CLP302 - MT (SG 6) - Merged (1) 2

CLP302: Mass Transfer and Fluid Particle Mechanics Lab
Semester II: 2021 - 2022
Experiment Name Vapour Liquid Equilibria
Group Day Tuesday
Subgroup Number 6
Date / day of submission Tuesday, 7th February 2022
Date / day of common doubt Tuesday, 1st February 2022

session for experiment
Names of group members Hemant Prakash Singh (2019CH70172)

Vinayak Dixit (2019CH70202)
Divyansh Garg (2019CH70166)
Amit Kumar (2019CH70158)
Opal Harinkhere (2019CH10111)
Name of lab instructor Prof. A.N. Bhaskarwar
Marks (to be filled by instructor/TA)

VAPOUR LIQUID EQUILIBRIA
Objective:
To determine the vapour-liquid equilibrium curve for the ethanol-water mixture and
compare it with the VLE data.
Experimental Setup:
The experimental setup consists of a round bottom flask with three ways open at the
top and opened at the bottom. The reboiler is heated by a heating mantle with a
capacity of 1 litre. The reboiler is equipped with a vapour rising and reflux system, as
well as a reflux tube with condensate and sampling. The vapour is condensed using
a spiral glass tube condenser. Two thermocouples are given to measure the liquid
and vapour temperatures, and an above tank is provided to circulate condenser
cooling water.
Requirements:
● Water
● Ethanol
● Digital Refractometer
Figure-1: Experimental setup

Theory:
Mass transfer operations are a very essential part of all industries as evident from
the fact that at almost every step of any process there is a separation or transfer of
one material from one phase to another in steps like purification, preparation of new
mixtures, materials and final products and so on. Inherently a lot of processes thus
involve mass transfer of one material from one phase to another, for example to
separate a mixture of acetone and water, we first partially evaporate the solution and
then condense the vapours obtained (rich in acetone, more volatile than water) to
achieve separation. So, ultimately a change in composition is achieved and the
components are differently distributed across the phases as determined by the
equilibrium they attain. The amount of separation or equivalently the change in
composition achieved is the variable which are we concerned about.
The driving force for the mass transfer is ultimately the difference in chemical
potential or equivalently how far the current state is from equilibrium. Now
equilibrium is a dynamic state of the system post which we see no change in the
system parameters (macroscopic) as time passes by. The attainment of equilibrium
also indicates that the chemical potentials are now balanced. Coming to the system
of interest, we have an isolated vessel or system that has vapours and liquid in it
(two different phases). If they are not at equilibrium initially, then the system will
undergo a change in composition of the phases so that the amount of liquid
vaporising will be equal to the amount of the vapour condensing so that no change in
composition will be observed (both the fluxes are equal).
Let us now consider a liquid-vapour system that has two different chemical species
in it. From the Gibbs Phase Rule, F = C - P + 2, we can observe that the system has
2-2+2 ⇒ 2 degrees of freedom or the system can be characterised totally by 2
independent thermodynamic variables when they are made constant. For sake if we
keep the temperature and pressure of the system constant, the compositions of both
the phases can easily be found.
The curves given below were made by tabulating the data of composition of the
phases at a fixed pressure and varying temperature. yi represents the mole fraction
in the gas phase and xi represents the mole fraction of the component i in the liquid
phase. As we can see, there are two lines in the curves plotted, the upper one in
each of them is called the bubble line or the saturated vapor line and the below one
is called the saturated liquid line or the dew line.
Above graph shows the variation between the gas phase composition and the liquid
phase compositions at a given pressure when either one of them is kept constant.
This particular behaviour was approximated in the form of Henry’s Law and Raoult's
Law.
Henry’s Law
This law states that the amount of gas dissolved in a liquid is proportional to the
partial pressure present above the liquid and the proportionality constant involved is
called the Henry’s constant denoted by H.
𝑃1 = 𝑥1 𝐻
where P1 is the partial pressure of the vapor and x1 is the composition of the
component in the dissolved liquid.
This when combined with the Dalton’s law or Ideal gas equation gives
𝑦1 𝑃𝑡 = 𝑥1 𝐻
Here y1 is the mole fraction of components in the vapor phase and PT is the total gas
pressure.
Raoult’s Law
This law states that the partial pressure of each component of an ideal mixture of
liquids is equal to the vapour pressure of the pure component multiplied by its mole
fraction in the mixture.
𝑃1 = 𝑥1 𝑃1, 𝑣𝑎𝑝
Where P1 and x1 are the partial pressure and mole fraction of the component in
vapour phase and P1,vap is the vapour pressure of the component.
𝑦1 𝑃𝑡 = 𝑥1 𝑃1, 𝑣𝑎𝑝
As can be inferred this law predicts a linear relation between the liquid and the gas
phase compositions at equilibrium. It should be noted that this law is valid only for
ideal mixtures of liquid.
When one of the variables is fixed at a constant pressure, the graph below depicts
the volatility of y with x. Raoult's and Henry's Laws could be used as models for this
x-y behaviour.
Procedure:
Preparing the calibration chart
● Take out 10 mole % of water and 90 mole% of Ethanol and mix the contents
well, after that calculate the refractive index of that mixture.
● Make another sample by taking out 30 mol% of water and 70 mole % of index
and also calculate the refractive index of this mixture.
● Make a table 1 in which keep noting the change in refractive index by
changing the concentration.
● Once generated , the calibration chart can be used repeatedly.
Experiment setup based procedure

● Prepare a mixture of water and ethano;l containing 50 mol% of ethanol with
volume of 500 ml and feed it to the vapor liquid equilibrium apparatus.
● Boil the mixture to distil it. Recycle the vapour at least 30 minutes to achieve
equilibrium between the liquid and vapour phases.
● Take the samples at the temperature specified . allow them to cool to the
room temperature and determine their Refractive Index (RI).
● Repeat the previous step for the next batch of samples.
Procedure to use the refractometer

● Using a few drops of distilled water fill the sample well of the refractometer
and then press the zero button.
● Using a dropper take the sample and put 1-2 drops on the sample well of the
refractometer.
● Close the sample well covered.
● Now, push the read button to obtain the refractive index value.
Method:
Observations Table:
Calibration Chart of Water and Ethanol mixture
S.No. Mole % of Ethanol Mole % of Water Refractive Index
1 0 100 1.3345
2 10 90 1.3465
3 20 80 1.3521
4 30 70 1.3553
5 40 60 1.3573
6 50 50 1.3581
7 60 40 1.3584
8 70 30 1.3585
9 80 20 1.3586
10 90 10 1.3586
11 100 0 1.3592
Vapour Liquid Equilibrium

Refractive Index
o
Reading Sets Vapor Temperature ( C)
Vapor Sample Liquid Sample
86.4 1.3592 1.3376

16 85.3 1.3589 1.3395
86.7 1.3586 1.3387
Calculations:
Using the calibration data, the calibration curve is plotted which relates the
composition of ethanol in ethanol-water solution to its refractive index.
Using the above calibration curve, the mole fraction or the mole % of ethanol in liquid
and vapour state can be easily determined.
For example, at T = 85.3 oC,

The refractive index of the vapor sample is 1.3589. The corresponding mole % of
ethanol in the sample is 95% or y1 = 0.95 (by simply looking at the curve and finding
from it).
Similarly, the refractive index of the liquid sample is 1.3376. The corresponding mole
% of ethanol in the sample is 2.4% or x1 = 0.024.

Vapor Vapor Sample Liquid Sample
Temperature Mole Fraction of Mole Fraction of
Refractive Index Refractive Index
(oC) Ethanol (y1) Ethanol (x1)
86.4 1.3592 1 1.3376 0.024
85.3 1.3589 0.95 1.3395 0.04
86.7 1.3586 0.8 1.3387 0.032
The T-x-y data is shown in a separate table below:
T (oC) y1 x1
86.4 1 0.024
85.3 0.95 0.04
86.7 0.8 0.032
Using the above data, the y-x plot can be made for our VLE system.
The theoretical data for VLE in Ethanol and water system is obtained from literature:
Best model and data parameters for T-x-y equilibrium of ethanol-water mixture
T(℃) x y
95.5 0.019 0.17
89 0.0721 0.3891
86.7 0.0966 0.4375
85.3 0.1238 0.4704
84.1 0.1661 0.5089
82.7 0.2337 0.5445
82.3 0.2608 0.558
81.5 0.3273 0.5826
80.7 0.3965 0.6122
79.8 0.5079 0.6565
79.7 0.5198 0.6599
79.3 0.5732 0.6841
78.74 0.6763 0.7385
78.41 0.7472 0.7815
78.15 0.8943 0.8943
Results:
Error Analysis:
● The data given in the experiment is highly inaccurate and unrealistic. For
example, at 86.4 oC, the composition of ethanol in vapor phase is 1 which is
practically impossible to achieve. y = 1 means that pure ethanol is obtained on
distillation and none of the water has gone into vapor phase which is ofcourse
not true because water is also volatile.
● For very small values of x, y is coming out to be very high and also, y does
not increase every time when x increases (which is true according to theory).
Error in x
Temperature(℃) 𝑥𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 x error(%)

