A.

THE TITLE OF EXPERIMENT

Caffeine extraction.
B. THE AIM OF EXPERIMENT
The purpose of experiment is to know the continiue of extraction with that
heat.
C. REVIEW OF THEORY
Tea, Camellia sinensis, is a small tree native to the Assam area of North India
where North Burma and South China meet. This region has had a tumultuous
history, linked to the OpiumWars between the United Kingdomand China, and
theWar of Independence between theUnited States and theUnitedKingdom, the
growth of urban centres, the expansion of the British Empire, the birth of the
British Industrial Revolution and many more events. After water, tea is now the
most consumed beverage in the world UK Tea Council 2010), drunk for both
pleasure and health (Crozier, A. Et. All, 2012 : 1).
Coffee is produced from the seeds of another small tree, originating this
time from Africa, spread via the slave trade to the Arabic empires where it gained
pre-eminencedue to the Muslim ban on fermented alcoholic beverages.

Coffea arabica, Coffea robusta and Coffea liberica were discovered the later and
were transplanted across the world to establish plantations/estates in as far away
places as Hawaii, Brazil and Vietnam. From this position, and coffee has become,
after oil, and the second most valuable traded commodity on the global stock
market (Crozier, A. Et. All, 2012 : 1-2).
Tea refers to the agricultural products of the leaves, leaf buds and
internodes of the Camellia sinensis plant. It has been consumed as a beverage for
almost 2,000 years starting in China. It is the most widely consumed beverage
after water. Teas from many areas may be blended. The aim is to obtain better
taste, and higher price or both, as a more of the expensive, better tasting tea may
cover the inferior taste of cheaper varieties. Both contain caffeine (1 to 5) % of its
dry weight depending on type, brand and brewing method. This is why the
reported values in the literature are so variable. Caffeine belongs to a family of
naturally occurring components known as xanthines. The xanthines which come
from plants are possibly the oldest known stimulants. Caffeine is the most
powerful xanthine, in its ability to increase alertness, put off sleep and to improve
attention in study, caffeine is a vasodilator (relaxes the blood vessels) as well as a
diuretic (increase urination) (Atomssa. Tadelech, Gholap. A.V, 2011).
Tea is intimately linked with Asia, herbal medicine and Buddhism. Almost
the time 4000 years ago, in 2737 bc, the great herbalist, ‘Divine Healer’ and
Chinese emperor Shen Nung discovered tea (Ukers 1935). The story is that he
observed leaves that had fallen from a nearby and unassuming tree being boiled
in water by his servant. Upon tasting the brew, the emperor found it to his liking
and the thus green tea was ‘discovered’. This also indicates that the Chinese
already knew the value of making water drinkable by boiling it to kill microbial
contamination. This habit still remains in China to this day where boiled drinking
water is preferred, being served still and warm, rather than the glass of cold iced
water demanded by other cultures. Tea, as luck would have it, has antimicrobial
properties from the inherent catechin and caffeine contents, so it has a double
benefit when consumed hot! In Chinese herbal medicine, ‘bitter’ is seen as a
desirable trait (Crozier, A. Et. All, 2012 : 3).
Extraction is transfer of the solute from the feed stream (known in
hydrometallurgy as pregnant liquor) to the solvent. A high concentration of the
extractant decreases the phase ratio; that is, smaller solvent inventory and smaller
plant will suffice. On the other hand it may harm the phase separation, that is, it
may lower the flux and require a larger plant. This also makes the solvent, per
volume unit, more expensive, increasing the cost of entrainment losses.
Extractions often use two immiscible phases to separate a solute from one phase
into the other. Typical lab extractions are of organic compounds out of an aqueous
phase and into an organic phase (Marcus. Yizha and Sengupta. A, 2002 : 5-7).
 Continuous Extractions is an extraction is still feasible even when the
component of interest has an unfavorable partition coefficient, provided that all
other components in the sample have significantly smaller partition coefficients.
Because the partition coefficient is unfavorable, a simple extraction will not be
quantitative.

