LAB# 05

VACUUM DISTILLATION FOR THE SEPARATION OF ACETONE AND WATER

Objective:
To study vacuum distillation for the separation of acetone and water.

Apparatus:
Vacuum Distillation Tester.
Model: SYD-9168A
This apparatus consists of:

• Display Unit: Digital display and control unit contains temperature, time and fan speed
• Vacuum Pump: to create a vacuum in vacuum distillation chamber
• Cooling Fan: Located sidewise to the furnace and automatically operates to cool the
heating furnace after the test.
• Oil Temperature Sensor: to check the temperature inside the test flask especially when
the sample is oil.
• Heating Furnace: electric heating furnace and the temperature is adjusted by display
screen with an accuracy of 0.5 %
• Furnace uplift: a platform for up and down and automatically it adjust the level according
to sample level
• Vapor Temperature sensor: to check the temperature of vapors going above
• Distillation Assembly: main assembly for the distillation
• Cold Trap: Semiconductor hydrazine supply
• Hydrazine Bottle: Cold Liquid Hydrazine residue. The liquid can be taken out from here
for further analysis.
• Main Power switch

• Pump Switch
• Water supply
• Clamps
Figure:

Areeba Naqvi B20F0454CHE030 LAB 05

Vapor temperature Display Meter
sensor

Cold Hydrazine

Cooling Fan
Distillation
Assembly
Vacuum Pump

Heating Furnace

Fig 01: Vacuum Distillation Tester

Model: SYD-9168A

Fig 02: Display Screen

Areeba Naqvi B20F0454CHE030 LAB 05

Solution:
• Water
• Acetone
• Hydrazine

Theory:
Distillation is the process of vaporizing a liquid, condensing the vapor, and collecting the
condensed liquid (or condensate) in a different container. It is a general technique that permits
liquid compounds to be purified or solvents to be selectively removed from non-volatile
materials. Simple, fractional, steam, and vacuum distillation are four modifications of the basic
distillation technique. Distillation is a commonly used method for purifying liquids and separating
mixtures of liquids into their individual components. Familiar examples include the distillation of
crude fermentation broths into alcoholic spirits such as gin and vodka, and the fractionation of
crude oil into useful products such as gasoline and heating oil. In the organic lab, distillation is
used for purifying solvents and liquid reaction products.
At any temperature, some molecules of a liquid possess enough kinetic energy to escape into the
vapor phase (evaporation) and some of the molecules in the vapor phase return to the liquid
(condensation). An equilibrium is set up, with molecules going back and forth between liquid and
vapor. At higher temperatures, more molecules possess enough kinetic energy to escape, which
results in a greater number of molecules being present in the vapor phase. Rotary evaporation is
a common technique used in laboratories to concentrate or isolate a compound from a solution.
Many solvents are volatile and can easily be evaporated using rotary evaporation. Even less
volatile solvents can be removed by rotary evaporation under a high vacuum and with heating.
It is also used by environmental regulatory agencies for determining the number of solvents in
paints, coatings, and inks. When you have a solution that you need to separate using distillation,
you need to heat the mixture above the boiling point of one component so that it can be
converted into vapor form and then condensed to cover again in liquid form.
If the boiling point of the component is very high (generally boiling point of more than 150 is
considered high) it is difficult to achieve as it requires a utility that can evaporate it which can be
costly. So the pressure of the column is reduced, as pressure decrease, the boiling point of the
compound also decrease. This decrease in the boiling point of the compound can be achieved
with cost-effective utilities also and can achieve easily. To create a vacuum is a distillation
column, a steam ejector is used. The steam ejector or vacuum pupm is used to generate a vacuum
which is connected to a vacuum trap where the vacuum is stored. The distillation column receiver
is then connected through-line with the vacuum to get the vacuum in the column receiver.
Through the column receiver, we can get the vacuum in the distillation column. This was the
procedure where the column is used for the distillation operation.
Advantage of VDU:

Areeba Naqvi B20F0454CHE030 LAB 05

 • It allows you to heat the material at a lower temperature
• It prevents other side reactions that can occur at high temperature
• It prevents material to get decomposed which it can be at high temperatures.

