Jessica Brizuela

Rodney Pujada
LAB REPORT No 2 : Separation of Hexane and Toluene by Simple and
Fractional Distillation
Date: September 24th, 2016

I.

PURPOSE: This experiment we aim to demonstrate that we can separate two

volatile compounds from a mixture due to the different chemical properties of
each compound. We will accomplish this by a separation procedure known as
distillation, which relies on each compound having a distinct and separate boiling
point.
Our pure products will be analyzed with gas chromatography to
determine the success of the distillation .

II. INTRODUCTION:
There are four basic distillation techniques for separating and purifying the
components of a liquid mixture: simple distillation, fractional distillation, vacuum
distillation and steam distillation. The chosen distillation method and extent of
purification will depend on the nature of the mixture, specifically the difference
in the boiling points of miscible liquids. In distillation, the mixture is heated,
vaporizing a substance. Under boiling reflux, the vapor phase becomes richer in
the lower boiling component as vapors continue to condense and move up the
distillation head, purifying the mixture.
Simple distillation is most effective when applied to mixtures where the liquid
components differ in their boiling points by at least 50C. As the first component
distills, the temperature is measured from vapor it condensing on the bulb of a
thermometer positioned just below the sidearm of the distilling head. With
simple distillation, the rate of change of temperature is a slow as the
composition of the boiling liquid changes as distillation progress. Thus, the range
over which liquid is purified is not sharp. The temperature of the distilling liquid
is observed to plateau and then drop before rising again, as the process of
distilling the second component begins. Here, the temperature will plateau near
the boiling point of the second lowest boiling liquid in the mixture, thus distilling
the second fraction. The process continues for each subsequent component,
leaving the highest boiling liquid in the distilling flask. By carefully controlling the
rate of distillation, it is possible to affect reasonably good separation. If
distillation is rapid, then separation of the components of the mixture is poorer
than if the mixture is distilled slowly.
III. PROCEDURE:
2.1. Reagents :
2.11. Toluene
------------------------------------------------------------------------------------------------------------

CAS Number 108-88-3 Abbreviations: PhMe, MePh,

BnH
Properties Chemical formula
C7H8
Molar mass 92.14 gmol1
Appearance Colorless liquid, Odor
sweet,
pungent, benzene-like
Density
0.87 g/mL (20 C)
Melting point
95 C (139 F; 178 K)
Boiling point
111 C (232 F; 384 K)
Solubility in water: 0.52 g/L (20 C)
Vapor pressure
2.8 kPa (20C)
Hazards
------------------------------------------------------------------------------------------------------------------Main hazards
highly flammable
Flash point 6 C (43 F; 279 K)
Explosive limits
1.1%-7.1%
Potential Acute Health Effects:
Hazardous in case of skin contact (irritant), of eye contact (irritant), of
ingestion, of inhalation. Slightly hazardous in case of skin contact
(permeator).
2.12. Hexane
------------------------------------------------------------------------------------------------------------CAS Number 108-88-3 Abbreviations:
Properties Chemical formula
C6H14
Molar mass 88.18 gmol1
Appearance Colorless liquid, Odor: Petrolic
Density
0.6548 g/mL (20 C)
Melting point
96 C 94C
Boiling point
68.5 C
Solubility in water: 9.5 g/L (20 C)
Vapor pressure
17.60 kPa (20C)
Hazards
-------------------------------------------------------------Main hazards
highly flammable
Flash point 6 C (43 F; 279 K)
Explosive limits
1.2%-7.7%
Potential Acute Health Effects: Hazardous in case of skin contact
(permeator), of ingestion, of inhalation. Slightly hazardous in case of skin
contact (irritant), of eye contact (irritant).
2.2. Procedure Simple Distillation
a. Prepare a table of 30 measures for temperature vs volume
b. Label 2 mL test tube sample with s1, S2, F1 and F2
c. Mark until 1 mL level.
d. Set the distillation apparatus.

e. Place 10 mL Hexane and 10 mL toluene into 50 mil round flask . Add

boiling chips.
f. Check joints and connections.
g. Adjust the heat to get 0.5 mL liquid collected and record the
temperature

2.3. Procedure Fractional Distillation:

a. Prepare a table of 30 measures for temperature vs volume
b. Set up fractional distillation and add the fractional column careful.
c. Label the collect sample with F1 and F2.
d. Check the fractional distillation apparatus.
e. Place 10 mL Hexane and 10 mL toluene into 50 mil round flask . Add
boiling chips.
f. Check joints and connections.
g. Adjust the heat to get 0.5 mL liquid collected and record the
temperature

IV. RESULT AND

4.1 DATA
Table No
of Hexane
Table No
Distillation

DISCUSSION
1: Simple Distillation
in Toluene
2: Fractional
of Hexane in Toluene

Table No 3: Graph the table No 1 and table No 2 in Volume vs Temperature

We appreciated the curve for simple distillation is more straight and ascendant that
the fractional distillation. When the substances in a mixture have significant
differences in boiling points, a simple distillation is adequate to be implemented. As
the name suggests, it is as simple as it gets. No fractionating column is required for
use. A single distillation cycle is enough to separate the mixture. For example
Hexane boiling point is 68.5 C and toluene boiling point is 111 C that we conclude
that the first compound in distillate is hexane and after toluene. When we have
mixture with more heat boiling point fractional distillation shows us the difference.
In our graph the curve jumps between the 10 mL and 11 mL of distillated. It is point
where we can find more percent of pure solvent that come first to the distillation. In
our experiment this is Hexane because it has the low boiling point.
4.2 CALCULATION
Table No 4: Calculation of Correct Area
By the Chromatograph result in annex No 1 of how much areas for simple
distillation.
Table No 3:
Peak

