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ANALYTICAL CHEMISTRY II LABORATORY WORK REPORT


EXPERIMENT VIII
VAPOR DISTILLATION

Name of Apprentice
Students Number
Study Program
Education
Group

: Retnani Arum Pertiwi


: 13303241060
International
Chemistry
:3

Date of Laboratoy Work

: October,

12th

2015

Date of Report Collection

: October,

19th

2015

ANALYTICAL CHEMISTRY LABORATORY


DEPARTMENT OF CHEMISTRY EDUCATION
FACULTY OF MATHEMATICS AND NATURAL SCIENCES
YOGYAKARTA STATE UNIVERSITY
2015

VAPOR DISTILLATION
A. OBJECTIVE
1. After doing this experiment, practitioners are expected to have skills in separating
an organic compound in a sample.
B. THEORETICAL BACKGROUND
In simple distillation, steam mixture is taken and condensation entirely, droplets of a
liquid composition contains more essential oils of the original fluid. The distillation process
consists of two parts, the first part consists of the condensed steam is called distillate, and the
second part is called the residual liquid left, the structure more difficult components
evaporate. (Atkins, 1999)
The general way to describe the results of distillate is to describe the curve distillate,
wherein the composition, the boiling point or other physical properties of distillate described
the percent or amount of distillate. (Anwar, 1994)
Distillation is a joint process between the heating and cooling of the steam that is
formed in order to obtain pure liquid back. In the heating fluid is usually added boiling stones
(boililng chips), to prevent sudden boiling (bumping). Boiling stones are porous need to be
replaced every time you perform a distillation back. For vacuum distillation (vacuum
destilation), the flow of air through the capillary into the bottom of the pumpkin is the
replacement of stone boiling. (Basset, 1983)
Distillation is the separation of components in a solution based on the distribution of
substances in the gas phase and liquid phase by using differences in the volatility of the
components are quite large. Mass transfer of oil in granular solids to solvent include two
serial processes, namely diffusion in solids to the surface of the granules and mass transfer
from the solid surface into the solvent. If one process go faster, the speed of the mass transfer
controlled by a slower process. (Sutijan, 2009: 69-73)
The basic principle in the process of distillation is based on differences in boiling
point, the compound with the lowest boiling point will be separated first. Cooling water
entered from the end closest to the adapter, and the water comes out through the other end of
the coolant. Thermometer mounted in such a way so as to demonstrate the boiling point
compounds were separated. The tip of the thermometer is placed exactly at the position of the
tip of the cooler. (Khamidinal, 2009: 137)

Distillation method commonly used in the production of essential oil is steam distilled
water and distilled water. Because the method is a method that is simple and requires a lower
cost when compared to steam distillation. However, no studies on the effect of the two
methods of distillation of the essential oil is produced. Essential oils in aromatic plants
covered by the oil glands, vessels, oil sacs or granular hair. Before being processed,
preferably chopped plant material (reduced in size) in advance. But in the traditional
distillation process is generally the size of the material used is not uniform, because the
diminution in size only by the destruction process is simple. (Yuliarto, 2012: 12-23)
The main requirement of separation of liquid mixtures by distillation are all the
components contained in the mixture should be volatile. At the same temperature, the
evaporation rate of each component will vary. This means that at a certain temperature, the
more volatile components in the liquid mixture will generate more steam. Such properties
would occur otherwise, which is at a certain temperature the liquid phase will often contain
compounds that are less volatile. So fluid equilibrium with its vapor at a certain temperature
has a different composition. Differences in the composition of the vapor-liquid equilibrium
can be easily learned on the separation of a mixture of alcohol distillation of water. (Alimin,
2007: 36)
The distillation process at a certain temperature, the vapor liquid equilibrium has a
different composition. Steam is always more to contain more volatile components as well as
the other way around. At different temperatures the liquid vapor composition will be
different. Thus, the composition of the vapor equilibrium with the liquid will change in line
with changes in temperature. (Alimin, 2007: 39)
Distillation diffusion speed is influenced by several factors, including the composition
of materials in the boiler, temperature and vapor pressure, density and moisture content of the
material, as well as the molecular weight of chemical components in a sample. (Sutijan,
2009: 69-73)
Efforts to improve the performance of steam distillation has been carried out. Intrinsic
(2007) using the boiler berpenghalang to extend the contact time of the steam with leaf
clovers. Existence of contact time that is better shown to reduce significantly the time
distillation .. Installation barrier (baffles) in the kettle will cause trouble when inserting and
removing leaf clovers. The use of pressure to raise the boiling point of water led to the
increase in equipment cost of having to use equipment which is thicker in order to withstand
the pressure. (Sutijan, 2009: 69-73)