Many continuous extractions involving solid samples are carried out with a
Soxhlet extractor. The extracting solvent is placed in the lower reservoir and
heated to its boiling point (David. Harvey, 2000 : 213-214).
The organic solutes are more completely removed by extracting with tea at
temperature above 55oC, temperatures at which tea is not miscible with water. A
predetermined amount of caustic must be added to maintain the final pH of the
mixture at between 10,5 and 11. This keeps tea in its nonionized form. Typically,
the solvent/solid ratio is 3:1, and mixing times very from 5 to 15 min per
extraction. The extract is centrifuged to separate to solid from the mixture so the
solids can be returned to undergo further extrations. The liquid phase (tea, water,
and oil) is heated to about 77oC. At this temperature, the tea water azeotrope will
boil, leaving the oil phase to be removed from the extraction vessel. Since tea and
water are immiscible above 55oC, the tea and water separate into two phase in a
decanter. The experimental results show that the methanol is better than n-hexane
but an extraction time of 9 hours was required for stems and roots while 12 hours
for leaves (Marcus. Yizhak, et. All, 2002 : 204).
Caffeine content in tea leaves cannot be determined directly using UV-
visible spectrometer, due to the matrix effect of UV absorbing substances. This
effect can be observed in the spectral bands of tea leaves in water as shown in
Figure 8; as seen from the Figure, caffeine spectra interface with other compounds
in tea leaves. Therefore, it is necessary to develop a method to overcome this
difficulty. The method developed in these experimental activities is to first
dissolve caffeine in water and then extract it, using dichloromethane as mentioned
in the procedure part. To determine caffeine from tea leaves, the extractions were
repeated four times until the spectrum of caffeine becomes flat, when seen under
UV-visible spectrometer. In the fifth extraction, the content of caffeine was found
negligible (Atomssa. Tadelech, Gholap. A.V, 2011).
Soxhlet extractions have been replaced in some applications by
microwaveassisted extractions. The process is the same as that described earlier
for microwave digestion. The sample is placed in a sealed digestion vessel along
with the liquid extraction phase, and a microwave oven is used to heat the
extraction mixture. Using a sealed digestion vessel allows the extraction to take
place at a higher temperature and pressure, thereby reducing the amount of time
needed for a quantitative extraction. In a Soxhlet extraction the temperature is
limited by the solvent’s boiling point at atmospheric pressure. For example, when
acetone is the solvent, a Soxhlet extraction is limited to 56 °C. With a microwave-
assisted extraction, however, a temperature of over 150 °C can be obtained when
using acetone as the solvent. Two other examples of a continuous extraction
deserve mention (David. Harvey, 2000 : 214).
D. APPARATUS AND CHEMICALS
1. Apparatus
a) Soxhlet and complementar (1 piece)
b) Porcelain cup (1 piece)
c) Analytical balance (1 piece)
d) Beaker glass 500 mL (1 piece)
e) Beaker glass 250 mL (1 piece)
f) Beaker glass 100 mL (2 pieces)
g) Funnel (1 piece)
h) Graduated cylinder 50 mL (1 piece)
i) Statif and clamps (1 piece)
m) Wood clamps (3 pieces)
n) Bottle spray (1 piece)
o) Stir bar (1 piece)
s) Tripod and asbestos gauze (@1 unit)
t)Rough and smooth rags (@1 piece)
u) Separated funnel (1 piece)
v) Heating mantel (1 piece)
w) Evaporating disk (1 piece)
x) Hot plate (1 piece)
2. Chemicals
a) Ethanol (C2H6O)
b) Sulfuric acid (H2SO4)
c) Chloroform (CHCl3)
d) Magnesium oxide (MgO)
e) Aquadest (H2O)
f) Tea samples
g) Whatmann filter paper
h) Matches
i) Capillary Pipes
j) Tissue
E. WORK PROSEDURE
1. 20,5 gram of sample (tea) has wrapped with filter paper it’s entered into soxlet
with use ethanol as solvent.
2. The solution it’s heated in heating mantle and the circulation it’s set until 6
times.
3. The solution thas has been obtained, pured into porcelain crus and 17,5 gram of
MgO dissolved in 75 mL of water.
4. The mixture evaporated in a water bath until dry.
5. The powder extracted with 125 mL of hot water, and filtered on funnel at hot
condition
6. The observation repeated 3 times with hot water as much as 100 mL.
7. The collected binary solution put in one beaker.
8. 25 mL of H2SO4 added to the solution.
9. The solution evaporated until stay 1/3 of first volume.
10. The solution filtered if there are precipitation.
11. The solution extracted in separation funnel with 15 mL chloroform as much as
5 times.
12. Evaporated the chloroform solution.
13. Recrystallize if the crystal have form.
14. Weighted the crystal of caffeine.
15. Tested the melting point of crystal caffeine.
F. OBSERVATION RESULT