Sample Peak Area

S1Hexane

1435.9697

S1 Toluene

715.3242

S1 Total peak area

S2 Hexane
S2 Toluene
S2 Total peak area

2151.2939
156.4222
1810.0782
1966.5004

By the Chromatograph result in annex No 2 of how much areas for Fractional

distillation.
Table No 4
Peak
Sample Peak Area
F1Hexane
1446.646
F1 Toluene
485.9424
F1 Total peak area
1932.5884
F2 Hexane
618.819
F2 Toluene
1778.0548
F2 Total peak area
2396.8738

4.2.1 Calculate the correction factor for hexane and toluene by the graphic for
one solution 50:50 mixture GC analysis

Compone
nt

Retention

Height

Peak Area Standard

sample Measured

S1Hexane

1.156

118.224

1464.8665
(1210.7+254.1)

3.203

91.463

2038.7444

S2
Toluene
S1 Total
Peak Area

3503.6109

Response Factor
1464.8/3503.6=
0.719
2038.7/2038.7=
1.000

IV.2.2.

Calculate the corrected Area

Peak

Sample Peak
Area
(Measured)

S1Hexane

1435.9697

1435.9697/0.719 =

1997.176217

S1 Toluene

715.3242

715.3242 /1.00 =

715.3242

S1 Total peak area

S2 Hexane
S2 Toluene
S2 Total peak area
.

2151.2939
156.4222
1810.0782
1966.5004

156.4222/0.719 =
1810.0782/1.000 =

2712.5004
217.5552156
1810.0782
2027.6334

Correct Area

Correct Area

1446.646/0.719 =
485.9424

2012.025035
485.9424
2497.9674
860.6662031
1778.0548
2638.7210

Peak
F1Hexane
F1 Toluene
F1 Total peak area
F2 Hexane
F2 Toluene
F2 Total peak area

Sample Peak
Area
1446.646
485.9424
1932.5884
618.819
1778.0548
2396.8738

Correct Area

618.819/0.719
1778.0548

4.2.3 calculate the percent of each sample

by for hexane in S1 sample.
Area of S1 Hexane = 1997.176217
S1 Total peak area
=
2712.5004

% of Hexane in S1 = Area of S1 Hexane*100 / S1 Total

peak area
From the Tables Annex 1 :
% Hexane in S1 = 1997.176217*100/2712.5004
% Hexane in S1 = 73.6 %

By the calculation before we get this table No 5 as the result of percent of each
sample.
Peak Area

% Hexane

% Toluene

S1 sample
S2 Sample
F1 sample
F2 sample

73.6
10.7
80.5
32.6

26.4
89.3
19.5
67.4

In our second part, we calculate

the percent of hexane in toluene.
In simple distillation we observe el
percent of hexane is 74% that
show us it is the first solvent to
come in the distillation. After we
analyze the second sample S2, we
obtain a 26.4 % for hexane and
89.3% for toluene which is the
second compound in our mixture.
That shows we purified the
solution from the hexane with a
high percent of purity. However, in
our fractional distillation this
process is better for our hexane in
80.5 % in F1, but it not better for
toluene which concentration in
percentage is less than simple
distillation. The concentration of
Toluene in percentage have to be
more than 89.3 % that could be for
taking the sample in the incorrect
time.

V. CONCLUSION
We found many differences in both distillations. For example, simple distillation
is the method used to separate substances in mixtures with significantly
different boiling points, while fractional distillation is used for mixtures
containing chemicals with boiling points close to each other. In our experiment
we notice the purification of hexane is high in 80.5% of purity. Simple distillation

will only have one distillation (vaporization-condensation) cycle in the whole

process, while the fractional cycle will have at least two cycles. Beside, Fractional
distillation will use additional equipment called the fractionating column, while
the simple distillation will not need that equipment. Simple distillation is often
used to separate the liquid substance from the solid substance. Doing such
separation with fractional distillation is not sensible. We concluded the fractional
distillation is more effective.
The difference between simple and fractional distillation is the number of
times that the liquid is vaporized and condensed. Simple distillation condenses
the liquid once, so the boiling points of the two liquids must be far apart to make
it efficient. The number of simple distillations in a fractional distillation apparatus
depends on the length and efficiency of the fractionating column. The process is
the same; the difference is mainly one of iteration.
To obtain the maximum efficiency in any distillation, the distillation rate must
be kept constant and slow (for our apparatus a rate of about 1 drop per 20 30
seconds produces the best separation).In our experiment, we keep a constant
heat because the fluctuation of temperature can give us a not a pure distillated.
Distillation rate is the single most important variable that contributes to an
effective distillation.
VI. REFERENCES
ANALYTICAL CHEMISTRY FOR TECHNICIANS. Third Edition. Lewis
Publishers.2003. Pages 337-341
MSDS SHEET. Toluene: Material Safety Data Sheet No 1A2875
http://www.sciencelab.com/msds.php?msdsId=9927301
MSDS SHEET. Toluene: Material Safety Data Sheet No 1A2984
http://www.sciencelab.com/msds.php?msdsId=9927187
Laboratory Techniques in Organic Chemistry. Morhig and others. 1 st.
Edition .W. H. Freeman and Company. 2014. Pag: 180-184