Visayas State University

Visca, Baybay City, Leyte, Philippines

Department of Pure and Applied Chemistry
Organic Chemistry 127.2
Laboratory Report

SIMPLE AND STEAM DISTILLATION

Abstract
The objectives of this experiment was to compare and assemble simple and steam
distillation set-ups. It also aimed to purify liquid substances using simple distillation. And lastly,
it also aimed to separate slightly volatile substances from non-volatile substances. Three samples
was subjected to different types of distillation processes to separates each components present in
each sample. Seawater and used ethanol was subjected to two separate simple distillation processes
to separates the components presents in each sample into its pure components. Then, the freshly
cut lemon grass plant was subjected to steam distillation process to separate the essential from the
plant itself. After the distillation processes, the purity of the ethanol was computed and so as with
the percentage yield for the essential oil. Given the parameters obtained in the three distillation of
three samples, it showed that an approximate 90% was the percent purity of the ethanol present in
the used ethanol obtained in the laboratory stock room. Then, the seawater was then separated into
two components; the liquid distillate and white precipitate left in the distillation flask. Furthermore,
the computation for the percent yield of the essential oil resulted to a 1.03%. Then, due to these
results obtained, it could be concluded that even with the errors that were inevitable in the
distillation processes, distillation was still useful in the separation of volatile components, and also
with the synthesis of purer substance which was dependent on the volatility of the components.
INTRODUCTION of vapor even in the body of the liquid. When
the vapor pressure equals to the atmospheric
Distillation is the process of
pressure, boiling occurred (Acabal, et al,
vaporizing a liquid and converting the vapor
2015).
to the liquid state by cooling. Distillation is
commonly used in the biorefinery processing There were type of distillations
of bioethanol production. This adds a namely; simple distillation, steam
significant energy load on the production distillation, fractional distillation and vacuum
process (Atheer, et al, 2016). Volatilization distillation. Fractional distillation is used
of components plays a great part in the when the boiling points of the components of
distillation process. Volatility is defined as a mixture are close to each other, as
the relative ease with which the substance determined to Raoult’s law. Vacuum
passes from the liquid to the gaseous state. distillation is used to separate components
Evaporation is slow volatilization by the that have high boiling points, since lowering
escape of surface molecules from the liquid the pressure of the apparatus also lowers
in to the air while boiling is the fast boiling points (Acabal, et al, 2015).
volatilization of a liquid in which a
In this experiment, the type of
turbulence is observed due to the formation
distillation used was the simple distillation
and the steam distillation. The fundamental Method on separation of pure ethanol and
module of complex multicomponent seawater through simple distillation:
separations by distillations is called the
A 20 mL of used ethanol/seawater
simple distillation. Basically this process
which was placed in a clean 50-mL distilling
involves the rising of the vapor as the result
flask. No liquid was allowed to enter the side
of boiling of the liquid in the still is richer in
arm of the distilling flask. A piece of
more volatile component than the residual
porcelain plate was added to the distillation
liquid. This may be used when the boiling
flask, then the rest of the distillation
points of two liquids are significantly
apparatus was assembled. The tip of the
different from each other or to separate
thermometer bulb was placed in the center of
liquids from solids or nonvolatile
the flask neck, about 5 mm below the side
components. Steam distillation is used to
arm. The connections of the set-up was
separate heat-sensitive components where
checked for tightness and the water on the
steam is added to the mixture causing some
condenser was turned on. Then the flask
of the components to vaporize. This vapor is
containing the sample was heated to boiling,
cooled and condensed into two liquid
with the flame to the condensate falls from
fractions. The fractions are sometimes
the condenser was then adjusted to the rate of
collected separately or they may have
one drop in 5 seconds. When the volume of
different density values causing the fractions
the distillate was 3 mL, the thermometer was
to separate on its own (Acabal, et al, 2015).
checked and so at each succeeding 3 mL
In this experiment, the sample used was the
interval until a total of 15 mL had been
lemon grass with a scientific name of
collected. The boiling range of the sample
cymbopogon citratus to yield essential oil
was the temperature indicated at the first drop
with a water-based distillate.
and the last drop collected, provided that the
MATERIALS AND METHODS distillation had proceeded at a steady rate.
