DEPARTMENT OF CHEMISTRY

FACULTY OF SCIENCE AND MATHEMATICS

SULTAN IDRIS EDUCATION UNIVERSITY

SKL3013

CHEMISTRY LABORATORY MANAGEMENT TECHNIQUES

EXPERIMENT 7: DISTILLATION

By

STUDENT’S NAME 1. NURSYAFIQAH BINTI ABDUL MALIK

& (D20182085817)
MATRIC NUMBER 2. NOR AIYNA SYERA BINTI MOHD ASRI
(D20182085843)
3. NHISHALINI A/P KARUNAKARAN
(D20182085833)
GROUP A
LECTURER’S NAME DR. NORLINDA BINTI DAUD

Date and Time of Practical Class

9th April 2019, 9.00 a.m – 1.00 p.m
TITLE : Distillation

OBJECTIVES

1. To set up simple distillation apparatus.

2. To separate two miscible liquids using simple distillation.
3. To differentiate the distillate.

CHEMICALS

 Methanol
 Distilled water
 Boiling chips

APPARATUS

 Thermometer
 Thermometer adapter
 Distilling head
 Round-bottomed adapter
 Heating mantle
 Retort stand
 Rubber tubbing
 Clamp
 Condenser
 Adapter
 Graduated cylinder
 Glass funnel
 Watch glass
 Bunsen burner
RESULT

Temperature of the first drop of distillate: 65oC

Temperature (oC) Volume of the Temperature (oC) Volume of the

distillate (mL) distillate (mL)
70 1 98 1
72 2 98 2
74 3 104 3
75 4 100 4
77 5 99 5
80 6 103 6
82 7 110 7
85 8 112 8
86 9 113 9
87 10 115 10
90 11
91 12
93 13
96 14
98 15
Test on distillate:

Test Distillate Observation Conclusion

Combustion test First 15 mL Burn, The first 15 mL is
There’s a fire inside methanol
the bowl. Contains
alcohol

Second 10 mL Doesn’t burn and The second 10 mL

there’s no change is water
and effect. Do not
contains alcohol.

Graph

QUESTIONS

1. From the graph, determine the boiling point methanol and water.
The boiling point of water is 100 ˚C and for methanol is 65.9 ˚C.
2. Between methanol and water, which has the lower boiling point based on the
combustion test? Explain.
Based on the combustion test, methanol has the lower boiling point than water. This is
because methanol has both a nonpolar methyl group –CH and a polar –OH group. In
methanol, CH3OH, the electronegativity of the oxygen makes O-H polar, which gives
the hydrogen in O-H a partially positive charge. Thus, the hydrogen bonds are formed
between the oxygen of one methanol and the hydrogen in the O-H of another
molecule of methanol. The bond between methanol molecules is not tight. So, it takes
less energy to enable the methanol to move apart into a gaseous state.
However, the hydrogen bonds in a water are much stronger than in methanol.
The water molecules have a more positive area where the hydrogen atoms are, and a
more negative area where the oxygen atom is. Because of this tight bond, water
molecules need more energy in order to move apart and turn into a gaseous state.
Therefore, based on the explaination above, less energy is required to
overcome the intermolecular forces of attraction in methanol but more energy
required to overcome the intermolecular forces of attraction in water.

3. What is the purpose of putting a few boiling chips into the pot?
The purpose of boiling chips are they will prevent superheating of the liquid being
distilled and they will cause a more controlled boil, eliminating the possibility that the
liquid in the distillation flask will bump into the condenser.

4. Between simple and fractional distillation, which type of distillation is more efficient
to separate methanol and water? Explain.
To separate the methanol and water, simple distillation is more efficient than
fractional distillation The boiling point between methanol and water have a big range
of differences so simple distillation is more efficient and convenient because the
simple distillation process is best for separating relatively pure liquids with large
boiling differences or liquids with solid impurities.
In simple distillation, this distillation condenses the liquid once, so the boiling
points of the two liquids must be far apart to make it efficient. The apparatus for a
simple distillation is a sealed system, which means nothing is open to the air, and
consists of a heat source, a still pot containing the liquid to be distilled, an air- or
water-cooled condensing line, and a vessel for the distillate. The mixture is heated and
 the liquid with the lower boiling point is vaporized and then condensed and drips into
the final vessel.
Fractional distillation completes several simple distillations in one apparatus.
In fractional distillation the mixture is boiled in a fractionating column, a long tube
that allows the liquid to vaporize and condense several times as it hits cooler air every
time it makes its way further up the column. Fractionating columns are often packed
with metal wire, metal ribbon or glass beads that give extra condensing surfaces to
refine the distillation process. This ensures that the vapor reaching the final condenser
is as pure as possible. However, fractional distillation only best used for separating
complex mixtures of liquids with smaller boiling point separations. For example, to
separate the mixture of ethanol and methanol.

