Indian Institute of Technology Gandhinagar

Experiment-5, 20 February, 2023

Steam Distillation

Mass Transfer and Reaction Engineering

CL-352 Lab Report (Group C)

Authors
Shreyansh Chourasiya 19110031
Sakshi Jain 20110181
Ayush Bhalala 20110037
Rajesh Kumar 20110161
Title
To understand the principle of steam distillation, compare the experimentally observed
results and phenomena to that predicted by theory.

Abstract
The aim of this experiment was to investigate the fundamental principles of steam
distillation and its advantages over traditional distillation techniques. A mixture of
nitrobenzene and distilled water in a volumetric ratio of 1:4 respectively was used.
Steam was passed through the mixture to vaporize the nitrobenzene, which has a higher
boiling point than water. Steam increases the vapor pressure of the nitrobenzene,
making it easier to vaporize and distill. Steam also provides gentle heating, preventing
thermal decomposition of the nitrobenzene and allowing distillation at a lower
temperature, preserving the quality and purity of the organic compound.

However, the experimental results showed a deviation in the weight ratio of

nitrobenzene and water calculated experimentally compared to the theoretical results
calculated using Rault's law for immiscible liquids, which predicts that partial pressure
is equal to saturated pressure. The deviation may be attributed to factors such as the
presence of dissolved gasses, non-ideal behavior of the mixture, and other practical
limitations encountered during the experimental procedure. Overall, the results
demonstrate the usefulness of steam distillation as a technique for the purification of
organic compounds which has more boiling point from immiscible mixtures.

Introduction
The act of selectively boiling and condensing substances from a liquid mixture is known as
distillation, or classical distillation. This is often done inside of a device called a still.
Distillation may result in essentially complete separation , resulting in nearly pure components,
or it may be a partial separation that increases the concentration of selected components; in
either case, the process exploits differences in the relative volatility of the mixture's
components. Usually, a column is inserted between the pot and the condenser to improve the
efficiency of the separation process. In order to concentrate the more volatile liquid in the first
fractions and the less volatile components in the later fractions, a distillation column is a tube
that offers surfaces on which condensations and vaporization can occur before the gas hits the
condenser. Prior to reaching the condenser, the analyte normally travels through a number of
vaporization-condensation processes.
Here we have done steam distillation of Nitrobenzene to measure the weight fraction of
Nitrobenzene and water in the product obtained. The principle behind steam distillation is
based on the fact that water and organic compounds have different boiling points.
When water is heated to its boiling point, it vaporizes and forms steam. If a mixture of
water and the volatile compound is heated, the steam will carry the volatile compound
with it, and the mixture can be condensed to get the weight fraction of each component
in the extract. The flow in the condenser tube in this case is counter current.

The key to the success of steam distillation is that the vapor pressure of the volatile
compound must be lower than the boiling point of water, but high enough to allow it to
evaporate and be carried by the steam. The steam is then cooled, usually by passing it
through a condenser, which causes it to condense back into a liquid. The condensate
contains both water and the volatile compound, and the two can be separated by
decantation, extraction, or other means.

Fig 1. Diagram of the set up

Steam distillation is widely used in the production of essential oils, as it allows for the
isolation of the volatile compounds without subjecting them to high temperatures that
could damage or alter their chemical properties. Here we have not used steam
distillation as a method of separation of components based on their boiling points. But
it should be kept in mind that for steam distillation, the components must not react
with each other at the higher steam temperature. Also, the component should be
insoluble in water.

° °
Let 𝑁𝑊 and 𝑁𝑁 be the moles of water and nitrobenzene respectively and 𝑃𝑊 and 𝑃𝑁 are
their partial pressure in the gas phase.

𝑊𝑒 𝑙𝑒𝑡, 𝑁𝑇 = 𝑁𝑊 + 𝑁𝑁

° 𝑁𝑊
𝑃𝑊 = 𝑃 × 𝑁𝑇
° 𝑁𝑊
𝑃𝑊 = 𝑃 × 𝑁𝑊 +𝑁𝑁
° 𝑁𝑁
Similarly, 𝑃𝑁 = 𝑃 × 𝑁𝑊 +𝑁𝑁

°
𝑁𝑁 𝑃𝑁 𝑊𝑁 × 𝑀𝑊
So, 𝑁𝑊
= ° = 𝑊𝑊 × 𝑀𝑁
𝑃𝑊

°
𝑊𝑁 𝑃𝑁 × 𝑀𝑁
We now can get, 𝑊𝑊
= °
𝑃𝑊 × 𝑀𝑊

Procedure
Materials and Equipment:
1. Round bottom 2-necked flask.
2. 200 ml of Distilled water and 50 ml of Nitrobenzene.
3. Condenser tube
4. Connecting tubes
5. Beaker, measuring cylinder and test tube.

