A.

Title of Experiment
Caffeine Extraction
B. Objective of Experiment
The objective of this experiment is regarding the continuous extraction by
root method.
C. Literature Review
Extraction is one of the most important techniques for isolating and
purifying organic substances. In this method, a solution is mixed thoroughly with
a second solvent that is immiscible with the first solvent. The solute is extracted
from one solvent into the other because it is more soluble in the second solvent
than in the first. Extraction is not only a technique used by organic chemists but it
is also used to produce common products with which you are familiar. For
example, vanilla extract, the popular flavoring agent, was originally extracted
from vanilla beans using alcohol as the organic solvent (Pavia, 2013: 34).
Extraction is a method used for the separation of organic compound from a
mixture of compound. This technique selectively dissolves one or more
compounds into an appropriate solvent. The solution of these dissolved
compounds is referred to as the extract. In the case of Caffeine extraction from tea
powder, the solubility of caffeine in water is 22mg/ml at 25°C, 180mg/ml at 80°C,
and 670mg/ml at 100°C. Here the organic solvent Dichloromethane is used to
extract caffeine from aqueous extract of tea powder because caffeine is more
soluble in dichloromethane (140mg/ml) than it is in water (22mg/ml).The
dichloromethane - caffeine mixture can then be separated on the basis of the
different densities of dichloromethane and water because dichloromethane is
much denser than water and insoluble in it. Residual water is separated from
dichloromethane by drain out the dichloromethane through separating funnel, thus
dichloromethane passed through the funnel while polar solvents such as water is
still remaining in the funnel (Chaugule, 2019:13).
Caffeine is one of the xanthine derivatives found in tea, coffee and
chocolate, has the formula C8H10O2N4. From the research results, it was found that
tea contains more caffeine than coffee. The structure of caffeine is as follows:
 (Lecturer Team, 2020: 15).
The constituent elements of the alkaloids carbon, hydrogen, nitrogen and
oxygen. There are only a few alkaloids whose chemical structure does not contain
oxygen. There are also alkaloids containing other elements of the four elements
that have been mentioned. The presence of nitrogen in the alkaloid chemistry
makes the alkalodies alkaline. Therefore, this class of compounds is called
alkaloids. Dicot plants are a major source of alkaloids. The extraction method is
used to get alkaloids from plants. Now, several alkaloids with simple chemical
structures can be synthesized in the laboratory. Several means have been used to
identify alkaloids, eg crystal microscopy, solubility in various types of solvents,
absorption and optical cycling spectra or their pharmacological properties. Color
reactions are also used although they are not specific (Sumardjo, 2006:438).
The amount of caffeine in plants can be built up by several factors,
including the growing area, plant varieties, plant age, leaf age, length of the
growing season, field conditions, soil nutrients, rainfall, and pests. However, the
caffeine content in tea is more than the production system, as carbon dioxide in
free air can also affect caffeine levels in tea leaves. (Putri, 2015:107).
Caffeine from tea is extracted by liquid-liquid extraction followed by
recrystallization. Caffeine is the most commonly used psychoactive drug in the
world. It is a pharmacological active substance and depending on the dose, can be
a mild central nervous system stimulant. The purified caffeine is then analyzed by
using high performance liquid chromatography or Iodometric back titration
method. The serious concern about potential use of caffeine for pathogenic effects
has made it one of the most broadly studied drugs (Chaugule, 2019:18).
Industrial applications of Caffeine (a) The caffeine so extracted can be
further converted into items that we enjoy in our everyday lives - sodas, cosmetics
& pharmaceutical products. (b) Diet pills and cosmetic companies are the largest
consumers of caffeine. (c) It can also be used in manufacturing body wash, soap,
lip-balm, facial scrub and several other products such as caffeine lipstick. (d) It is