𝑥−𝑥𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙
( 𝑥𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙
* 100)
86.4 0.1024 0.024 76.59
85.3 0.1238 0.04 67.68
86.7 0.0966 0.032 66.87

Error in y
Temperature(℃) 𝑦𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 y error(%)

𝑦−𝑦𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙
( 𝑦𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙
* 100)
86.4 0.4445 1 124.97
85.3 0.4704 0.955 103.01
86.7 0.4375 0.8 82.85

Average error % in x = 70.38
Average error % in y = 103.61%
The main reasons for this error are:

1. The lid of the refractometer might not be completely closed while taking
the readings.
2. The system might not be at equilibrium when the readings are taken.
3. The measuring instruments might not be calibrated or stored properly.
4. The refractometer might be a little dirty while taking the readings,
causing measurements to be skewed.
5. Finally, due to carelessness or irregularity while taking the readings of
temperature and refractive index might also be the reason for the error.
Discussion and Conclusion:

The data for the experiment given is very inaccurate and unrealistic, which gives us
wrong results as shown above in the graph. Average error % in X is ~70% and error
% in Y is ~100%.
1. What is the conclusion of the experiment? Is the objective fulfilled?

- As the experiment's results do not completely agree with theoretical value, no
definite conclusion can be reached. However, based on the data we know,
experiment and theory are in disagreement, as evidenced by the VLE curve.
From the VLE curve obtained we get a very different plot for experimental
values compared with theoretical value, thus the result for the experiment
cannot be concluded and theory can’t be verified.
2. Give a physical interpretation of your results.

- In processes involving interphase mass transfer, the y vs. x equilibrium curve
is a particularly helpful plot. They are often employed in various contacting
equipment such as stagewise contact in cocurrent, counter-current, and
cross-current forms to determine interfacial concentrations, overall mass
transfer coefficients of the liquid and vapour sides, and material balance. This
information can also be used to comprehend any non-ideality connected with
the interactions of the two components, leading to more accurate modelling
techniques such as modified Raoult's law, which also takes deviations from
ideality into account. But in this experiment our result couldn’t verify the
theory. We got a very different experimental plot in comparison to the
theoretical plot.
3. Compare your results with those obtained from theory/literature. Justify

the differences in these, if any.
- The experimental and theoretical results show a very large difference. We
cannot establish a meaningful comparison because there are only a few data
points available for tests. To comment, the inaccuracies that occur due to the
use of the linear interpolation approach are the cause of the deviation as
calibration chart does not have values for ethanol mole fraction between 0
and 0.1, so linear interpolation in this range to find mole fraction from
refractive index values for liquid sample is giving large error.
Another reason is that the data given in the experiment is highly inaccurate
and unrealistic. For example, at 86.4 oC, the composition of ethanol in vapor
phase is 1 which is practically impossible to achieve. y = 1 means that pure
ethanol is obtained on distillation and none of the water has gone into vapor
phase which is ofcourse not true because water is also volatile.
4. What is the Equilibrium Phase rule? What are the free and the
dependent variables in this experiment?
- The Equilibrium Phase Rule is a governing principle for thermodynamic
systems at equilibrium. It defines the degree of freedom for a closed system
that can be calculated as:
F=C-P+2
Where,
F= Number of degrees of freedom
C = Number of components
P = Number of phases
Free or Intensive Variables are the ones that are independent of the total
mass of the system while dependent or extensive variables depend on the
mass of the system. In out experiment, the free variables are Temperature (T)
and Mole Fraction in liquid phase (x) while dependent variables are Mole
Fraction in vapour phase (y) and Refractive Index (R.I)
5. Define bubble point and dew point.

- In thermodynamics, at any given pressure when the liquid that consists of
more than one component is saturated i.e. saturation point is achieved and
the first bubble of vapor is formed, this temperature is known as bubble
point.
Dew Point is the temperature to which the air is cooled so that it becomes
saturated with water vapor. When it is cooled further, the first liquid drop is
formed due to condensation. As the composition of vapor and liquid are
different, the calculation of bubble point and dew point for different
compositions can be useful for designing distillation systems.
6. Describe in brief how the interactions between the components affect

the vapor liquid equilibrium.
- The interactions between the components can have a great effect on the
vapor liquid equilibrium. Let's take a binary mixture, if the interaction between
1-2 components is greater than that of between 1-1 and 2-2, then the mixture
will have less vapour pressure and it will result in a negative deviation from
the Raoult’s Law for ideal mixture. In contrast, if the interaction between 1-1
and 2-2 is greater than that of 1-2 components, then this will result in a
positive deviation.
Also, in our experiment it has been observed that the ethanol - water mixture
exhibits positive deviation
Hence, it can be shown that the interaction between components is
considerable in VLE.
a. Positive deviation
b. Negative deviation
7. Is it always possible to obtain a pure component using a distillation
process? Why/why not?
- Distillation is the process to separate components of a liquid mixture by
performing selective evaporation and condensation steps. This process
makes use of different boiling points of different components. During
distillation, once the thermodynamic equilibrium is attained, the liquid
evaporates and the liquid's surface is the phase boundary. On increasing
pressure, components boil but due to VLE, liquid phase is maintained. So, on
condensing the gas mixture, condensed liquid is not pure. For example, the
mixture of ethanol and water forms a minimum-boiling azeotropic mixture at
89.4 mole% ethanol at 78.15 ℃, it is not possible to obtain a product richer
than 89.4 mole% ethanol using conventional distillation. To obtain a relatively
pure ethanol, azeotropic distillation can be performed.
Some more examples includes liquid mixture that contains organic liquid
having boiling point < 150℃, it's not possible to obtain pure component using
distillation because of decomposition .Also, when a non-volatile component is
present with boiling points separated by less than 70℃ fractional distillation at
atmospheric pressure is employed.
Scope of Improvement:
1. More data points can give results which are more comparable with the
literature.
2. The measurement of the refractive index to determine the concentration of
ethanol in the solution resulted in wrong results many times. We may have an
alternative method to measure to find concentration.
3. To calibrate the refractometer, a greater range of mole percent of ethanol and
water should be used to have a value with less fluctuation.
Precautions:
1. Ensure that the valves are correctly closed as necessary to avoid leaks.
2. Before switching the heat on make sure that the mixture inlet valve is closed.
3. The voltage must be kept constant throughout the experiment free from
variation.
4. Clean the sample well of the digital refractometer with dry tissue paper to
remove dust particles.
5. Only take reading refractometer valves , after achieving a stable reading.
Experiment Name Mass transfer with and without chemical

reaction
Group Day Tuesday
Subgroup Number 6
Date / day of submission Tuesday, 18th January 2022
Date / day of common doubt Tuesday, 11th January 2022



MASS TRANSFER WITH AND WITHOUT CHEMICAL REACTION
Objective:
1. To study the dissolution of benzoic acid in aq. NaOH solution
2. To calculate the enhancement factor comparing Mass Transfer Coefficient of
with and without chemical reaction dissolution.
Experimental Setup:
The apparatus where the reaction will happen is a reactor tank. The solvent is made
in a form of cylinder which will dissolve in the solvent present in the reactor with the
help of a rotating rod.For maintaining the reactor's temperature, a water bath with a
stirrer and a heat source has been supplied.
Materials Required:
1. Benzoic Acid
2. NaOH solution
3. Indicators (Phenolphthalein and Methyl Orange)
4. HCl
Theory:
Molecular diffusion is the movement of molecules (of liquid and gas) under the
influence of a concentration gradient by the help of their thermal energy which they
possess at all temperatures above absolute zero or 0 K. Some of the factors on
which it is dependent are namely Size of moving entities, Temperature and Viscosity.
The process of dissolution (mixing of solid and liquid) is also dependent on molecular
diffusion. But in this case as the molecular size is large so the process is inherently
slow and so for better and optimal results in industrial usage the movement is
enhanced by giving the additional help of bulk flow.
Now as the mass transfer is also influenced by the interactions of solid and liquid
reactants in the dissolution process so for better understanding of the phenomenon
the mass transfer is classified into two types- one in which there is no chemical
reaction and the other in which there is chemical reaction and these can be further
understood better by Film theory and Boundary Layer Theory concepts.
Let A be the solid reactant and B be the liquid reactant and the process comprises of
A dissolving into B and then reacting with B instantaneously and the reaction be
represented as follows
A + nB → products
A dissolves into B and then reacts with it at the reaction interface while B is present
in the space from the interface to the rest of the beaker where liquid is present and it
diffuses from bulk to interface.
By using film theory, the enhancement factor is given by solid liquid mass transfer
coefficient with reaction divided by the mass transfer coefficient without reaction.
where [A* ] is the (saturation) concentration of A at the solid-liquid interphase, [Bo] is