Procedure:
1. A solution of 200 ml distilled water and 50 ml of nitrobenzene is prepared.
2. The apparatus is set up by connecting tubes and as shown in the figure.
 Fig 2. Experimental set-up
3. The heater is switched on and the voltage is set at 40 V.
4. After some time, the distillate will start collecting in the receiving flask.
5. After around 30 minutes, when the distillate in the receiving flask reaches 40 ml,
it is taken out and another empty flask is put in its place.
6. The temperature of the solution in the round bottom flask is duly noted at certain
intervals of time for precaution and to keep the boiling point of nitrobenzene in
check.
7. Both distillates obtained were kept for 24hrs at room temperature to be able to
settle down and separate out.
8. A layer is observed between both the components after 24 hrs.
9. The volume for each component is noted down for both the receiving flasks.

Results
Observation table:
The following has been referred from NIST database
● Density of Nitrobenzene(ρ𝑁) = 1.2 g/mL.
● Density of water (ρ𝑊)= 0.997 g/mL.
● Molecular Weight of Nitrobenzene ( 𝑀𝑁)= 123.11g/mol
● Molecular Weight of Water ( 𝑀𝑊) = 18g/mol

Component Nitrobenzene Water

 Extract 1 Volume (ml) 10 58

Extract 2 Volume (ml) 5 35

Table 1: Volume of components in obtained extract.

Observation No Time (min) Temp (Celcius)

1 0 24

2 5 55

3 10 106

4 15 116

5 20 123

6 25 127

7 30 132

8 35 137

9 40 139

10 45 140

Table 2: Temperature variation with time.

Calculation:

Sample Calculation:
● For immiscible liquids:
° °
𝑃𝑊 = 𝑃𝑊 , 𝑃𝑁 = 𝑃𝑁
● Steady state temperature of mixture = 413.15 K.
° °
● 𝑃𝑊 and 𝑃𝑁 can be calculated by Antoine's equation for water and nitrobenzene at
T = 413.15K.
° 𝐵
𝑙𝑜𝑔𝑃𝑊 = A - 𝑇+𝐶
°
Similarly for 𝑃𝑁, by putting the respective values of A,B, and C.
° °
On calculating in excel sheet we get, 𝑃𝑊 = 3.689 bar and 𝑃𝑁 = 0.135 bar.
● Now from equation 1, theoretical value of weight ratio of Nitrobenzene to water -
°
𝑃𝑁 × 𝑀𝑁 0.135×123.11
𝑤𝑒𝑖𝑔ℎ𝑡 𝑟𝑎𝑡𝑖𝑜 = ° = 3.689 × 18
= 0. 25
𝑃𝑊 × 𝑀𝑊
 ● Extract-1,
Volume of nitrobenzene ( 𝑉𝑁) = 10ml.
𝑊𝑁 = ρ𝑁* 𝑉𝑁 = 1.2*10 = 12g
Volume of nitrobenzene ( 𝑉𝑊) = 58ml.
𝑊𝑊 = ρ𝑊* 𝑉𝑊 = 0.997*58 = 57.826g
𝑊𝑁 12
𝑊𝑊
= 57.826
= 0. 208.
Similarly we can find the weight ratio for extract 2, Calculation is given in the attached
excel sheet.

Weight Weight W(A) / P(A)*M(A)

Nitrobenzene (in gm) Water (in gm) W(B) P(A) P(B) /(P(B)*M(B)) Error %

Extract 1 12 57.826 0.208 0.135 3.689 0.25 16.8

Extract 2 6 34.895 0.172 0.135 3.689 0.25 31.2

Table 3: Calculation Table

Plots:

Plot 1. Graph of Temperature of mixture vs time(min).

