International University, Vietnam National University - HCMC

School of Biotechnology
Department of Biochemistry

ORGANIC CHEMISTRY LABORATORY

REPORT 5: SIMPLE DISTILLATION
INSTRUCTOR: PhD. Hoàng Lê Sơn

TEACHING ASSISTANT: Nguyễn Thanh Phong

DATE OF SUBMISSION: 15-07-2019

Group member:

1. Trương Thị Ngọc Hằng - BTBCIU16041

2. Võ Minh Hạnh - BTBCIU16083

3. Nguyễn Hồng Anh Phương - BTBCIU16015

4. Nguyễn Tấn Phú - BTBCIU16057

Organic Chemistry Laboratory 1

 International University, Vietnam National University - HCMC
School of Biotechnology
Department of Biochemistry

I. Abstract
The aim of experiment is to separate hexane from mixture with toluene by technique of
simple distillation. After setting up the apparatus for a simple distillation, the mixture was
separated by starting heat up. The temperature was record once sample was collected, and
the refractive index of samples was measured triplicate. The first sample collected is most
purity one, with 81% hexane, and the following samples was decreased the purity one by
one until the last one was 18% hexane.

II. Introduction
Simple distillation relies on volatilization or evaporation and subsequent condensation of
liquids for separation and purification. Simple distillation may be used when the boiling
points of two liquids are significantly different from each other or to separate liquids from
solids or nonvolatile components. In simple distillation, a mixture is heated to change the
most volatile component from a liquid into vapor. The vapor rises and passes into a
condenser. Usually, the condenser is cooled to promote condensation of the vapor, which is
collected.

Figure1 : Simple distillation apparatus

A beaker is heated to the boiling point of the liquid. As it boils, the liquid turns into vapor
(gas). The vapor is directed through tubes (condenser) connected to another beaker. As the
vapor goes through the tube, it is cooled down by running cold water around the tubes.
This forces the temperature of the vapor to fall, causing the gas to turn into liquid again
(condensation).

Simple distillation is used for a variety of applications. One of them is to make wine and
spirits. Simple distillation is used to purify water for home use, schools or hospitals if there
is no bottled water or clean tap water available.

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 International University, Vietnam National University - HCMC
School of Biotechnology
Department of Biochemistry

However, in simple distillation, a mixture of liquids is heated to the temperature at which

one of its components will boil, then the vapor from the hot mixture is collected and re-
condensed into liquid. This process is fast and relatively straightforward, but there are
many kinds of mixtures that cannot be separated this way and require a more advanced
approach.
III. Materials and chemicals:
 Materials
The materials used through this experiment were distillation
apparatus with thermometer, stand, heating mantle and
water pump. The others were one 100 mL round- bottom
flask, 1 water bath, 2 glass pipets, 2 cylinders (10 mL), 11
test tubes, aluminum foil, refractometer.
The chemicals used in this experiment were hexane,
toluene and distilled water.

Figure 2: Refractometer
 Method of distillation:
First, 25 mL of hexane and 25 mL of toluene were mixed together in a 100 mL round
bottom flask. Then, boiling chips were added in order to prevent superheating of the liquid
being distilled and cause a more controlled boil, eliminating the possibility that the liquid in
the distillation flask will bump into the condenser. Then, set up the apparatus as the
following picture (Figure 2):

Figure 3: The apparatus for simple distillation

Note: Water in should be placed at the bottom to make sure that the entire volume of the
chamber would have to be filled before the water left and provide far more efficient
cooling. It was also the way to prevent thermal shock which could cause the glass to crack.
The coldest point of the condenser is at the bottom, where the water enters and the
condensate leaves, while the warmest is at the top, where the hot vapors enter and the

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 International University, Vietnam National University - HCMC
School of Biotechnology
Department of Biochemistry

warmed water leaves. Therefore, the temperature difference between the condensate and
glass it's in contact with is slightly lower than if it were set up the other way.
At the following step, 11 test tubes were prepared and marked 1 mL liquid extent for 1
tube and the rest with 5 mL liquid extent. Then, the first tube was put at the outlet of the
condenser. Next, the distillation flask was heated slowly until the liquid begins to boil. As
the liquid began to drop from the condenser, the temperature observed on the
thermometer should be changing steadily. 1 mL of the initial distillate was collected
approximately and then the rest were transferred one by one until the distillation was
complete or when the temperature started to drop or fluctuate. Finally, the refractive index
of each fraction was measured by using refractometer and recorded for sketching the
graph.
IV. Result:
Table 1 : The Boiling Points of distillation
Total volume of Boiling point (˚C)
distillate (mL)
1 73
5 74
10 83
15 85
20 90
25 93
30 97
35 97
40 96