the bulk concentration of B.
If boundary layer model is used then

Procedure:
1. Measure the weight of the cylinder steel rod and take it as Wi.
2. Measure the steel rod's dimensions.
3. Place the rod in the dice set's middle and fill it with Benzoic Acid until it
reaches the top.
4. Compress the cake by closing the die set.
5. Take the cake out of the oven and weigh it, Wf.
6. First, use the dye set to prepare the benzoic acid cylinder.
7. Determine the cake's measurements.
8. Fill the jar with deionized water with a specified concentration and record the
volume of deionized water supplied (V).
9. Turn on the water bath heater and set the temperature for dissolving.
Otherwise, carry out the experiment at room temperature and record the
results.
10. Place the Benzoic acid cake in the deionized water vessel, activate the motor,
and adjust the rotating speed (N, rpm).
11. Run the experiment for a predetermined amount of time, such as 10–15
minutes.
12. Turn off the motor and take out the benzoic acid cake.
13. Thoroughly mix the contents of the vessel and titrate against a standard
NaOH solution for dissolved Benzoic Acid concentration (use Phenolphthalein
indicator).
14. Repeat the procedure with various amounts of aqueous Benzoic Acid
solution.
15. In the reactor, repeat steps 1–14 with an aqueous NaOH solution of known
concentration. Titrate the samples against a standard HCl solution to
determine the amount of unreacted NaOH (use Methyl Orange indicator).
Method:
Observations:
For Mass Transfer without reaction

● Diameter of rod, dr = 0.007 m
● Length of rod, Lg = 0.163 m
● Temperature, T = 50 °C
● Speed of motor = 120 rpm
● Diameter of Cake, Dav = 0.0337 m
● Length of Cake, Lav = 0.0438 m
● Volume of water in the reactor, V = 1.6 x 10-3 m3
● Volume of sample taken for titration, V1 = 10 ml
● Concentration of NaOH (N2) = 0.01 N
● Indicator = Phenolphthalein
Time (min) Volume of Std. NaOH used for 10 ml of soln (V2)
10 8.3
20 9.9
30 11.2
40 13
For Mass Transfer with reaction

● Diameter of rod, d´r = 0.007 m
● Length of rod, L´g = 0.163 m
● Temperature, T = 50 °C
● Speed of motor = 120 rpm
● Diameter of Cake, D´av = 0.032 m
● Length of Cake, L´av = 0.04246 m
● Volume of NaOH in the reactor, V´ = 1.6 x 10-3 m3
● Initial Concentration of NaOH = 0.01 N
● Volume of sample taken for titration, V'1 = 10 ml
● Concentration of HCl (N'2) = 0.01 N
● Indicator = Methyl orange
Time (min) Volume of Std HCl used for 10 ml of soln (V'2)
10 6.3
20 5.1
30 3.7
40 0.8
Calculations:
● Mass Transfer without Chemical Reaction
Average surface area of Cake

(Aav) = π𝐷 𝐿
𝑎𝑣 𝑎𝑣
+ 2 ×
⎣ 4 ( )
⎡⎢ π (𝐷2 − 𝑑2 )⎤⎥
𝑎𝑣 𝑟 ⎦
(Ap) = π𝐷 𝐿 = 3.14*0.0337*0.0438
𝑎𝑣 𝑎𝑣
= 0.004634 m2
(Aav) = 0.004634 + 2*[(3.14/4)*({0.0337}2 - {0.007}2)]
= 0.006341 m2
Aav = 6.341 x 10-3 m2
The mass balance gives the following relation for change in benzoic acid
concentration with time
𝐴𝑎𝑣 𝐶
𝑘 𝑡= − 𝑙𝑛⎡1 − ⎡ 𝐶* ⎤⎤
𝑉 ⎣ ⎣ ⎦⎦
To calculate Concentration of Benzoic acid (C) at time (t), we will use mole
balance equation at neutralisation point.
𝑁1 × 𝑉1 = 𝑁2 × 𝑉2
𝑉2
𝑁1 = 𝐶 = 𝑁2 × 𝑉1
Where,
N - normality,
V - volume,
1 - sample of benzoic acid taken for titration (V1 =10 ml),
2 - Standard NaOH used for titration (N2= 0.01N, V2 - given in reading)
Solubility of benzoic acid in water at 50 ℃ is

C* = 0.0682 kmol/m3 = 0.0682 mol/L
At t = 10 minutes
𝐶 = 𝑁2 × ( )
𝑉2
𝑉1
= (0.01)*(8.3/10) = 0.0083 mol/L
𝐶
𝐶*
= 0.0083/0.0682 = 0.1217
− 𝑙𝑛⎡1 −
⎣ ( )⎤⎦ =− 𝑙𝑛[1 − 0. 1217] = 0.1298
𝐶
𝐶*
At t = 20 minutes
𝑁1 = 𝐶 = 𝑁2 × ( )
𝑉2
𝑉1
= (0.01)*(9.9/10) = 0.0099 mol/L
𝐶
𝐶*
= 0.0099/0.0682 = 0.1452
− 𝑙𝑛⎡1 −
⎣ ( )⎤⎦ =
𝐶
𝐶*
− 𝑙𝑛[1 − 0. 1452] = 0.1568
Volume of Std. NaOH

Time Time
(min)
used for 10 ml of soln
(V2)
(sec)
C = N2* V2/V1
𝐶
𝐶*
− 𝑙𝑛⎡1 −
⎣ ( )⎤⎦
𝐶
𝐶*
10 8.3 600 0.0083 0.1217 0.1298

20 9.9 1200 0.0099 0.1452 0.1568
30 11.2 1800 0.0112 0.1642 0.1794
40 13 2400 0.013 0.1906 0.2115
(0.2115−0.1298) −5
Slope = (2400−600)
= 4. 54𝑥10 s-1
We know,
𝑘𝐴𝑎𝑣
𝑆𝑙𝑜𝑝𝑒 = 𝑉
𝑆𝑙𝑜𝑝𝑒 * 𝑉
𝑘= 𝐴𝑎𝑣
Therefore,
Aav = 6.341 x 10-3 m2
V = 1.6 x 10-3 m3 (Volume of water in reactor)
−5 −3
4.54𝑥10 * 1.6𝑥10 −5
𝑘= −3 = 1. 145𝑥10 m/s
6.341𝑥10
k = 1.145 x 10-5 m/s
● Mass Transfer with Chemical Reaction
Average surface area of Cake

(A’av) = π𝐷' 𝐿'
𝑎𝑣 𝑎𝑣 ⎣
π
( ) 2 2
+ 2 * ⎡⎢ 4 (𝐷' 𝑎𝑣 − 𝑑' 𝑟)⎤⎥
⎦
(A’p) = π𝐷' 𝐿'
𝑎𝑣 𝑎𝑣
= 3.14*0.032*0.04246
= 0.004266 m2
(A’av) = 0.004266 + 2*[(3.14/4)*({0.032}2 - {0.007}2)]
= 0.005796 m2
A’av = 5.796 x 10-3 m2
Reaction
C6H5COOH + NaOH → C6H5COONa + H2O
Formula Used:
𝐶−𝑂
𝑅' = 𝑇
𝑉'
Where,
C = initial concentration of NaOH in the feed tank,
O = Concentration of NaOH at time T,
V’ = Volume of water in reactor
To calculate Concentration of NaOH at time (T), we will use mole balance

equation at neutralisation point.
𝑁'1 × 𝑉'1 = 𝑁'2 × 𝑉'2

𝑉'2
𝑁'1 = 𝑂 = 𝑁'2 × 𝑉'1
Where,
N’ - normality,
V’ - volume,
1 - sample of benzoic acid taken for titration (V’1 =10 ml),
2 - Standard HCl used for titration (N’2= 0.01N, V’2 - given in reading)
Solubility of benzoic acid in water at 50 ℃ is

C* = 0.0682 kmol/m3 = 0.0682 mol/L
At time t = 10 min
𝑉'2
𝑁'1 = 𝑂 = 𝑁'2 × 𝑉'1
= (0.01)*(6.3/10) = 0.0063
𝐶 −𝑂
R’ = 𝑇
V’ = (0.01 - 0.0063)*(1.6x10-3)/(600) = 9.87x10-9 kmol/s
At time t = 20 min
𝑉'2
𝑁'1 = 𝑂 = 𝑁'2 × 𝑉'1
= (0.01)*(5.1/10) = 0.0051
𝐶 −𝑂
R’ = 𝑇
V’ = (0.01 - 0.0051)*(1.6x10-3)/(1200) = 6.53x10-9 kmol/s
Concentration of
Time Volume of Std. HCl used Time 𝐶 −𝑂
NaOH at time (t) R’ = V’
(min) for 10 ml of soln (V'2) (sec) 𝑇
O = N’2*V’2/V’1
10 6.3 600 0.0063 9.87E-09
20 5.1 1200 0.0051 6.53E-09
30 3.7 1800 0.0037 5.60E-09
40 0.8 2400 0.0008 6.13E-09
R’Avg 7.03E-09
−9 −9 −9 −9
9.87𝑥10 + 6.53𝑥10 + 5.60𝑥10 + 6.13𝑥10 −9
R’Avg = 4
= 7. 03 × 10 kmol/s
Specific rate of dissolution