5. List down the precautions that should be taken during distillation experiment.
 Allow sufficient space to work in, where the distillation area should be well
lit, clean and well
 Perform a cleaning distillation steps before starting the experiment.
 Monitor the temperature constantly.
 Avoid touching the pot while it is still hot. Allow it to cool down first.
 Place the receiver low on the floor, away from the heat source.
 Clean your work area immediately after distillation.
DISCUSSION

This experiment is carried out to investigate the relationship between methanol and water. A
mixture of methanol-water with known composition is initially fed into the evaporator. When
the heater is switched on, the mixture will start to boil. The mixture vapour will rise up and
will be cooled down by the condenser at the top of the evaporator. As the vapour starts to
condense, the liquid falls back into the evaporator. Samples of distilled water was taken to
check the compositions by lighten it up in crucible. The reading is observe and recorded. The
graph x-y diagram is construct as volume at axis X and temperature at axis Y. The simple
distillation was very slow. There was no large jump in temperature difference during 1st
receiver distillation. The simple distillation also seemed to have been distilling water at the
end of the distillation even though the temperature would not go above 98 degrees Celsius.
As shown in the result table distillates were collected with each having a 0.1mL
portion.The total volume of fractions collected in the 1st receiver was 15.0mL. The first
receiever has a maximum temperature of 98 degree celsius. But at the 2nd receiver
temperature from 98 degree Celsius it rose to 115 degree Celsius. The simple distillation did
have a large jump in temperature once we had collected about 15 mL of distillate. This might
occurred due to human error, like not greasing the joints well enough, creating air to escape
the apparatus defeating the purpose of a closed simple distillation apparatus. Too many
boiling chips causes the mixture to heat unevenly which causes molecules with higher
boiling point to gain energy before the molecules of the lower boiling point does.
The large jump is appropriate because it represents the point where we begin to
distilled water because there wasn’t much methanol left in the boiling solution.We also
exposed the methanol in air quite a long time. So overall the 1st receiver was a success
whereas the the next receiver was a fail because the temperature rose more than 100 degree
Celsius. When we conduct the flammability test we got to know that The first fraction
produced a blue flame when lighted match was applied. This shows that the first fraction still
contains alcohol. When a lighted match was applied to the last fraction, there was no
appearance of flame, meaning there is no alcohol in it.
CONCLUSION

Distillation is a very effective method of separating the constituent parts of a mixture. It is the
process of separating the components or substances from a liquid mixture by using
selective boiling and condensation. Distillation may result in essentially complete separation
or it may be a partial separation that increases the concentration of selected components in
the mixture. In either case, the process exploits differences in the volatility of the mixture's
components.
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 non volatile
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.. Simple distillation is a
effective method of distillation. The data collected throughout the experiment revealed that
the simple distillation more effective when two liquids in a mixture have a larger difference
in boiling points. The information and techniques of this experiment are very important to
understand because we used real world applications. Overall, this lab accomplished what it
set out to do. New skills and techniques were learned when the distillation apparatus were set
up and used. Moreover, the data collected from the experiment illustrates how boiling point
and temperature affect the method of distillation.

REFERENCES

Internet

1. Retrieved from
https://www.academia.edu/27940646/Sample_Lab_Report_Simple_and_Fractional_D
istillation on 14th May 2019.
2. Retrieved from
https://www.coursehero.com/file/13393183/Lab-Report-Simple-Distillation/ on
15th May 2019.

Books

1. Laboratory Manual 9th May 2019. Retrieve from SKL3013 chemistry laboratory
management techniques lab manual.