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 International University, Vietnam National University - HCMC
School of Biotechnology
Department of Biochemistry

VOLUME DISTILLED VERSUS BOILING POINT

120

93 97 97 96
100 90
83 85
BOILING POINT (˚C)

80 73 74

60

40

20

0
0 5 10 15 20 25 30 35 40 45
TOTAL VOLUME OF DISTILATE (mL)

Figure 4. The graph of volume distillate versus boiling point for the simple distillation of

Table 2 : The Refractive Index of distillation

Total volume of distillate Refractive index
(mL)
1 1.3983
5 1.4045
10 1.4072
15 1.4139
20 1.4202
25 1.4334
30 1.4383
35 1.4646
40 1.4744

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 International University, Vietnam National University - HCMC
School of Biotechnology
Department of Biochemistry

VOLUME DISTILLED VERSUS REFRACTIVE INDEX

1.5
1.47
1.48
1.46
REFRACTIVE INDEX

1.46
1.44
1.44 1.43
1.42
1.42 1.41
1.4 1.41
1.4
1.4

1.38

1.36
0 5 10 15 20 25 30 35 40 45
TOTAL VOLUME OF DISTILATE (mL)

Figure 5. The graph of volume distillate versus refractive index for the simple distillation of a
mixture of hexane and toluene
The percentage volume of hexane in a fraction was calculated using the following
equation:
X x (1.3751) + (1-X) x 1.4961 = N
Table 3 : The percentage of hexane and toluene in each distillate volume
Fraction The volume The volume
fraction of fraction of
hexane toluene
1 81% 19%
2 76% 24%

3 73% 27%
4 68% 32%

5 63% 37%
6 52% 38%

7 48% 52%
8 26% 74%
9 18% 82%

V. Discussion :
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 International University, Vietnam National University - HCMC
School of Biotechnology
Department of Biochemistry

Simple distillation best used for separating relatively pure liquids with large boiling
differences or liquids with solid impurities. The solvent is used to separate the small
amount of a high-boling product from a reaction mixture, the residue should be transferred
into the other flask and then be continued distilling. If the first distillation was used to
isolate the mixture, the solvent may be contaminated which influence on results.
The percentage volume of hexane in a fraction was calculated using the following
equation:
X x (1.3751) + (1-X) x 1.4961 = N
With:
 N is the refractive index of the fraction
 RI Hexane = 1.3751, RI Toluene = 1.4961 with near the RI in experment
Simple distillation, when used to separate two substances, is used mostly when those two
substances have boiling points approximately 40ºC apart. The difference between
toluene(boiling point of 111ºC) and hexane(boiling point of 69ºC) is 41ºC, making these
two substances most easily separated by simple distillation. Distilled between 60ºC and
68ºC, the first fraction collected contained 81% hexane and toluene 19% since hexane has
such a lower boiling point than toluene, so he toluene was distilled in the first fraction. This
fraction contained 18% hexane and 82% toluene, so the hexane mostly distilled in the first
fraction.
When a solvent is used to extract a small amount of a high-boiling product from a reaction
mixture, it is common practice to first distil the solvent by simple distillation, transfer the
residue to a lower flask, and isolate the product in a second distillation. It not just continue
the first distillation to isolate the product since at the end of the first distillation, the liquid
remains in the round bottom flask is low. And there would not be enough molecules of
toluene to increase the vapor pressure up to a point that equals to the atmospheric
pressure, so the boiling process would not occur.

VI. Conclusion :
Simple distillation is one of method used to separate and purify the mixtures by boiling
point or refractive index by evaporation and condensation of the sample liquid – hexane
and toluene, for example. We also learned how to set up the operation for the distillation
and collect the figure to sketch graphs and compare them to see how two ways could show
their ability to separate mixture in the distillation

VII. Reference :
1. Organic Chemistry Laboratory Manual of the experiment 5. Ho Chi Minh:
International University, HCMC, 2018.

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 International University, Vietnam National University - HCMC
School of Biotechnology
Department of Biochemistry

2. Distillation. Wired Chemist. Date Accessed October 17, 2017

http://www.wiredchemist.com/chemistry/instructional/laboratory-
tutorials/distillation
3. Odinity. General Chemistry Labs. Date Accessed October 17, 2017
http://www.odinity.com/simple-distillation-separation-hexane-toluene

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