Procedure:
Water connections:
In the distillation assembly, there is three inlet water connections. At the inlets, there is a cold
water, supply in order to condensate the vapors coming from the flask because of heating. That
cold water takes the heat from the vapors and then goes out from the outlets and with the help
of coolant which is hydrazine it again becomes cool. And the process continues like this until the
experiment ends. The water used here is distilled water and it circulates in the jacket around the
glass flasks.
PROCEDURE:
First of all, it was ensured that the apparatus is working properly and that all connections are
connected accordingly. It was ensured that the water connection pipes at inlet and outlet are
tight. Afterward, initially, the sample was prepared which was about 50% acetone and 50% water
mixture. That mixture was poured into the conical flask and then flask was fixed with distillation
assembly with the help of clamps. After putting the sample make sure to close the protecting
doors in order to be safe from any splitting. In the next step, the apparatus was turned on from
the main power button along with the vacuum pump. Then the heating furnace was lifted up
through the button on the display meter. From the setting go to the new test and then test begin
and then start the test by giving 100% heating. Now as time proceeds the acetone starts to boil
first as its boiling point is low around 56 degrees. Acetone vapors are then collected in the
distillate residue chamber after passing through the assembly and by the process of
condensation. When the acetone vapors have completely collected the experiment was ended
from the display meter and the readings there were continuously observed during the
experiment were noted. And the fan automatically turns on in order to reduce the temperature
of the furnace. The furnace was then lifted down and samples were taken out. At the end, the
apparatus was turned off from the main power.

Readings:
Absolute Pressure setting:

(2, 5, 10, 20,50) mm of Hg

Absolute Measurement Range:

2 to 170 mm of Hg

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CONDUCTIVITY:

• Water = 1.2 micro Simon

• Acetone = 2.30 micro Simon

VOLUME (Percentage) VAPOR TEMPERATURE (0C)

10 % 24.2
20% 41.8
30% 42.6
40% 43.6
50% 44.0
60% 44.2
70% 45.2
80% 47.5
90% 47.9
91% 48.4
92% 69.3
FBP 70.2

Result and Discussion:

The main objective of this experiment was to separate the water and acetone by using vacuum
distillation. As the boiling point of acetone is less than that of water so it was evaporated first at
a temperature range (50-70). Vacuum distillation is used for those substances that are
temperature sensitive and they are difficult to separate at high temperatures. So by creating a
vacuum the pressure is decreased and hence the boiling point as well. In the separation of a
mixture of two substances, the one with the lower boiling point separates out first and its vapor
are condensate in the condensate chamber.
In this experiment, the desired acetone was separated at the volume range between 80% to 90%
at the relative temperatures of 47.5 to 69.3 oC.

Conclusion:

Areeba Naqvi B20F0454CHE030 LAB 05

The purpose of this experiment was to separate the acetone from the water. In the mixture, there
was 50% of water and 50% the acetone. Vacuum distillation is used for those substances which
have low boiling points or those which are temperature sensitive and decompose at high
temperatures. In this experiment, acetone has the low boiling point and it was evaporated first
and was separate out in the distillate filtrate. Moreover, in this experiment coolant was used in
order to condensate the vapor of the substances which have low boiling points. Coolant was used
to lower the temperature of circulating water and that water was basically helping to make the
condensate.

References:
1. Y.A. Cengel and A.S. Ghajar; Heat and Mass Transfer: Fundamentals and Applications; MC
Graw-Hill, 6th Edition, 2020.
2. Raj Chhabra V. Shankar Coulson and Richardson’s Chemical Engineering Volume 1B: Heat
and Mass Transfer: Fundamentals and Applications Seventh.
3. https://nitsri.ac.in/Department/Chemical%20Engineering/Distillation_Notes-PartVI.pdf
4. https://www.epicmodularprocess.com/blog/when-vacuum-distillation-is-
useful#:~:text=Vacuum%20distillation%20is%20the%20process,vapor%20pressures%20t
o%20evaporate%20off.

Areeba Naqvi B20F0454CHE030 LAB 05