The materials used in the experiment
were porcelain plate, 250 mL separatory
funnel, 50 mL distilling flask, 10 mL
graduated cylinder, spatula, thermometer,
wash bottle, 150 mL Erlenmeyer flask, and
the condenser. A quick-fit macro distillation
set-up was also used which was placed on a
hotplate which was the source of heat.
Different reagents was also used including
the 100 mL sea water which was subjected to
the simple distillation process; lemon grass
which was obtained from Pangasugan, Figure1. Simple distillation set-up
Baybay City, Leyte, Philippines; NaCl solid
which was used during the separation of the Method of separation of essential oil
essential oil and water; and ethanol which through steam distillation:
was also subjected to the simple distillation
About 50 grams of fresh finely cut
process.
lemon grass was weighed. The sample was
mixed with distilled water in the sample The experiment was held at the
flask. Enough water was added such that the Department of Pure and Applied Chemistry
flask was about 2/3 full. The distillation set- laboratory room AC208, Visca, Baybay City,
up was then assembled, making sure that the Leyte, Philippines. It was conducted on
tightness of all the connections was checked. September 24, 2019 and October 15, 2019.
The sample was then heated. About 100 mL
RESULTS AND DISCUSSION
distillate was collected into a 150 mL
Erlenmeyer flask. The separation of the pure ethanol
through subjecting the used ethanol in the
simple distillation process showed that an
approximate of 90% pure ethanol was present
in the used ethanol given the values in table
1.
Table1. Range of temperature per 3 mL
interval of the used ethanol
Volume of distillate
Temperature (ºC)
(mL)
3 78
6 79
9 79
Figure2. Steam distillation set-up 12 79
The observations was then recorded. 15 79.6
After subjecting the sample to the distillation 18 80
process, the distillate obtained from the The temperature of the first drop was
distillation process was then transferred to recorded to be 78ºC which was theoretically
the separatory funnel and was let to stand to within the range of the boiling point of the
separate the oily layer from the aqueous ethanol, the temperature of the succeeding
layer. A spatula of sodium chloride was volume of distillate does not have a drastic
added to the distillate if there was no change but instead, it only differs very
distinction of layers and was gently stirred. slightly in temperature until the last drop. It
The oily layer was then allowed to separate was also observed that due to the porcelain
to the aqueous substance. The oily layer was plate added to the sample, bumping was
then separated from the aqueous layer and avoided.
was placed in a pre-weighed Erlenmeyer On the other hand, the determination
flask/vial. The weight of the oil was of the first drop may had been the source of
determined and the percentage yield was then error in this distillation process since the
computed using the formula: condenser might had contain moisture that
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 (𝑔) may not come from the distillation flask. And
% 𝑦𝑖𝑒𝑙𝑑 = 𝑥 100 as the sample in the distillation flask had
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 (𝑔)
started to vaporize and went to the condenser,
Place and Time: the moisture that was already there was
pushed into the receiving flask and was essential oil. During the distillation process,
identified as the first drop. it was observed that there was no distinct
difference on the distillate inside the
On the separation of seawater through
receiving flask, and only spots of oily
simple distillation, it was observed in table 2
components was observed. After the
that the temperature from the first drop up to
distillation process, the distillate was
the last drop does not have a large difference,
transferred to the separatory funnel to
instead, it may had seemed that it does not
separate the essential oil with the aqueous
changed. It was also observed that the boiling
component of the distillate. However, since
temperature of the seawater sample does not
there was no distinct difference between the
went to 100ºC which was the boiling point of
oily layer and the aqueous layer, sodium
water which was present in seawater.
chloride solid was added to the distillate,
Table2. Range of temperature per 3 mL these helped in separating the oily
interval of the seawater sample components with the aqueous component.