𝑅'𝐴𝑣𝑔
𝑅= 𝐴'𝑎𝑣
kmol/m2s
−9
7.03 × 10
𝑅= −3
5.796 × 10
R = 1.212 x 10-6 kmol/m2s
The experimental value of the enhancement factor can be calculated as:

𝑅
ϕ𝑒𝑥𝑝 = 𝑘𝐶*
Where,
R is the specific rate of dissolution with reaction
k is mass transfer coefficient without reaction
( ) = 1. 552
−6
𝑅 1.212×10
ϕ𝑒𝑥𝑝 = 𝑘𝐶*
= −5
1.145𝑥10 ×0.0682
Φexp = 1.552
● Theoretical enhancement factor
Diffusion coefficient of Benzoic acid in mixture DA = 10-9 m2/s

Diffusion coefficient of NaOH in mixture DB = 5.79 x 10-9 m2/s
Bulk Concentration of NaOH [B0] = 0.01 mol/L
Saturation concentration of Benzoic Acid [A*] = 0.0682 mol/L
nB = 1
𝐷𝐴 10
−9
1
𝐷𝐵
= −9 = 5.79
5.79𝑥10
Enhancement factor using film theory:
𝐷𝐵[𝐵0]
ϕ𝑓𝑖𝑙𝑚 = 1 + 𝐷𝐴𝑛𝐵[𝐴*]
0.01𝑥5.79
ϕ𝑓𝑖𝑙𝑚 = 1 + ⎡ ⎤ = 1.8940
⎣ 0.0682 ⎦
Φfilm = 1.8940
Enhancement factor using boundary layer model:
1/3 2/3
ϕ𝐵 = ( ) ( )
𝐷𝐴
𝐷𝐵
+
𝐷𝐵
𝐷𝐴
[𝐵0]
𝑛𝐵[𝐴*]
1/3
ϕ𝐵 = ( )1
5.79
+ (5. 79)
2/3 0.01
0.0682
= 1.0297
ΦB = 1.0297
Results:
1. The mass transfer coefficient without reaction (k) = 1.145 x 10-5 m/s
2. The specific rate of dissolution with reaction (R) = 1.212 x 10-6 kmol/m2s
3. The value of the observed enhancement factor (Φexp) is 1.552
4. Enhancement Factor
Calculation Methodology Enhancement factor ϕ
Observed 1.5520
Theoretical Film Theory 1.8490
Theoretical Boundary Layer Model 1.0297
Error Analysis:
[𝑇ℎ𝑒𝑜. 𝑣𝑎𝑙𝑢𝑒 − 𝐸𝑥𝑝. 𝑣𝑎𝑙𝑢𝑒]

%𝐸𝑟𝑟𝑜𝑟 = 𝑇ℎ𝑒𝑜. 𝑣𝑎𝑙𝑢𝑒
Observed Value Theoretical value % Error
1.5520 Film Theory 1. 8490 16.06
1.5520 Boundary Layer Model 1.0297 50.72
We can see from the preceding data that the Experimental value differs
significantly from the Boundary layer model value when compared to the Film
theory value. This inaccuracy may emerge due to uneven pore size and
spaces in the benzoic acid cylinder created during compression, as well as
non-uniform mixing in the reactor and temperature variations. As a result,
we've received inaccuracies in our experimental value. The film theory value
has less inaccuracy because the resistance to mass transfer in a particular
fluid phase is present in a thin layer next to the reaction interface.
1. The effect of temperature on mass transfer coefficient.

The mass transfer coefficient increases with temperature because the
molecules have a significantly greater vibrational frequency and kinetic rate
constant, resulting in more collisions and a faster rate of transfer. At the
molecular level, this is mirrored by an increase in molecular diffusivity DAB.
The reaction temperature is kept at 50 oC in the described dissolution
reaction, which is significantly above room temperature. With a higher
saturation concentration, this assures effective mass transfer.
The Sherwood’s number rises as the temperature rises. This indicates that
convective mass transfer is dominating, implying a higher mass transfer
coefficient.
2. Any five Industrial applications of dissolution reaction.

A. Dissolution of agglomerated water soluble powders such as tea,coffee,
milk powder, and so on in the food industry.
B. Sodium silicate, commonly known as water glass, is utilised in a variety
of industries, including construction, as a detergent binder and
adhesive, and as a flocculant in water treatment plants. To make a
viscous syrupy liquid water glass is dissolved in hot water under
pressure.
C. Dissolution rate ensures the amount of drug substance released per
unit time in the pharmaceutical industry. It investigates the performance
and stability of novel formulations and is used as a quality control tool
from batch to batch.
D. In Hydrometallurgy Industry the metal is extracted out from metal ore
using an aqueous solution performing dissolution reaction.
E. Solvolysis of Bituminous Coal is an alternate method of producing coal
tar.
3. Additional inferences from the experiment.

A. The experimental value of enhancement factor is obtained to be
greater than 1 which indicates that mass transfer with reaction is faster
as compared to that without reaction which is due to the fact that
concentration at the interface keeps getting lower due to chemical
reaction which increases the concentration gradient (driving force for
mass transfer) and so the mass transfer increases
B. The experimental value is closer to the theoretical value predicted from
the film theory model and the observed value is very close to the
average value of film and boundary layer values.
C. Both the models agree to the fact that mass transfer with reaction is
fast and this is also verified experimentally
4. Other methods used to measure concentration of solutions.

A. Spectrometry: With a changing solute concentration, the absorption
spectra of a solution will yield a different optical density of the solution.
As a result, concentration can be determined using absorbance
measurement.
B. Conductivity of solutions: A calibration curve of conductivity vs solute
concentration can be drawn, and the concentration can then be
determined from the conductivity of solution using the inverse
relationship. The equipment, on the other hand, is complicated and
prone to faults.
1. Making sure the temperature of the reaction beaker is constant as the mass
transfer coefficient is temperature dependent. This can be done by process
control systems or putting the beaker in a cold water bath
2. Measuring the height of the meniscus at the tangent drawn to the surface
3. The titration should be carried out carefully making sure that the burette drops
the liquid drop by drop only because any threshold gives color change with
the indicator
4. Despite all the measures taken mixing won't be uniform in the beaker which is
contradictory to the assumption taken that conditions are uniform throughout
the reaction mixture
5. Some amount of human error is unavoidable forsake in measuring the
dimensions of rod, volumes of samples collected along with preparing
solutions of a required concentration
6. Heat released in the acid base reaction will lead to non uniformity of
temperature in the beaker which will lead to variable mass transfer coefficient
7. One of the starting assumptions that reaction is instantaneous (to remove the
possibility of coexistence), but in reality it won't be as the acid is relatively
weak
8. Uneven pore size and air gaps in the acid cake may lead to faulty calculations
9. Presence of dead zones in the beaker can lead to non uniform base
concentration in the beaker
Sources of Error:
1. Parallax error in burette reading.
2. Improper cake compression and insufficient mixing but we have assumed
uniform mixing for the experiment.
3. Due to incorrect mixing, heat from neutralisation will be discharged, and the
temperature of the reactor will fluctuate in the reactor tank, and MTC is a
strong function of temperature.
4. Using uncleaned and faulty equipment or apparatus.
5. It's possible that we got a neutralisation point during the titration because we
didn't adequately stir the sample collected in the conical flask or beaker.
Precautions:
1. To avoid distortion of the Benzoic Acid cylinder, fix the rod within the die
vertically.
2. Before beginning the experiment, wash the burettes and beakers.
3. Ensure that the samples are well mixed before titration.
4. The stirrer's speed should not be too high and should be the same for both
portions.
5. Try best to ensure that all the reaction parameters are as uniform as possible
Experiment Name Adsorption in packed bed
Group Day Tuesday
Subgroup Number 6
Date / day of submission Tuesday, 31st January 2022



