SEPARATION METHOD
SOLID-LIQUID EXTRACTION
Created
by:
Putu Ayu Swarni (1113031072)
Ni Luh Gede Enik Karnila Yanti (1113031079)
A.A. Ayu Mirah (111303107)
Ni Ketut Sepmiarni (111303107)
CHEMISTRY EDUCATION
DEPARTEMENT
FACULTHY OF MATHEMATICS AND
NATURAL SCIENCES
GANESHA UNIVERSITY OF
EDUCATION
SINGARAJA
2012
A. Title
Separate Atsiri Oil from Hazelnuts by using Solid-Liquid Extraction
(Soxhletetion technique ) and Separation Hazelnuts Oil from
n-Hexane by using Simple Distillation
B. Objectives
1. To explain the equipment use in soxhlet extraction
2. To separate atsiri oil from n-hexane by soxhlet
extraction and simple distillation.
3. To know the percentage of extraction at atsiri oil from hazelnuts by using
soxhletation technique.
C. Basic Theory
Extraction is a separation method based on different distribution of
solute between two solvents that are not intermingled. Based on the phase, extraction
can divided into two grouped are extraction liquid-liquid extraction and solid
liquid. Liquid-liquid extraction performed to obtain a compound in the
liquid-phase mixture with another solvent liquid phase. Solid liquid extraction
if you want to separate out the components in a solid by using a liquid
solvent. The tools used were Soxhlet extractor.
Solid liquid extraction techniques soxhletation performed by flowing
solvent to solid samples. The solvent flowed initially heated so evaporate and
subsequently undergo cooling and finally contact with the analyte in the
sample. Solvent will bring the analyte into the reservoir flask, and then the
solvent evaporated again because the heating process. The process takes place
repeatedly so that analyte in the sample to be extracted quantitatively. Soxhletation
extraction technique was performed for analytes readily soluble in hot
temperatures and analyte not decomposes under the influence of heat. For
example, to extract the atsiri oils in hazelnuts.
Distillation is a separation technique mixed in a homogeneous liquid
phase by evaporation and condensation to obtain a relatively more distillate
containing components more volatile than the original solution.
One type of distillation is often used simple distillation, known also
by the name of distillation at atmospheric pressure. Distillation is done on
the separation of mixtures relatively high boiling point and boiling point
difference is quite large components. In this case a lower boiling point will
come out as the first distillate. This technique is used primarily for the
purification of one component in the mixture, such as separation hazelnut oil
from the n-hexane.
To determine the percentage of extraction can use the following formula:
D.
Materials
First Experiment (Soxhletation extraction)
No
|
Name of materials
|
Concentration
|
Amount
|
1
|
Hazelnuts
|
-
|
50 gram
|
2
|
n-hexane
|
-
|
220 mL
|
3
|
Water
|
-
|
sufficient
|
Second Experiment (Simple Destilation)
No
|
Name of materials
|
Concentration
|
Amount
|
1
|
Atsiri
oil in n-hexane
|
-
|
222 mL
|
2
|
Water
|
-
|
sufficient
|
E. Equipment
First Experiment (Soxhletation extraction)
No
|
Name
of equipment
|
Specification
|
Number
|
1
|
Mortal
and portable
|
-
|
1
|
2
|
Erlenmeyer
flask
|
-
|
1
|
3
|
Mantle
heat
|
-
|
1
|
4
|
Beaker
glass
|
250 mL
|
1
|
5
|
Soxhlet
equipment
|
-
|
1 set
|
7
|
Filter paper
|
||
8
|
Statif
|
-
|
1
|
9
|
Clamp
|
-
|
1
|
Second Experiment (Simple Destilation)
No
|
Name
of equipment
|
Specification
|
Number
|
1
|
Erlenmeyer
flask
|
-
|
1
|
2
|
Mantle
heat
|
-
|
1
|
3
|
Beaker
glass
|
250 mL
|
1
|
4
|
Simple
destilation equipment
|
-
|
1 set
|
6
|
Statif
|
-
|
1
|
7
|
Clamp
|
-
|
1
|
8
|
Thermometer
|
-
|
1
|
F.
Procedures
First Experiment (Soxhletation extraction)
1.
Hazelnuts were
pounded by using mortal and portable until softly.
2.
50 gram of hazelnuts
were measured by using electrical balanced
3.
50 gram of hazelnut
were wrapped by using filter paper, at either end the filter paper was tied.
4.
Filter paper
parcel containing a hazelnut was put into tube soxhlet
5.
220 mL of
n-hexane was poured into still pot.
6.
Some of boiling
stones were added into still pot.
7.
The soxhlet extraction equipment was prepared like the
picture bellow:
8.
Cooling water
was flowed, and still pot was heated by using heating mantel.
9.
Extraction was
carried out about 10 times circulation and then the solution was allowed until
cooling.