Sodium chloride was an ionic bond, adding
Volume of distillate ions in the distillate helps increase the
Temperature (ºC)
(mL)
polarity of one component which then
3 97.8
separates the nonpolar and polar substances
6 97.8
in the distillate. However, even after the
9 98
addition of the solid sodium chloride, only a
12 98
15 98 thin layer was observed in the flask. These
These was explained by the very small yield was the result of the drying
seawaters’ composition. These erroneous technique used. Instead of air drying the
temperature was due to the impurities present lemon grass, the sample was subjected to sun
in the seawater. Impurities may result to the drying for more than an hour which may had
change of the temperature from its theoretical deteriorate the essential oil present in the
value. It may decrease or increase the sample. The range of heating process in the
temperature depending upon the impurities sample during the distillation process may
present in the compound. The location at had also caused errors.
where the seawater was obtained may had CONCLUSION
also caused this error in temperature of the
acquired sample experimentally. Distillation process was an effective
Nevertheless, the distillation process way of separating slightly volatile substance
separated the liquid distillate, leaving behind with a nonvolatile substance. It also was
the white precipitate which was the sodium effective in obtaining purified component in
chloride or what was known as the salt a mixture. The process was dependent on the
present in every seawater. temperature and volatility of the components
presents in the compound. Therefore,
Lastly, for the separation of essential distillation method was an effective method
oil from the lemon grass obtained at and was reliable enough to be used in
Pangasugan, Baybay City, Leyte, identifying purity and separating components
Philippines, the percentage of yield achieved of a mixture or compound. Careful
experimentally was computed to have 1.03% observation on the temperature reading was
needed to have an accurate result in this To the group’s family, especially to
method. their parents, who supported them endlessly
and who is always there to support the group
SIGNIFICANCE STATEMENT
morally and financially.
Separation of the components present
And all relatives, friends, groupmates and
in a compound through distillation was one
others who in one way or another shared their
of the many techniques in achieving a pure
support, either morally, financially and
compound out of a mixture. It was mostly
physically.
used in industries to declare the percentage of
purity content in the products produced by Thank you.
many companies. Distillation process was
REFERENCES
also very useful in separating essential oil
which was mostly used in aromatherapy Acabal, AM, Quevedo, ES, Lazona, YP,
sessions which gives ease and relaxation to Bandibas, KNS (2015). Laboratory Manual
humanity. in Chem 125 – Organic Chemistry, DoPAC
Visayas State University. pp. 3-7
ACKNOWLEDGEMENTS
(unpublished)
The completion of this undertaking
---(2004). Laboratory Manual for a course in
could not have been possible without the
Basic Organic Chemistry (Chem 40.1).
participation and assistance of so many
Division of Organic Chemistry and Natural
people whose names may not all be
Products. Institute of Chemistry, UPLB,
enumerated. Their contributions are sincerely
College, Laguna. pp.13-18.
appreciated and gratefully acknowledged.
However, the group would like to express Atheer, A., Hogg D., Zimmerman,
their deep appreciation and indebtedness W.,“Microbubble Distillation for Ethanol-
particularly to the following: Water Separation,” International Journal of
Chemical Engineering, vol. 2016, no.
First and foremost, the Almighty
5210865, p. 1, 2016.
God for the knowledge, wisdom and
understanding He bestowed. Additionally,
for His endless grace, blessings, and
everlasting love which gave the group the
strength to endure and overcome every
challenges, and unfavorable circumstances
and become self-dedicated in making this
experiment into reality. The author will
always give thanks to the Most High for His
goodness and faithfulness as well as the plans
He have for the author.
Ms. Mary Annilyn Villar for sharing
her invaluable knowledge of the subject
matter, her invaluable guidance, comments
and suggestions throughout the process.