 0.15 𝑀 after ∶ = 0.025 𝑀
10 20

0.15
Distribution Ratio = =6
0.025

100 ×6
%E= 20 = 75%
6 +( )
10

REFERENCES:

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https://studylib.net/doc/8218995/caffeine-extraction-lab-report-2
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