Second Experiment (Simple Distillation)
1. Mixture of hazelnuts and n-hexane that found from
soxhlet extraction was poured into still pot.
2.
Distillation
equipment was sets like picture bellow:
3.
The Mixture of hazelnut
oil and n-hexane at still pot were putted into mantle heat.
4.
Water was flowed
by hose, there are out water and in water.
5.
Simple
distillation was ready to start with turn on the mantle heat.
6.
Simple
distillation was stopped when n-hexane cannot drip again and the temperature
was observed.
G. Experiment
Result
First Experiment (Soxhletation extraction)
The
result that found at soxhlet extraction are:
-
Mass of hazelnuts : 50 gram
-
Hazelnuts oil that
found : 12 mL
-
The weight of hazelnuts
before extraction: 50 gram
-
The weight of hazelnuts
after extraction: 42.3 gram
-
The weight of the hazelnuts
oil = 9.268 gram
-
During the soxhlet
extraction process, occur 10 times circulation hazelnuts oil by n-hexane.
-
One circulation occur
every
2.54 minutes
Sebelum
Ekstraksi Sokhlet
|
Setelah
Ekstraksi Sokhlet
|
n-hexane have colorless color before use for soxlet
extraction process
 |
n-hexane have yellowiest color after soxhlet
extraction process because was mixed
with atsiri oil from hazelnut
|
Second Experiment (Simple Distillation)
Sebelum
Destilasi Sederhana
|
Setelah
Destilasi Sederhana
|
Terdapat campuran minyak kemiri dengan ether pada labu dasar
bulat.
|
The mixed separated qualitatively at pressure of 65o
C.
|
H.
Disscusion
A Soxhlet extractor is
lab equipment designed for solid-liquid extraction. Based on the experiment
observation, there are some lab equipment uses in soxhlet extractor. It shown
in the picture below:
Note:
1:
Stirrer bar or boiling stone is use to maximize the heat distribution
2:
Still pot is use for the place of solvent (the still pot should not be
overfilled and the volume of solvent in the still pot should be 3 to 4 times
(about 60%) the volume of the soxhlet chamber)
3:
Distillation path is use as the place of the solvent vapor flowing.
4:
Thimble is the place of the solid matter contains liquid that we want to take
out
5:
solid matter contains liquid that we want to take out
6:
Siphon top is the place of the mixture of solvent and the result of extraction
7:
Siphon exit is the canal for flowing mixture to the still pot
8:
Expansion adapter
9:
Condenser is use to condensed the solvent. Condenser has two main-water, the
first (10)Cooling water in and the second (11) Cooling water out.
After observe and doing
solid-liquid extraction, it also can describe the process of solid extraction
as follows: After a few minutes, the
n-hexane in still pot began to boil.
Bubbles arise on
the surface of the n-hexane.
Then, it began to evaporate. Vapor flow toward
to the cooler and then condensed to become liquid
droplets and eventually touch the
filter paper containing the hazelnuts is in the thimble
(soxhlet tube). The hazelnuts must be in the form of fine-grained to
increase the surface area. Essential oils in the hazelnuts are
extracted by n-hexane.
After a mixture of essential oils and n-hexane reach soxhlet tube,
the mixture will be streamed back
into the still pot. The flow of oil is
mixed with n-hexane took place repeatedly. The extraction caused the original color
(colorless) of n-hexane changes to yellowest due to mixed with hazelnuts oil.
The extraction must be
followed by simple distillation to separate the n-hexane from the hazelnuts oil.
First, the mixture is heated. After a while, it forms bubbles and vapor.
n-hexane will vaporize firstly, because it have smaller boiling
point that hazelnuts oil. Steam will flow to Liebig condenser. Then the vapor is condensing
into a liquid and collected in a beaker. Distillate that
we get is n-hexane
and remaining liquid in the flask is a hazelnuts
oils. Qualitatively, simple distillation process
is stopped when the distillate (n-hexane) no
longer dripped from
the distillation apparatus.
N-hexane distillate started dripping when temperatures
showed 65oC. This indicates that the
boiling point of the n-hexane
65oC.
From the data resulted
in the experiment we know that:
The
weight of hazelnuts before extraction: 50 gram
The
weight of hazelnuts after extraction: 42.3
gram
The
weight of the hazelnuts oil = 9.268 gr
So, the extraction percentage is
I.
Conclusion
1.
The equipment use in
soxhlet extraction are: Stirrer bar or boiling stone,
Still pot,
Distillation tube (containing
distillation path, Thimble, Siphon,
Siphon), and Condenser
2.
Through soxhlet
extraction and simple distillation, it was got 12 ml of
from 50 gr hazelnuts
3.
The percentage of
extraction of
is
J.
References
Wiratma, I Gusti Lanang, I Nyoman Selamat dan I Dewa Ketut
Sastrawidana. 2003. Dasar-Dasar Pemisahan
Analitik. Singaraja : IKIP Negeri Singaraja