also used with painkillers for simple headaches and preventing and treating
headaches after epidural anesthesia (Shinde, 2017:2370).
Historically, the Wiley and the Underwriters Laboratories continuous
extractors arranged for the sample in a porous container to be bathed in the reflux-
condensed vapour before it percolated back into the boiling flask, carrying soluble
substances with it.Therefore, these methods suited the extraction of stable solutes
only, and other methods were sought to avoid labile analytes spending long
periods of time in the boiling solvent in the flask. The intermittent Soxhlet
extractor was designed to extract solutes with the solvent at the condenser cooling
water temperature rather than at its boiling point. The boiling flask is of the
Erlenmeyer type and the reflux condenser is either the Allihn (a), an efficient
large surface area design, or a cold finger Hopkins (Self, 2005:175-176).
One of the most common extraction procedures involves using an organic
solvent (nonpolar or slightly polar) to extract an organic compound from an
aqueous solution. Because water is highly polar, the mixture will separate into two
layers, or phases: an aqueous layer and an organic (nonpolar) layer. After each
extraction, you will remove the organic layer. The organic layers from all three
extractions will be combined and dried over anhydrous sodium sulfate. After
transferring the dried solution to a preweighed container, you will evaporate the
methylene chloride and determine the weight of caffeine extracted from the
aqueous solution. This extraction procedure succeeds because caffeine is much
more soluble in methylene chloride than in water (Pavia, 2013: 35).
D. Apparatus and Chemicals
1. Apparatus
a. Soxhlet (1 unit)
b. Analytical balance (1 piece)
c. Erlenmeyer (2 pieces)
d. Beaker glass (2 pieces)
e. Graduated cylinder (1 piece)
f. Buchner funnel (1 piece)
g. Funnel (2 pieces)
h. Separation funnel (1 piece)
i. Porcelain Crucible (2 pieces)
j. Hotplate (1 piece)
k. Round flask (1 piece)
l. Stirrer (2 pieces)
m. Drop pipette (1 piece)
n. Clamp (2 pieces)
o. Spritus (2 pieces)
p. Watch glass (1 piece)
q. Tripod and asbestos gauze (2 pieces)
2. Chemicals
a. Tea
b. Ethanol (C2H5OH)
c. Magnesium oxide (MgO)
d. Sulfuric acid (H2SO4)
e. Chloroform (CHCl3¬)
f. Aquadest (H2SO4)
g. Filter paper
h. Boiling stone
i. Ice cube
j. Tissue
E. Work Procedure
1. 20 grams of tea was wighed
2. The tea was wrapped using filter paper
3. The bundle was put in the soxhlet
4. 250 mL of ethanol was added in to the soxhlet
5. The soxhletation process was carried out until 4 circulation (total time was
total time 44.84 minutes)
6. 15 grams of MgO was added 150 mL of aquadest
7. MgO suspension was added in to the solution from soxhletation process
8. The mixture was heated using porcelain crucible until form powder
9. The powder was extracted with hot water (2 times)
10. 50mL of H2SO4 was added in to the extract solution
11. Filter process was carried out
12. The mixture was heated
13. The mixture was chilled
14. The mixture was extracted with 25 mL of chloroform (3 times)
15. The bottom layer of seperation process was taken and heated
16. The crystal was weighed
F. Observation Result
No. Activity Result
1. The tea was weighted 20 grams
2. The tea was wrapped using filter paper The tea is bundle
3. The bundle was put in the soxhlet The bundle was in the soxhlet
4. Ethanol was added into the soxlet 250 ml
5. The Soxhlet process was carried Brown solution
Circulation I: 14.03 minutes
Circulation II: 10.08 minutes
Circulation III: 10.34 minutes
Circulation IV: 10.39 minutes
6. 15 grams of MgO was added 150 ml MgO suspension
 of aquadest
7. MgO suspension was added into the Brown solution
solution from soxhletation process
8. The powder was extrated with hot 550 ml of Soxhlet solution
water
9. H2SO4 was added into the extracted 125 ml, light brow solution
solution
10. Filter process was carried out Brown reddish solution
11. The mixture was heated Brown reddish solution
12. The mixture was chilled The mixture chill
13. The mixture was filtered Light brown reddish
14. The mixture was extracted with Upper layer : light brown
chloroform 25 ml Bottom layer : colorless
15. The mixture was heated Crystal caffeine
16. Weight the crystal 0,2 gram
17. Determination melting point 190 – 200oC