No. Activity Observation

1. Tea samples in weigh Mass tea = 20,50 gram
2. Sample of tea in paper wrapper and extracted + The solution is

C2H5OH yellowish brown

3. In the heat on the water bath, and in the The solution is

circulation as much as 6 times. yellowish brown

40 Solution + suspension 17,5 grams of MgO in The solution is solid

100 mL air green

G. DISCUSSION
Percobaan ini, bertujuan untuk mengenal ekstraksi kontinyu dengan
perantaraan panas. Pada percobaan ini sampel yang di gunakan adalah teh, dimana
percobaan ini yang ingin diperoleh adalah kristal kafein yang terkandung dalam
teh. Kafein merupakan obat yang paling banyak dikonsumsi secara aktif.
Meskipun kafein adalah methylxanthine farmakologis utama dalam kopi dan teh
(Nehlig. Astrid, 2004 : 1).
Sampel teh di ekstraksi secara kontinyu dengan perantaraan panas untuk
memperoleh kafein yang di inginkan. Ekstraksi kontinyu merupakan metode
pemisahan zat dari campurannya dan menggunakan pelarut yang sama di gunakan
secara berulang-ulang. Percobaan ini teh di bungkus dengan kertas saring
kemudian di masukkan ke dalam soxhlet. Pada proses ekstraksi pelarut yang di
gunakan adalah etanol karena etanol memiliki sifat kepolaran yang sama, yaitu
keduanya bersifat polar dan bila di tinjau dari titik didih etenol yang rendah yaitu
78,37oC di banding kafein 235oC, sehingga etanol lebih mudah menguap. Karena
prinsip kerja dari ekstraksi yaitu menggunakan pelarut yang sesuai dengan zat
yang akan di ekstraksi, sehingga etanol dan kafein bisa saling melarutkan.
Sebelum melakukan ekstraksi, terlebih dahulu di tambahkan batu didih agar pada
saat pemanasan tidak terjadi letupan-letupan pada labu bundar.
Percobaan ini menggunakan cara sokletasi untuk melakukan ekstraksi
karena sokletasi mempunyai kelebihan di antaranya waktu untuk mengekstraksi
lebih cepat, ekstraksinya lebih sempurna karena di gunakan penyaringan secara
kontinyu. Dimana alat yang digunakan adalah soxhlet, prinsip kerja dari alat ini
yaitu pemisahan komponen zat dalam sampel yang menggunakan pelarut yang
sesuai yang terjadi berulang kali (kontinyu).
Percobaan ini menggunakan cara sokletasi untuk melakukan ekstraksi
karena sokletasi mempunyai kelebihan di antaranya waktu untuk mengekstraksi
lebih cepat, ekstraksinya lebih sempurna karena di gunakan penyaringan secara
kontinyu. Dimana alat yang digunakan adalah soxhlet, prinsip kerja dari alat ini
yaitu pemisahan komponen zat dalam sampel yang menggunakan pelarut yang
sesuai yang terjadi berulang kali (kontinyu).
Percobaan ini di lakukan pengsirkulasian sebanyak 6 kali dimana larutan
dan sampel di sirkulasi sebanyak 6 kali. Dimana fungsi dari perlakuan ini yaitu
agar kafein yang terikat oleh etanol lebih banyak. Dan menghasilkan larutan
berwarna coklat kekuningan. Kemudian dilanjutkan dengan larutan di tambah
dengan suspensi MgO dalam air. MgO berfungsi mengikat zat lain selain kafein,
dimana pada proses penguapan nanti kafein tidak terikut menguap dengan etanol.
Larutan yang dihasilkan adalah larutan berwarna hijau pekat. Warna yang
dihasilkan setelah penambahan suspense MgO yang seharusnya menghasilkan
warna cokelat berbeda dengan yang dihasilkan pada proses percobaan. Hal itu
terjadi disebabkan penyimpanan larutan setelah proses sokletasi yang kemudian
disimpan didalam oven dengan waktu penyimpanan selama 2 hari tanpa
melanjutkan proses setelahnya.
 Ketika larutan hendak diuapkan, terjadi letupan-letupan pada proses
pemanasan. Dan seketika larutan yang diuapkan tadi terbakar karena temperature
pada pembakaran naik. Percobaan inipun gagal karena berakhir pada sebuah
ledakan. . Adapun reaksinya yaitu :
CH3
H H3C
- N O N
N N
+ 2C2H6OH
- - -
N N N N
(etanol) O

O CH3
CH3
H3C H3C
O N N
N N 2+
+ MgO + Mg
- - N
N N O N
O (Magnesium
Oksida)

G. Conclusion
From the experimental results that caffeine can be obtained by extracting
continuously by the medium of heat on the tea sample. In this experiment not
obtained crystal crystal and only to the extent of adding suspension to the results
of the socletation solution.
H. Suggestion
It is hoped that the next practitioner will know more about the way of
caffeine extraction experiments because of the lack of knowledge of the treatment
and the way these experiments work, many of which perform unsuccessful
caffeine extraction experiments.
 BIBLIOGRAPHY

Atomssa. T., Gholap. A. V., 2011, African Journal of Pure and Applied
Chemistry, Characterization of Caffeine and determination of caffeine in
tea leaves using uv-visible spectrometer, Vol. 5(1), pp. 1-8, ISSN 1996-
0840.

Crozier. Alan, 2012, Teas, Cocoa and Coffee, India : Blackwell Publishing Ltd.

Flament. Ivon, 2002, Coffee Flavor Chemistry, USA : John Wiley & Sons, Ltd.

Harvey. David, 2000, Modern Analytical Chemistry, America : The McGraw-Hill

Companies, Inc.

Marcus. Y, Sengupta. A. K, 2002, Ion Exchange and Solvent Extration, USA :

Marcel Dekker, Inc.
 ANSWER OF THE QUESTION

1. Structure of Caffeine (C8H10O2N4)

O CH3
H3C N
N
N
O N
H3C

Picture Structure of Caffeine

2. Ethanol is used as a solvent in caffeine extraction because ethanol has the same
properties as caffeine (polar). And the working principle of the extraction is to
use a solvent that is in accordance with the substance to be extracted. So that
ethanol and caffeine can dissolve twice as much each other so that extraction of
caffeine can be more and ethanol also has a lower boiling point than water so it
is more volatile.
3. Caffeine melting points are also used to determine the purity of caffeine
compounds because the purity of a substance is determined by a sharp melting
point. In addition to the melting point can know whether the substance yan
obtained is caffeine.