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ABSTRACT
The objectives of this experiment are to assemble a simple and a steam distillation set-up, to identify and recognize the
significance of all parts of the set-up, and to purify a sample using simple and steam distillation. Distillation is the separation
of two or more liquids of different volatility. In simple distillation, a liquid is boiled and the vapours work through the apparatus
until they reach the condenser where they are cooled and reliquify. Steam distillation is used for separating substances which
are immiscible with water, volatile in steam & having high vapour pressure at the boiling temperature of water. Simple
distillation of toluene was performed in this experiment having 32.32 % of percentage recovery and steam distillation of pdichlorobenzene was also performed and obtained 89% of percentage recovery. In boiling which a solvent becomes
superheated and then undergoes a sudden release of a large vapour bubble, explosively forcing liquid outside of a flask is
called bumping. To prevent this from happening we add glass beads in the distilling flask. Glass beads provide nucleation
sites; extremely localized budding for gaseous bubbles, so the liquid boils smoothly or more easily. Materials and procedures
on hoe to perform the experiment is mention in here, like the quick fit equipment was mostly used in this experiment having
one-necked pear-shaped flask, two-necked pear-shaped flask and the distillation set-up. Theories and relationships about
distillation, boiling point and volatility was learned and observed in this experiment.
Keywords: albumin, casein, invertase, Bradford Assay, Warburg-Christian Assay, Benedicts reagent
INTRODUCTION
The purpose of the experiment is to show to students
how simple and steam distillations are being
accomplished. To show us how to assemble a simple and
a steam distillation set up and identify ad recognize the
significance of all parts of the set-up. Also, learn the
techniques in purifying samples using these 2 methods.
According to the organic chemistry laboratory manual,
the volatility of a compound is based on the equilibrium
vapour pressure exerted by the compound at a particular
temperature. Different compounds will exert different
vapour pressures at a given temperature because of
variations in the intermolecular forces of attraction
working these different compounds. Compounds that
have stronger intermolecular forces will be harder to
detach from each other, hence lesser volatility.
Compounds that are more volatile will change faster in to
vapour than does that have low volatilities. The object of
distillation is the separation of a volatile liquid from a nonvolatile substance or, more frequently, the separation of
two or more liquids of different volatility.
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FIGURE 1
The distilland we collected was 15 ml of toluene. We
started the distillation beginning with switching the heat
regulator to number 6. Once the collected distillate
reached 1ml the temperature was read and recorded. We
record all the different temperatures as the volume of the
distillate increases. After collecting data, we plot the
temperature against the volume of the distillate collected
and recorded the temperature range at which most the
liquid distils.
FIGURE 2
DISCUSSION AND RESULTS
I. Simple Distillation
Graph 1: Volume of the distillate vs. Temperature
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100 110
13
Percentage recovery
32.31%
OBSERVATIONS
It took a very long time to have a distillate.
After a few minutes, the temperature increases.
The temperature remained at 110C and the
distillate continuously flowed in the graduated
cylinder.
At 110C, the total volume is 13 ml.
In boiling which a solvent becomes superheated and then
undergoes a sudden release of a large vapour bubble,
explosively forcing liquid outside of a flask is called
bumping. To prevent this from happening we add glass
beads in the distilling flask. Glass beads provide
nucleation sites; extremely localized budding for gaseous
bubbles, so the liquid boils smoothly or more easily. The
air bubbles break the surface tension of the liquid being
heated and prevent superheating and bumping. Glass
beads should not be added to liquid that is already near
its boiling point, because it can cause to solvent to boil
over violently that causes product loss, hence it must be
add before distillation. It is necessary to control the heat
rate to prevent the continuous flow of distillate that may
contain impurities, therefor when the heat is controlled
the ways of the impurities to evaporate is lesser since it
may not reach its boiling point.
II. Steam Distillation
Table 3: Steam Distillation Data
56-58 C
49-51C
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2.0 g
1.78 g
Percentage recovery
89 %
OBSERVATION
The crude p-dichlorobenzene was dissolved in
water wherein there were red-orange and white
colors.
The red-orange solution was on the top and the
white portion is at the bottom.
The white part of the solution started to
vaporized and condensed by the condenser as
the distillation continues.
In the inner wall of the condenser, white solids
are formed.
The solution crystallized in the cooling bath.
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an/bastyr/summer%2007/organic
%20lecture/Lab%20Packetfall07.pdf
Baluyot, J. Y., & De Castro, K. A. (n.d.).
Organic Chemistry Laboratory Manual
for Chemical Engineering Students.
Klein, D. (2012). Organic Chemsitry.
Massachusetts: John Wiley & Sons, Inc.
Young, S. (1922). Distillation Principles and
Processes. London: Macmillan and Co.,
Limited.
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