One way to speed up the time of distillation is to accelerate the process of mass
transfer of oil from the leaves to the separating agent (steam). Essential oil distillation speed
is generally controlled by the speed of diffusion of molecules of essential oils in the water
within the tissue cells leaves or twigs of a substance. One way to accelerate the speed of
diffusion of mass transfer is to increase the temperature of the system (usually with water
vapor). Steam temperature can be increased by utilizing the relationship vapor pressure of a
solution to the boiling point. Distillation using a high-temperature steam at atmospheric
pressure is called the Super Steam Distillation. In this study, high-temperature saturated
steam is obtained by evaporating the water-glycerol mixture. (Sutijan, 2009: 69-73)

C. APPARATUS AND MATERIALS


1. Apparatus
a. Vapor generator flask

2. Materials
a. Lemongrass
b. Aquades
c. Vaseline

b. Distillation flask

c. Leibig cooler

d. Hose connector

e. Erlenmeryer

f. Electric stove

g. Adaptor

h. Separatory funnel

i. Flask plug

j. Aluminium foil

D. PROCEDURE
E. RO
Aquades
F.
sufficiently
G.
Placed into

Lemongrass leaves
that have been cut
Placed into
Distillation flask

Vapor generator flask

String the steam distillations apparatus

Completed with

Condensor

Turned on
Tap water

Electric stove

Aquades

Filled witth

Erlenmeyer
Produced
Distillate
Placed into
Separatory funnel

Aquades

E. EXPERIMENT SET UP

Lemongrass leaves
oil

Weighed using

Analytical
balance

Stative and clamp


Distillation flask
Water in

Water out

adaptor

Leibig cooler

Vapor generator flask

Erlenmeyer

Erlenmeyer
Electric stove
Explanation :
1. Stative and clamp : as a clamp and buffer.
2. Electic stove : to heat the vapor generator flask.
3. Vapor generator flask : to produce vapor in the vapor distillation process.
4. Adaptor : to a condensor funnel from distillate before come into the container.
5. Distillation flask : to place the material that will be didtillated.
6. Leibig cooler : to freeze the vapor.
7. Erlenmeyer : as a container of distillate.
8. Water in : place for water in.
9. Water out : place for water out.
10. Connector hose : as a connector between one componenet and other
component to stream the product of distillation.
11.

F. RESULT
Mass of lemongrass leaves = 16,955 gram.
Mass of empty erlenmeyer = 169,69 gram
Mass of erlenmeyer+lemongrass oil = 0 gram
Mass of lemongrass oil = 0 gram
G. CALCULATION
mass of lemongrass oil
Randemen = mass of lemongrass initially
=

100

0 gram
100
16,955 gram

=0%

H. DISCUSSION
The experiment titled Vapor Distilation was conducted on Monday, October
12th 2015 in Analytical Laboratory, Chemistry Education of Yogyakarta State
University. The objective of this experiment is practitioners are expected to have skills
in separating an organic compound in a sample. In this experiment, we separated the
lemongrass leaves to produce lemongrass oil by distillation process.
According to Sunarto, distillation is a method that used to separate two or
more components of the liquid substance based on boiling point difference.
Distillation is the separation of components in a solution based on the distribution of
substances in the gas phase and liquid phase by using differences in the volatility of
the components are quite large. Mass transfer of oil in granular solids to solvent
include two serial processes, namely diffusion in solids to the surface of the granules
and mass transfer from the solid surface into the solvent. If one process go faster, the
speed of the mass transfer controlled by a slower process.
Vapor distillation process mainly used for taking an essential oil from the
natural materials. Essential oil also known as aetheris oil or aromatic oil is a large
group of vegetable oil that form in viscous liquid in room temperature, but easily
volatile so it will give a specific odor. Essential oil is raw materials for making
perfume or natural balm. trade, essential oils commonly known as seeds of perfume.
Essential oil has volatile characteristic because the vapor pressure is low. Besides, the
arrangement of the component compounds strongly affect the nerves of the human so