ADSORPTION IN PACKED BED
Objective:
To study Adsorption in a packed bed for a Solid-Liquid system and to find the
breakthrough curve and the length of unused bed.
Experimental Setup:
The device is designed for adsorption in packed columns with a static solid phase
and a flowing fluid phase. A pump and rotameter are provided for fluid flow. A
Bypass valve is also provided. Sump tank is installed behind the setup to hold
chemical solution. Three borosilicate columns of various diameters and lengths are
available. Valves are installed at the column's inlet to allow only one column to be
fed at a time. After running the apparatus, valves which are at the bottom of
columns and liquid tanks are used to drain the device. To prevent the charcoal from
draining, filters are placed in front of the column drain valves.
Figure-1: Experimental setup
Requirements:
1. Electricity supply: Single phase, 220 V, 50 Hz, 5-15 Amp socket with earth
connection
2. Water supply,Test tubes, Measuring cylinders
3. Colorimeter or Spectrophotometer
4. Chemical required: KMnO4
Theory:
Adsorption is defined as the selective concentration or retention of one or more

components of a mixture on a solid surface. The adsorption process is a result of
interaction between the adsorbate molecules and the surface of the adsorbent. It is
considered as an important mass transfer operation as it provides an excellent
method of separation of a variety of fluid mixtures, particularly at low
concentrations. Some common adsorbents include Activated carbon, CMS, Silica
gel, ZMS, Silicate and Polymer adsorbents.
Adsorption of a substance occurs because of an ‘affinity’ of the surface for the

particular substance. Based on the strength of the interaction between adsorbate
and adsorbent, it can be classified as physical adsorption or chemical adsorption. If
the force of interaction is weak, it is called physical adsorption. The forces involved
here are Van der Waals force and electrostatic force. Whereas if the interaction
between a solute and the adsorbent is very strong, a chemical bond is formed and
this is classified as chemical adsorption.
The Adsorption wave

Let the concentration of the solute in the feed stream be C₀, and that in the bulk
fluid at any axial position z in the bed be C. The adsorbent concentration in the solid
in equilibrium with the feed (i.e. saturated bed) is q₀. The solute concentration in the
adsorbent is q at the axial position z in the bed. When the flow of feed into a fresh
bed (total length of the bed = L) starts, the initial rate of adsorption, particularly near
the bed entrance, is pretty fast. As the gas flows through the bed, the concentration
of the solute in it decreases because of adsorption. The solute concentrations in the
fluid and in the solid change along the bed at any time, and also with time at any
location in the bed [ i.e. C = C(z, t), and q = q(z, t)].
A. At a small time ( t = 0⁺), no part of the bed is 'saturated'. At a later time t = t1

the bed gets saturated near the inlet (i.e. x' = q/q₀ = 1 at z = 0), but the
adsorbed solute concentration decreases along the bed up to z = L
(Adsorption of the solute occurs in the unsaturated section of the bed, 0 < z
< L. This section 0 < z < L is called the mass transfer zone (MTZ).
B. The below figure shows the concentration profile of the adsorbed solute in
the bed at the time tb and the mass transfer zone (Lb < z < L). At this time the
leading edge of the mass transfer zone reaches the top of the packed
section (z = L) such that the dimensionless concentration of the solute in the
solid at the top of the bed has a small value, say x; Correspondingly, at time
𝑡 = 𝑡𝑏, the effluent fluid from the bed also has a small but measurable
concentration of the solute, 𝐶 = 𝐶𝑏. This phenomenon of the appearance of
a small but detectable concentration in the effluent from the bed is
called breakthrough.
Length of Unused Bed Calculation

The Length of Unused Bed (LUB) is given by the length of the mass transfer zone.
If the mass transfer rate were infinitely rapid, the Breakthrough curve would be the
vertical line at θ𝑠, which can be located so that the shaded areas are equal. The
adsorption zone of the figure can then be idealised as reduced to a plane, with the
length of bed 𝑍𝑠 upstream of the plane at concentration Yₜ and the length 𝑍 − 𝑍𝑠
downstream equal to the length of unused bed (LUB).
Calculation
If V = velocity of advancement of the “adsorption plane”,
then at breakthrough 𝑍𝐵 = 𝑉θ𝐵
Also, 𝑍 = 𝑉θ𝑆
Therefore, 𝐿𝑈𝐵 = 𝑍 − 𝑍𝐵 = 𝑉θ𝑆 − 𝑉θ𝐵 = 𝑍(θ𝑆 − θ𝐵)/θ𝑆
θ𝐵 = Time when the colour of product starts changing rapidly
θ𝑆 = Time required for idealised breakthrough
θ𝑇 = Time at which concentration almost saturates
θ𝑆 = (θ𝐵 + θ𝑇)/2
𝑀𝑇𝑍 = 2 * 𝐿𝑈𝐵
Thus, if the field flow is continued till the breakthrough time, virtually all the solute
entering the bed gets captured. On further continuation of the feed flow, the solute
shows up in the effluent with gradually increasing concentration.
Procedure:
1. Before starting the experiment ensure that all the valves are closed and also
the rotameter is properly calibrated.
2. Ensure that every column is filled with activated charcoal.
3. Prepare a KMnO4 solution by diluting 4g of KMnO4 crystals into 20 L of
water and ensure that the KMnO4 solution is not too concentrated.
4. Pour the KMnO4 solution into the feed tank.
5. Open the valve of the column which you want to operate.
6. Start the pump and use a rotameter to fix a low flow rate in the column.
7. Take the output samples from the corresponding column in fixed time
intervals.
8. Take water as a reference for measuring absorbance using a colorimeter.
9. Measure the optical density of the other samples with the reference sample
(water).
10. After this plot a calibration curve between concentration and optical density.
11. Using a calibration curve, find the concentration of the liquids.
12. Note down the flow rate, time, and concentration after each time interval.
13. Keep repeating the experiment until the change in the colour of the output
becomes stable.
14. Switch off the pump and close all the valves.
15. Repeat all of the above steps for each column and record the data.
Method:
Observations:
● Height of column 1, Z1 = 1 m
● Height of column 2, Z2 = 0.5 m
● Height of column 3, Z3 = 0.3 m
● Flow rate of liquid, F = 20 LPH
● Initial conc. of KMnO4 solution, C0 = 0.2 g/L
Observation Table:
Calibration Curve Data

Concentration of KMnO4 solution
Optical Density, O.D. (absorbance)
(g/L)
0.025 0.061
0.05 0.145
0.1 0.475
0.12 0.683
0.133 0.821
0.15 0.991
0.176 1.096
0.206 1.25
0.24 1.33
0.272 1.572
0.3 1.704
● Absorbance vs time data of KMnO4 solution through each column
Column 1 (Z1 = 1 m) Column 2 (Z2 = 0.5 m) Column 3 (Z3 = 0.3 m)
Time Time Time

Absorbance Absorbance Absorbance
(sec) (Sec) (Sec)
0 0.05 0 0.339 0 0.499
10 0.072 10 0.389 10 0.534
20 0.174 20 0.466 20 0.634
30 0.205 30 0.522 30 0.689
40 0.275 40 0.584 40 0.706
50 0.287 50 0.642 50 0.734
60 0.338 60 0.667 60 0.744
70 0.342 70 0.702 70 0.758
80 0.381 80 0.715 80 0.783
90 0.397 90 0.722 90 0.795
100 0.427 100 0.747 100 0.823
110 0.439 110 0.759 110 0.839
120 0.455 120 0.742 120 0.846
130 0.528 130 0.775 130 0.837
140 0.545 140 0.77 140 0.843
150 0.556 150 0.801 150 0.903
160 0.636 160 0.807 160 0.9
170 0.667 170 0.783 170 0.906
180 0.674 180 0.797 180 0.93
190 0.698 190 0.807 190 0.951
200 0.733 200 0.783 200 0.972
210 0.748 210 0.797 210 0.947
220 0.827 220 0.821 220 0.982
230 0.859 230 0.832 230 0.963
240 0.869 240 0.845 240 1.014
250 0.872 250 0.84 250 1.022
260 0.873 260 0.861 260 1.023
Calculations:
Using the calibration curve data, the calibration curve is plotted which relates the
concentration of KMnO4 solution to its optical density.
The calibration curve follows the Beer Lambert’s law and hence, it should be a
straight line. Using the data and plot, the concentration is related to optical density
by:
𝐶 = 0. 1714 × (𝑂. 𝐷.)
Using the above relation and plot, all the concentration values corresponding to
each optical density (or absorbance) obtained in 3 columns can be found out easily.
For example, consider column 1 first.