G. Data analysis
Known : Weight the sample = 20 gram
Weight of crystal = 0,2 gram
Ask : %Yield = ...?
Settlement :
(Weight of crystal)
%Yield) = x 100%
(Weight of sample)
(0,2 gram)
%Yield = = ) x 100%
(20 gram)
%Yield = 4%

H. Discussion
Eksperimen ekstrak kafein ini bertujuan untuk mengenal ektraksi
kontinyu dengan perantaraan panas. Sampel yang digunakan dalam percobaan ini
ialah teh. Ekstraksi adalah pemisahan suatu zat dari campurannya dengan
pembagian sebuah zat terlarut antara dua pelarut yang tidak dapat tercampur
untuk mengambil zat terlarut tersebut dari satu pelarut ke pelarut yang lain.
Ekstrasi yang digunakan dalam percobaan ini yaitu ekstraksi padat cair yang
bertujuan untuk mengekstraksi zat padat menggunakan zat cair. Prinsip ekstraksi
yang digunakan yaitu ekstraksi kontinyu melalui perantaraan panas, artinya
ekstraksi ini dilakukan secara berulang (lebih dari satu kali) dengan
menggunakan energi panas sebagai sumber energy dalam mengekstraksi. Adapun
prinsip kerja dalam percobaan ini yaitu Adapun prinsip kerjanya yaitu
penimbangan, pemanasan, penguapan, pengembunan, penyaringan, pemisahan,
dan pengujian titik leleh.

Percobaan ini praktikan menimbang 20 gram teh yang kemudian teh

dibungkus dengan kertas saring Whatman dan diikat dengan benang yang
berfungsi untuk menguatkan kertas saring agar sampel tidak tumpah, dimana
ikatannya disini tidak terlalu kuat. Hal ini bertujuan agar kafein yang ada dalam
teh dapat terekstrak secara maksimal. Kemudian diekstraksi dengan
menggunakan pelarut etanol. Penggunaan etanol juga disebabkan oleh sifat basa
dari kafein dapat mudah larut dalam etanol yang bersifat asam. Sirkulasi yang
terjadi pada pemanasan tidak teratur, hal ini disebabkan karena suhu pada
sirkulasi pertama masih rendah sehingga tekanan yang memungkinkan terjadinya
sirkulasi yang terakhir. Pada proses ekstraksi di masukkan beberapa butir batu
didih agar pada saat pemanasan tidak terjadi letupan–letupan pada labu

Percobaan ini digunakan cara sokletasi untuk melakukan ekstraksi karena

sokletasi mempunyai kelebihan diantaranya waktu untuk mengekstraksi lebih
cepat. Prinsip dari sokletasi adalah perendaman bahan yang diakstraksi melalui
pengaliran ulang secara kontinyu sehingga bahan yang diekstraksi melalui aliran
bahan pelarut melintasi bahan yang akan diekstraksi secara kontinyu. Pada
percobaan ini dilakukan 4 kali sirkulasi yang bertujuan agar kafein yang diperoleh
nantinya betul-betul terpisah dari sampel campuran. Pada proses sirkulasi di
masukkan beberapa butir batu didih agar pada saat pemanasan tidak terjadi
letupan–letupan pada labu. Sehingga pada sirkulasi ini diperoleh ekstrak kafein
yang berwarna coklat.