often creates a certain psychological effect. Mostly, essential oil is including in the
group of organic compound, terpeine and terpenoide that dissolve in the oil.
Lemongrass oil from Java are contain componentas followed:
Sitronelal 32-45%, geraniol 12-18%, sitronelol 11-15%, beranil acetate 3-8%,
sitronelil acetate 3-4%, sitral, khavikol, Eugend, elenol, kadinol, kadinen, vanilin,
limonen and kamfen. The main component of lemongrass oil are : sitronelal,
sitronelol, and geraniol also ester compound from geraniol and sitronelol. These
compounds are the raw mateials which is used in perfume, and pharmacy product.
In this experiment, lemongrass leaves that will be used must be cut into small
pieces. This is done in order to extend the surface of lemongrass leaves so the process
will occur faster. Then, the lemongrass leaves that already cut into small pieces is
placed into the distillation flask that heve been connected with vapor generator flask
and other string. Vapor generator flask is filled with aquades and connected with
heater (electric stove) so the water vapor that produced will stream come into
distillation flask that filled with piece of lemongrass leaves. It purpose is to decrease
the boiling point of compounds, because the boiling point of mixture is lower than the
boiling point of its component. The vapor will bind the lemongrass oil and will
strream passed through the Leibig cooler and then condensed and then drop to the
erlenmeyer. Erlemnmeyer should filled with the lemongrass oil and aquades which
then will be separated using separatory funnel. But in this experimenet, when we
placed the distillate into separatory funnel, there is no separated layer, the erlenmeyer
only contain one layer of aquades, so the separation process cant be done.
From this eperiment, mass of the lemongrass leaves that used is 16,955 grams.
Mass of empty erlenmeyer is 169,69 grams and mass of the lemongrass oil cannot be
obtained because in the erlenmeyer only contain aquades. The mass of lemongrass oil
can be calculated with formula =
Mass of lemongrass oil = (mass of erlenmeyer+distillate) mass of empty erlenmeyer
Because in this experiment didnt produce the distillate that contain the lemongrass
oil, the mass of lemongrass oil cant be obtained.
The rendement can be calculation can be calculated using formula=
mass of lemongrass oil
100
Randemen = mass of lemongrass initially
The calculation resulted the rendement 0%. The amount of randement is very small
and reached 0%, it may be caused by several factor, such as :
1. The small amount of lemongrass leaves that used in the experiment. The
lemongrass leaves that used in the vapor distillation must be in a large amount.

The lemongrass leaves must filled all the space in the distillation flask. The
larger amount of lemongrass leaves, the larger amount of lemongrass oil that
will be produced.
2. The distillation process only carried out in about 80 minutes. It may caused
the process didnt conduct perfectly. From the litelature, distillation proses
must be conducted about 4-5 hours to produce the larger amount of product.
3. There is a byproduct of water vapor that amount is greater than the amount of
expected product. The volume of liquid in the erlenmeyer is gain up, but when
it placed in the separatory funnel it didnt perform the separated layer. In other
word it only produced one layer of aquades.
For, the next experiment about vapor distillation, if expected to get rendement
in big quantity, it is better if the distillation process is carried on more than in
70 minutes and make sure the pieces of lemongrass leaves filled all the space
in distillation flask.

I. CONCLUSION
Based on the experiment we can conclude that :
Vapor distillation can be used to purify process and isolation compound from natural
material. Especially to produce essential oil. In this experiment has already separated
lemongrass oil from lemongrass leaves by using vapor distillation method which
produce the mass of lemongrass oil is 0 gram and the rendement is 0%.

J. ASSIGNMENT
1. Calculate the rendement of lemongrass oil from distillation:

Randemen =

mass of lemongrass oil


mass of lemongrass initially
=

100

0 gram
100
16,955 gram

=0%
H. REFERENCES
Alimin, dkk. Kimia Analitik. 2007. Makassar: Alauddin Press.
Anwar, C. 1994. Pengantar Praktikum Kimia Organik I. Yogyakarta : UGM Press.
Atkins. 1999. Kimia Fisika. Jakarta: Erlangga.
Basset. 1983. Vogels Text Book of Quantitative Inorganic Analysis 4th ed. London:
Longman Inc.
Khamidinal. 2009. Teknik Laboratorium Kimia. Yogyakarta: Pustaka Pelajar.
Sunarta, dkk. 2006. Petunjuk Praktikum Kimia Analisis II. Yogyakarta: FMIPA
UNY.
Sujtijan, dkk. Pengaruh Perlakuan Daun dan Suhu Terhadap Waktu Destilasi pada
Isolasi Minyak Cengkeh Menggunakan Super Steam Distillation. Jurnal
Teknik Kimia Indonesia. Vol. 8 No. 2 (Agustus 2009). Hal. 69-73.
Yulianto Fuki Tri, dkk. Pengaruh Ukuran Bahan dan Metode Destilasi (Destilasi Air
dan Destilasi Uap-Air) Terhadap Kualitas Minyak Atsiri Kulit Kayu Manis
(Cinnamon Burmanni). Jurnal Teknosains Pangan. Vol. 1 No.1 (Oktober
2012). Hal 12-23.