1. At time, t = 0 sec:
Optical density (or absorbance), O.D. = 0.05
Concentration of solution, 𝐶 = 0. 1714 × (𝑂. 𝐷.) = 0. 1714 × 0. 05
= 0. 00857 𝑔/𝐿
= 0. 035137 𝑔/𝐿
= 0. 0579332 𝑔/𝐿
Column 1 (Z1 = 1 m) Column 2 (Z2 = 0.5 m) Column 3 (Z3 = 0.3 m)

Time
(sec) Absorbance Concentration Absorbance Concentration Absorbance Concentration
(g/L) (g/L) (g/L)
0 0.05 0.00857 0.339 0.0581046 0.499 0.0855286
10 0.072 0.0123408 0.389 0.0666746 0.534 0.0915276
20 0.174 0.0298236 0.466 0.0798724 0.634 0.1086676
30 0.205 0.035137 0.522 0.0894708 0.689 0.1180946
40 0.275 0.047135 0.584 0.1000976 0.706 0.1210084
50 0.287 0.0491918 0.642 0.1100388 0.734 0.1258076
60 0.338 0.0579332 0.667 0.1143238 0.744 0.1275216
70 0.342 0.0586188 0.702 0.1203228 0.758 0.1299212
80 0.381 0.0653034 0.715 0.122551 0.783 0.1342062
90 0.397 0.0680458 0.722 0.1237508 0.795 0.136263
100 0.427 0.0731878 0.747 0.1280358 0.823 0.1410622
110 0.439 0.0752446 0.759 0.1300926 0.839 0.1438046
120 0.455 0.077987 0.742 0.1271788 0.846 0.1450044
130 0.528 0.0904992 0.775 0.132835 0.837 0.1434618

140 0.545 0.093413 0.77 0.131978 0.843 0.1444902
150 0.556 0.0952984 0.801 0.1372914 0.903 0.1547742
160 0.636 0.1090104 0.807 0.1383198 0.9 0.15426
170 0.667 0.1143238 0.783 0.1342062 0.906 0.1552884
180 0.674 0.1155236 0.797 0.1366058 0.93 0.159402
190 0.698 0.1196372 0.807 0.1383198 0.951 0.1630014
200 0.733 0.1256362 0.783 0.1342062 0.972 0.1666008
210 0.748 0.1282072 0.797 0.1366058 0.947 0.1623158
220 0.827 0.1417478 0.821 0.1407194 0.982 0.1683148
230 0.859 0.1472326 0.832 0.1426048 0.963 0.1650582
240 0.869 0.1489466 0.845 0.144833 1.014 0.1737996
250 0.872 0.1494608 0.84 0.143976 1.022 0.1751708
260 0.873 0.1496322 0.861 0.1475754 1.023 0.1753422
From the above graph,

Time at which the colour of product starts changing rapidly, θB = 10 sec
Time at which concentration of product saturates, θT = 240 sec
θ𝐵+θ𝑇 10+240
Time required for idealised breakthrough, θ𝑆 = 2
= 2
= 125 𝑠𝑒𝑐
Length of column 1, Z1 = 100 cm

θ𝐵 10
So, Length of Unused Bed, 𝐿𝑈𝐵 = 𝑍1(1 − θ𝑆
) = 100(1 − 125
) = 92 𝑐𝑚

θ𝐵+θ𝑇 6+220
= 2
= 113 𝑠𝑒𝑐
θ𝐵 6
) = 50(1 − 113
) 𝑚 = 47. 345 𝑐𝑚
θ𝐵+θ𝑇 8+240
= 2
= 124 𝑠𝑒𝑐
θ𝐵 8
) = 30(1 − 124
) 𝑚 = 28. 064 𝑐𝑚
Results:
Column Z (cm) θB (sec) θT (sec) θS (sec) LUB (cm)

Column 1 100 10 240 125 92
Column 2 50 6 220 113 47.345
Column 3 30 8 240 124 28.064
1. What is the conclusion of the experiment? Is the objective fulfilled?

From the experiment done we can easily infer facts like concentration varies
directly with optical density, the breakthrough time increased when column
length dropped and the likelihood of axial dispersion along with backmixing
being present in the experiment due to which the breakthrough curve
obtained was asymmetrical.
From the utilisation of material present in the columns (the most
consumption being in column 3) we can use column number 3 for scale up.
The objective of the experiment was to study the absorption in packed

columns and this was successfully conducted for a solid-liquid system by
studying the absorption of KMnO4 on Boro Silicate surface by studying
samples at different intervals of time via analysing their optical density
through the photo colorimeter instrument. This aided in finding out the
concentration of the solution and further estimating the solution that got
absorbed.
Further, the breakthrough curves for three columns studied were obtained
from the concentration tabulated against time and via these three curves θB
and θT were calculated to find θS which in turn was used to enumerate the
length of unused column
2. Give a physical interpretation of your results.

According to the Beer-Lambert law, the optical density has a linear variance
with concentration of the solution and when the calibration curve of optical
density vs concentration was plotted a straight line was obtained which
indicated that the law was followed. Using the graph concentrations at
different values of absorbance were computed.
Due to the sparse capacity of absorbent, the effluent coming from the
top of the bed should be very dilute in concentration (nearly solute free) and
this should continue until the breakpoint. These inferences were evident with
the breakthrough curve tabulated. After some time has elapsed a quasi-static
equilibrium was attained when MTZ arrived at the top of the bed as
concentration attained a fixed value because the absorbent capacity got
saturated and no longer absorbed any particle
3. Compare your results with those obtained from theory/literature.

Justify the differences in these, if any.
Some of the results obtained were contradictory, forsaking the breakthrough
curve theoretically must have been symmetrical but when experimental data
was tabulated an asymmetrical plot was obtained which can be explained
due to the possibility of axial dispersion and backmixing being present.
Along with this, the final effluent concentration did not attain the initial
concentration value which should have happened theoretically. This can be
explained on the grounds of uneven absorbent distribution in the bed and the
geometry and porosity dependence of absorption capacity. This will lead to
absorbance of solute by the component of layer below MTZ post shift of
theoretical MTZ
One of the issues that was faced in this experiment was that the absorbent
capacity was attained in a very short span of time and so was the
breakthrough point which made it hard to tabulate the experimental data
accurately.
4. Provide any additional suitable inference.

Some clear inferences that can be made from the results are -
Columns that are shorter in size give higher absorbance as they possess
higher breakthrough time. Smaller columns gave lesser concentration as
compared to columns with larger size at the breakthrough point because the
smaller columns had larger area of cross section that gave the solution more
time to get adsorbed and become saturated with liquid
LUB method also shows limitations like, method is valid for isothermal mass
transfer operations and we can scale up breakthrough curves only under
similar flow conditions, which need to be maintained constant for a time
period in which we get a stable mass transfer zone.
5. What is the mechanism or steps for adsorption to occur? Compare the

rate constants of these steps to the superficial velocity and describe
how the velocity of the propagation of adsorption-plane depends on
these.
A one-dimensional model for the movement of fluid in a packed adsorption
vessel is proposed. It describes the entire process as follows:
● The entire fluid bulk moves axially in the vessel, and the solute is
adsorbed on the adsorbent particles. The fluid loses solute gradually,
and the concentration of solute decreases axially, with no radial
distribution of concentration happening. Since the loss is only along
the axis, it is a one dimensional model.
● At every point of time, solute molecules are deposited from the fluid
bulk to the surface of adsorbent pellets by convective mass transfer,
by development of a fluid film around the pellet.
● The majority of the solute diffuses inside the pellet via pores in it, and
there is little to none solute present on the physical surface of the
pellet.
● While the solute diffuses inward, it also adsorbs on the walls of the
pores of the pellet.
By taking a unit cross section of the bed to find the unsteady state
concentration distribution of the solute in the fluid along the bed, we can get
the differential equation:
2
δ𝐶 δ𝐶 1−ϵ𝑏 δ𝑞 δ𝐶
𝐷𝐸 2 −𝑢 δ𝑧
− ϵ𝑏
ρ𝑝 δ𝑡
= δ𝑡
δ𝑧
The equation can be simplified by neglecting axial dispersion effects and
written as:
δ𝐶 δ𝐶 1−ϵ𝑏 δ𝑞
δ𝑡
+𝑢 δ𝑧
+ ϵ𝑏
ρ𝑝 δ𝑡
=0
The velocity of the adsorption plane or the velocity of propagation of the
concentration front can be given as:
𝑢
𝑢𝑐 = 1−ϵ𝑏 𝑑𝑞
1+ ϵ𝑏
ρ𝑝 𝑑𝐶
Where,
𝐷𝐸 = axial dispersion coefficient of solute in bed
𝐶 = local concentration of solute in bulk of fluid
𝑧 = axial position u = interstitial/bulk fluid velocity
ϵ𝑏 = porosity of the packed bed
ρ𝑝 = density of pellet
𝑞 = average concentration of solute in a pellet
● To prevent the accumulation of KMNO4, the liquid should be drained off as
soon as possible.
● By changing the feed supply mechanism we can make complete use of the
mass transfer area.
● By taking more data points in equal time differences we can get better plots.
Sources of Error:
● Any one of the valves may not be open while performing the experiment.
● The rate of adsorbent removal and regeneration can differ depending on the
location of the column.
● The rotameter hasn’t been calibrated initially.
● As we are performing many experiments in a short time span this can create
a situation of error due to not proper cleaning of the column.
● Any default in the colorimeter can create errors in readings.
Precautions:
● The bypass valve should be fully closed throughout the experiment.
● We must ensure that there is no leakage.
● In order to get correct results, we must ensure that the apparatus should be
drained off as soon as possible in order to prevent the accumulation of solute
particles.
● Make sure that at a time only one valve is opened.
● Make sure that the rotameter is properly calibrated and the rotameter is
closed before the start of the experiment.
Experiment Name A. Mass Transfer Coefficient