Larutan yang diperoleh kemudian di tambahkan suspensi dari 15 gram

MgO dalam 110 ml aquadest. Fungsi MgO yaitu untuk mengikat zat zat dalam
ekstraksi sehingga kafein tidak terganggu. Proses penguapan menggunakan cawan
porselin. Tujuan penggunaan cawan porselin adalah untuk menguapkan campuran
dalam suhu tinggi. Setelah diuapkan maka terbentuk powder berwarna coklat
gelap. Campuaran yang menjadi padat ini menandakan bahwa etanol sudah
menguap seluruhnya.

Powder yang telah dihasilkan tadi kemudian diekstraksi dengan air panas.
Fungsi dari air panas untuk mempercepat terjadinya pemisahan kafein, kemudian
disaring panas – panas dengan corong. Hal ini dilakukan untuk menyaring
endapan pada campuran dan menyaring kotoran-kotoran yang ukuran kecil. Filtrat
yang diperoleh ditambahkan dengan asam sulfat encer. Penambahan H2SO4 encer
didasarkan pada kafein yang mengandung alkaloid yang merupakan basa organik,
sehingga cara pengambilan kafein yang maksimal maka digunakan H 2SO4 karena
pHnya dapat stabil dengan H2SO4. Sehingga akan dapat terpisah zat yang
dibutuhan yaitu kafein dan akan pula melepaskan zat-zat pengotornya. Setelah
penambahan H2SO4. Larutan lalu diuapkan untuk memekatkan larutan tadi dan
menguapkan air yang terdapat pada larutan tersebut. Larutan diuapkan hingga 1/3
larutan semula. Larutan yang diperoleh berwarna cokelat.
Larutan kemudian diekstraksi dengan kloroform. Fungsi dari kloroform
adalah sebagi pengikat kafein yang terdapat dalam larutan. Dalam corong pisah
larutan yang ditambahkan dengan kloroform akan terpisah Karena kloroform
bersifat non polar. Corong pisah berfungsi untuk mendistribusikan kafein dari fasa
air ke fasa kloroform. Setelah itu, larutan di kocok dan di diamkan hingga
terbentuk dua lapisan yaitu lapisan atas (air dan kafein). Berat jenis air adalah 1
gram/cm3 dan lapisan bawah (kloroform) Berat jenisnya yaitu 1,48 gram/cm3.
Lapisan bawah di buang dan lapisan atas di ekstraksi. Adapun mekanisme
reaksinya yaitu:
 Kristal yang dihasilkan berwarna kuning dengan berat 0,2 gram. Tahapan
selanjutanya seharusnya dilakukan uji titik leleh, yang dimana menghasilkan suhu
190 – 200oC. titik leleh yang diperoleh tidak terpaut jauh dengan teori dimana
dalam teori menyatakan bahwa kafein yang tidak mengandung air kristalna
mencair pada suhu 238oC.
I. Conclusions and Suggestion
1. Conclusions
From this experiment we can conclude that caffeine can be obtained from
continue extraction with heat intercession through the tea. In this experiment,
the caffeine crystals obtained from the tea sample were 0.2 grams with a yield
of 4%.
2. Suggestion
 As the suggestion for the next experiment is the apprentice used to be
master by doing extraction and also should really master the theory and the
work procedure in order that to reduce the mistaken and the result that we
obtained is better
 BIBLIOGRAPHY

Chaugule, Aniket. 2019.Extraction of Caffeine. International Journal of

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Pavia, Donald L. et al. 2013. A Microscale Approach To Organic Laboratory

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Putri,Dianita Devi and Ita Ulfin. 2015. Pengaruh Suhu dan Waktu Extraksi
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No. 2,ISSN: 2337-520

Self, R. 2005.Extraction of organic analytes from foods. UK. The royal society of
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Shinde,Ms.R.R. 2017. Extraction of Caffeine From Coffe And Preparation of

Anacin Drug. International Journal Of Engineering Research And
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Sumardjo, Damin. 2006. Pengantar kuliah. Jakarta. EGC