● Theoretical weight ratio = 0.25

● Experimental weight ratio = 0.208 (Extract 1) and 0.172 (Extract 2).
Precautions & Possible sources of errors
● While preparing the solution, make sure that the amount of water and
nitrobenzene is exactly the same as required.
● After pouring the solution into the flask, tightly join the flask & condenser such
that there is no leakage of vapor.
● Make sure that heater is set at desired voltage (~40 V).
● While noting down the temperature of the solution, make sure that you have
taken the readings accurately.
● While taking the volume readings once Nitrobenzene settles at the bottom, make
sure to gently place the measuring cylinder on the table, so that there is no
disturbance in the mixture.
● When condensed vapor is collected in a cylindrical vessel, put it away once it
reaches the 40 ml. This is one of the major sources of error in our case since the
collected solution was overflowed and was around ~ 70 ml.
● While measuring the 40 ml level of the condescending vapor, make sure that
there are no bubbles remaining at the surface of the vessel. This can also cause a
potential amount of error in the results.

Discussion
Through this experiment, we were able to use steam distillation to successfully find the
weight fraction of the two immiscible components in the product obtained. The volume
of nitrobenzene gathered in the final two extracts was also examined and measured.
According to our calculations, the weight ratio of nitrobenzene to water for extracts 1
and 2 was 0.208 and 0.172, respectively. The weight ratio, 0.25, was also calculated
theoretically using partial pressure and molar mass knowledge. As a result, while extract
2 showed divergence, one of our extracts was near to the theoretical value.

We can easily determine the weight ratio of the components in steam distillation by
carrying out this experiment. It is clear that there is more water in the distillate than
nitrobenzene. Because water is more prone to evaporate, we can infer that it has a lower
boiling point than nitrobenzene. Overall, the steam distillation process was effectively
studied, and the relationship between vapor pressure and mole fraction of immiscible
liquids was understood.
Conclusion
In conclusion, the experiment was a success in showing how steam distillation works
and how to use it to find the weight fraction of immiscible mixtures of organic
molecules with higher boiling points. The weight ratio of nitrobenzene and water that
was calculated experimentally deviates from the theoretical results obtained using
Rault's law for a number of reasons, including the presence of bubbles on the cylinder
wall, the mixture's less-than-ideal behavior, and other practical constraints encountered
during the experimental procedure. The experimental findings demonstrate that the
purification of volatile organic molecules using steam distillation is a delicate and
successful process without exposing them to high temperatures that can harm or
change their chemical properties.
Steam distillation is used in the following industrial processes: crude oil refineries,
pharmaceuticals , alcoholic drinks, extraction of dairy tastes from dairy products,
purification of fatty acids from mixtures.

References:

● Excel Sheet used for calculation - Exp-5_Group-C

● Antoine Coefficient-

-“Benzene, Nitro-.” Benzene, Nitro-,

webbook.nist.gov/cgi/cbook.cgi?ID=C98953&Mask=4&Type=ANTOINE&P
lot=on.

-“Water.” Water,
webbook.nist.gov/cgi/cbook.cgi?ID=C7732185&Mask=4&Type=ANTOINE
&Plot=on.

● “Steam Distillation- How It Actually Works?” Chemistry Stack Exchange, 12 Mar.

2014,
chemistry.stackexchange.com/questions/9130/steam-distillation-how-it-actually-
works.
● “5.5D: Step-by-Step Procedures for Steam Distillation.” Chemistry LibreTexts, 11
Aug. 2020,
chem.libretexts.org/Courses/SUNY_Oneonta/Chem_221%3A_Organic_Chemistry
 _I_(Bennett)/2%3ALab_Textbook_(Nichols)/05%3A_Distillation/5.05%3A_Steam_
Distillation/5.5D%3A_Step-by-Step_Procedures_for_Steam_Distillation.

Contribution:

Sakshi Jain Experiment: Observations and Readings,

Report: Theory, Procedure, Discussion and
Conclusion

Rajesh Kumar Experiment: Observations and Readings,

Report: Abstract, Discussion and Conclusion,
References, Sample Calculation

Shreyansh Chourasiya Experiment: Observations and Readings,

Report: Calculation, Results, Discussion and
Conclusion

Ayush Bhalala Experiment: Observations and Readings,

Report: Precaution, Sources of error,
Discussion and Conclusion, Diagram