B. Diffusion Coefficient
Group Day Tuesday
Subgroup Number 6
Date / day of submission Tuesday, 3rd February 2022



A. MASS TRANSFER COEFFICIENT
Objective:
To determine the mass transfer coefficient for flow of air over a naphthalene sphere.
Experimental Setup:
The Setup of the given experiment experiment consists of:
a. Glass pipe with T section
b. Naphthalene ball
c. Metal wire (stiff)
d. Rubber cork
e. Blower
f. Orifice metre
g. Screw gauge
h. Weight Balance
Experimental Setup for measuring mass transfer coefficient of naphthalene ball

The glass pipe (about 50 mm inner diameter) is the contacting unit. In the middle of
this pipe there is a T section of about 12mm diameter. At the centre, a naphthalene
ball is held by means of a stiff metal wire, which is fitted into a rubber cork that is
tightly fitted in the T section. The blower blows air inside the pipe which is measured
by the orifice metre of bore size 25mm.
Theory:
Mass transfer coefficient relates the mass transfer rate with the mass transfer area
and the concentration change (which is the driving force here). The relation between
them is
Where kc is the mass transfer coefficient with units m/s, nA is the mass transfer rate
in mol/s, A is the effective mass transfer area in m2/s and DeltaC is the concentration
difference.
As evident from the expression above the mass transfer coefficient controls the
mass transfer rate as they have a direct linear dependence. Usually mass transfer
coefficient is found empirically by using correlations and the mass transfer coefficient
correlations are generally of the form
Kc = f(D, 𝝂, 𝜇,⍴, lc)
Several correlations are present that depend on the type of flow present which could
be laminar, turbulent or transitional, free or forced convection and so on.
For single spheres the mass transfer correlation is represented by molecular

diffusion and forced convection factors in the form of following expression -
Sh = Sh0 + C Rem Scn
where C, m constants and n = ⅓

When the reynolds number is very low, Sh approaches value 2 which can be derived
by theoretical modelling of molecular diffusion from a sphere into large volume of
stagnant fluid
In this particular case the equation transforms to
Sh = 2 + C Rem Scn
Froessling’s correlation - in this correlation C = 0.6 and m = 0.5
Sh = 2 + 0.6 Re0.5 Sc0.33
This is valid for Re in [2,800] and Sc in [0.6,2.7]
In case of gas flow across a single sphere the forced convection mass transfer can
be related with Sherwood number by
where
𝐾𝐺 𝑅 𝑇 𝑑 𝑃𝐵𝑀 0.5 0.33

𝑆ℎ = 𝑃 𝐷𝐴
= 2 + 0. 6 𝑅𝑒 𝑆𝑐
Sh is the Sherwood number

Re is the particle Reynolds number
Sc is Schmidt Number and
R is the Universal Gas constant
T is the temperature on the absolute scale
d is the diameter of the sphere,
P is the total pressure of diffusing gas at the interphase and bulk
PBM is the log mean pressure of air between interface and bulk
DA is the Diffusivity of Naphthalene in air.
Procedure:
1. Using the wire , determine the starting weight of the naphthalene ball as (W1).
2. Using the screw gauge measure the ball’s initial diameter as (d1).
3. After taking the measurement , place the ball and wire in the proper position.
4. At the same time start the airflow and the stopwatch.
5. At every subsequent 30 minutes , take the measurement (weight and
diameter) of the naphthalene ball.
6. Carry out ( Step no.5) for another 2 hours and write down the results.
Method:
Observations:
For Flow rate calculation

Coefficient of discharge, CD = 0.725
Ratio of orifice diameter and pipe diameter, β = 0.5
Expansibility factor, ϵ = 0.9
Internal orifice diameter, do = 0.025 m
For Mass Transfer Coefficient Calculation

Initial weight of wire alone, w0 = 1.3878 g
Initial weight of Naphthalene ball in wire, W1 = 5.4867 g

Initial weight of Naphthalene ball alone, w1 = W1 - w0 = 5.4867 - 1.3878 = 4.0989 g
Initial diameter of naphthalene ball, d1 = 19.55 mm
Difference
Weight of ball
Time Weight of ball between the level Temperature, Diameter of ball,
without wire, wt
(min) with wire, Wt (g) of manometer, ∆P T (°C) dt (mm)
(g)
(mm of water)
30 5.4604 4.0726 12 28 19.48
60 5.4386 4.0508 12 29 19.41
90 5.4195 4.0317 12 31 19.37
120 5.4037 4.0159 12 32 19.32
Final weight of naphthalene ball with wire, W2 = 5.4037 g

Final weight of naphthalene ball alone, w2 = W2 - w0 = 5.4037 - 1.3878 = 4.0159 g
Final diameter of naphthalene ball, d2 = 19.32 mm
Molar weight of naphthalene, MB = 128.1705 g/mol
Note: By looking at the data, it can be observed that Naphthalene diffused into the
air is very small at any time. Hence, partial pressure of Naphthalene in air can be
assumed to be 0 at every time in the experiment for simplicity.
Therefore, Partial pressure of naphthalene, P = 0 (At every time from 0 min to 120
min).
Calculations:
Weight of Naphthalene ball without wire @t = 0 sec, w1 = 4.0989 g

Diameter of Naphthalene ball @t = 0 sec, d1 = 19.55 mm
Partial pressure of naphthalene, P = 0
EXPERIMENTAL MASS TRANSFER COEFFICIENT:
1. At time t = 30 min = 1800 sec,
Weight of Naphthalene ball without wire, wt = 4.0726 g
Diameter of Naphthalene ball, dt = 19.48 mm

𝑑1+𝑑𝑡 19.55+19.48
Mean diameter of ball, 𝑑 = 2
= 2
= 19. 515 𝑚𝑚
Temperature at which air is flowing in upstream tapping, T = 28 oC

Vapour pressure of Naphthalene is given by,
3857
𝑙𝑜𝑔[𝑃1(𝑖𝑛 𝑚𝑚𝐻𝑔)] = 11. 8452 − 𝑇 (𝑖𝑛 𝐾)
3857
(11.8452− 𝑇 (𝑖𝑛 𝐾) )
⇒ 𝑃1(𝑖𝑛 𝑚𝑚𝐻𝑔) = 10
3857
(11.8452− 𝑇 (𝑖𝑛 𝐾) )
⇒ 𝑃1(𝑖𝑛 𝑃𝑎) = 133. 32 × 10
So, at T = 28 oC,
3857
(11.8452− 28+273.15 )
𝑃1 = 133. 32 × 10 = 14. 53866 𝑃𝑎
Experimental Mass Transfer Coefficient is given by,

(𝑤1−𝑤𝑡)𝑅𝑇 −3
(4.0989−4.0726)×10 ×8.314×(28+273.15)
𝑘𝑔 , 𝑒𝑥𝑝 = 2 = −3 2
π𝑑 (𝑡−0)(𝑃1−𝑃)𝑀𝐵 π(19.515×10 ) (1800)(14.53866−0)×128.1705
−5
= 1. 6409 × 10 𝑚/𝑠
Similar calculations can be carried out for all other times. These are shown in the
below table.
Vapour
Weight of Weight of Mean
Time, t Temperature, Pressure of
ball with ball without Diameter of kg , exp (m/s)
(min) T (°C) Naphthalene,
wire, W (g) wire, w (g) ball, d (mm)
P1 (Pa)
30 5.4604 4.0726 28 19.515 14.53866 1.6409E-05
60 5.4386 4.0508 29 19.48 16.02922 1.3704E-05
90 5.4195 4.0317 31 19.46 19.44699 1.0612E-05
120 5.4037 4.0159 32 19.435 21.39981 8.9857E-06
THEORETICAL MASS TRANSFER COEFFICIENT:
Diffusivity of Naphthalene into air, DA ≈ 6.92 x 10-6 m2/s
1. At time t = 30 min = 1800 sec,
Temperature at which air is flowing in upstream tapping, T = 28 oC

Density of air at T = 28 oC, ⍴air = 1.172 kg/m3
Dynamic viscosity of air at T = 28 oC, 𝜇air = 1.851 x 10-5 Pa.s
Pressure difference across orifice plate, ∆P = 12 mmH2O = 117.72 Pa
Flow rate of Air,

𝐶𝐷 π 2 0.725 π 2
𝑄= 4
ϵ 4
𝑑𝑜 2ρ𝑎𝑖𝑟∆𝑃 = 4
(0. 9) 4
(0. 025) 2 × 1. 172 × 117. 72
1−β 1−0.5
= 5.49501 x 10-3 kg/s
𝐷𝑖𝑎𝑚𝑒𝑡𝑒𝑟 𝑜𝑓 𝑜𝑟𝑖𝑓𝑖𝑐𝑒 𝑑𝑜
It is given that β = 𝐷𝑖𝑎𝑚𝑒𝑡𝑒𝑟 𝑜𝑓 𝑡𝑢𝑏𝑒
= 𝐷
= 0. 5
𝑑𝑜 0.025
Therefore, 𝐷 = 0.5
= 0.5
= 0. 05 𝑚
−3 −3
4𝑄 𝑑 4×5.49501 × 10 ×19.515×10
Reynolds Number, 𝑅𝑒 = 2 × µ
= 2 −5 = 2950. 5362
π𝐷 π×0.05 ×1.851×10
−5
µ 1.851×10
Schmidt Number, 𝑆𝑐 = ρ𝐷𝐴
= −6 = 2. 2823
1.172×6.92×10
Sherwood Number,
1/2 1/3 1/2 1/3
𝑆ℎ = 2 + 0. 6𝑅𝑒 𝑆𝑐 = 2 + 0. 6(2950. 5362) (2. 2823) = 44. 91008
Total Pressure in upstream, 𝑃 = 𝑃𝐴 + 𝑃𝐵 = 𝑃𝐴 + 𝑃𝐵 = 101325 𝑃𝑎 (1 atm)

1 1 2 2
Partial pressure of air at interface,

𝑃𝐵 = 𝑃 − 𝑃𝐴 = 101325 − 50. 92639 = 101274. 07361 𝑃𝑎
1 1
Partial pressure of air in the bulk,

𝑃𝐵 = 𝑃 − 𝑃𝐴 = 101325 − 0 = 101325 𝑃𝑎
2 2
(𝑃𝐵 −𝑃𝐵 )
101325−101274.07361
Log-mean pressure of air, 𝑃 = 2 1
=
( )
𝑃𝐵 101325
𝐵𝑀 2 𝑙𝑛( 101274.07361 )
𝑙𝑛 𝑃𝐵
1
= 101299. 53467 𝑃𝑎
Theoretical Mass Transfer Coefficient is given by,

𝑆ℎ𝑃𝐷𝐴 44.91008×101325×6.92×10
−6
−6
𝑘𝑔 , 𝑡ℎ𝑒𝑜 = 𝑅𝑇𝑑𝑃𝐵𝑀
= −3 = 6. 3609 × 10 (𝑚/𝑠)
8.314×(28+273.15)×19.515×10 ×101299.53467
Similar calculations can be carried out for all other times. These are shown in the
below table.
Time
T (°C)
⍴air 𝜇air (Pa.s) ∆P (Pa)
Flow rate of
Re Sc Sh kg , theo (m/s)
(min) (kg/m3) Air, Q (kg/s)
30 28 1.172 1.851E-05 117.72 5.49501E-03 2950.5362 2.2823 44.91008 6.3609E-06
60 29 1.168 1.856E-05 117.72 5.48563E-03 2932.2933 2.2963 44.86452 6.3449E-06
90 31 1.161 1.865E-05 117.72 5.46916E-03 2906.3982 2.32135 44.82943 6.3048E-06
120 32 1.157 1.870E-05 117.72 5.45974E-03 2889.9121 2.33562 44.79512 6.2875E-06
● The conditions are similar at every time step such as temperature, density of
air, viscosity of air, DA etc. Therefore, an average mass transfer coefficient can
be estimated to represent our results.
Average Experimental Mass Transfer Coefficient:
−6
(16.409 + 13.704 +10.612 + 8.9857) × 10 −6
𝑘𝑔 , 𝑒𝑥𝑝 = 4
= 12. 428 × 10 𝑚/𝑠
Average Theoretical Mass Transfer Coefficient:

−6
(6.3609 +6.3449 + 6.3048 + 6.2875) × 10 −6
𝑘𝑔 , 𝑡ℎ𝑒𝑜 = 4
= 6. 3245 × 10 𝑚/𝑠
Results:
● The theoretical mass transfer coefficient for transfer from Naphthalene

surface to bulk of air, kg , theo = 6.3245 x 10-6 m/s
● The experimental mass transfer coefficient for transfer from Naphthalene

surface to bulk of air, kg , exp = 12.428 x 10-6 m/s
Error Analysis:
|𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑣𝑎𝑙𝑢𝑒 − 𝐸𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑣𝑎𝑙𝑢𝑒|

Percentage Error (%𝐸𝑟𝑟𝑜𝑟) = 𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑣𝑎𝑙𝑢𝑒
𝑥100
|𝑘𝑔, 𝑡ℎ𝑒𝑜 − 𝑘𝑔, 𝑒𝑥𝑝|
(%𝐸𝑟𝑟𝑜𝑟) = 𝑘𝑔, 𝑡ℎ𝑒𝑜
× 100
% error for Average value of Theoretical and Experimental Mass transfer coefficient
−6 −6
|6.3245 𝑥 10 − 12.428 𝑥 10 |
%𝐸𝑟𝑟𝑜𝑟 = −6 × 100
6.3245 𝑥 10
%𝐸𝑟𝑟𝑜𝑟 = 96. 50 %
Time, t (min) kg, exp (m/s) kg, theo (m/s) %Error

30 1.64E-05 6.36E-06 157.97%
60 1.37E-05 6.34E-06 115.98%
90 1.06E-05 6.30E-06 68.32%
120 8.99E-06 6.29E-06 42.91%
Average 1.24E-05 6.32E-06 96.50%
As observed, error is very large initially and decreases with time but error remains
very large. Experimental value is higher compared to Theoretical value.
Reasons for this error are as follows:-
● Variances in Air flow condition.
● Error in measuring the diameter and mass of naphthalene balls.
● Large error values may result from the non-uniform sphere shape,
asymmetrical exposure of the balls, and temperature variations.
1. Give a physical interpretation of your results and compare your results

with those obtained from theory. Justify the differences in these, if any.
● The major aim of the experiment was to determine the Mass Transfer
Coefficient for the convective mass transfer of Naphthalene from its solid
form to air flowing around it experimentally.
● The theoretical value of mass transfer coefficient was also determined using
correlation given by Froessling based on the flow conditions, properties of
materials etc., and later was compared with the experimentally determined
value.
● On comparing, it was clearly observed that experimental value was almost
twice that of theoretical value. The experimental MT coefficient came out to
be 12.428 x 10-6 m/s while the theoretical MT coefficient came out to be
6.3245 x 10-6 m/s.
● This difference in values could be due to many possible reasons:
○ The Froessling’s correlation gives proper results when the Reynolds
number is in range [2,800] but the flow conditions in which this
experiment was conducted gave Re >> 800. Hence, Froessling’s
correlation might not be the best option to determine theoretical mass
transfer here.
○ The partial pressure of Naphthalene in air was assumed 0 so as to
make things easy and this assumption affected the driving force in the
formula.
○ There could be errors in measurement of diameters of naphthalene ball
since it had non uniform shape and effective diameter was determined.
○ Temperature fluctuations are also possible in the system.
● It was also observed that the mass transfer coefficient slightly varied with
time. This was due to its dependence on properties like density of fluid,
viscosity of fluid, dimensions of ball, Diffusivity (which itself depends on many
factors like temperature, molecular weight of fluid etc.). As time progressed,
these properties varied slightly and hence the mass transfer coefficient.
2. What is the difference between diffusion coefficient and mass transfer

coefficient? Which of them depends on the other? Why do we need the
dependent parameter?
● Mass Transfer happens when there is a concentration gradient, whereas
diffusion is an intermolecular event.The interaction of solute with the solvent
determines the diffusion flux. Molar flow per unit concentration gradient via a
surface is the diffusion coefficient is defined. The mass transferred is related
to the area of interaction and concentration gradient. The mass transfer
coefficient depends upon the diffusion coefficient. We need the diffusion
coefficient inorder to know at what rate the constituents are transferred and
how can it be optimised to our needs.
3. Give the physical significance of Sherwood number, Schmidt number

and Reynolds number. Show that the Sherwood number is 2 in the case
of diffusion from a sphere when there is no flow.
● The Sherwood number(Sh) is the ratio of convective mass transfer to diffusive
mass transfer.
The Schmidt number(Sc) is the ratio of momentum diffusivity to mass
diffusivity. It describes the fluid flows that undergo both momentum and mass
diffusion at the same time.
The Reynolds number(Re) is the ratio of viscous force to the inertial force. It
tells us about the flow pattern i.e laminar or turbulent.
Assuming Ni flow:
𝑁𝐴 = 𝐷𝐴(𝐶𝐴 − 𝐶𝐴 ) = 𝐾𝑐(𝐶𝐴 − 𝐶𝐴 )
𝑖 𝑖 0 𝑖 𝐵
𝐷𝐴 𝐾𝐶 𝐷𝐴
⇒ 𝐾𝑐 = 𝑅
& 𝑅
=1
𝐾𝐶 𝑑 𝐾𝐶 (2𝑅)
⇒ 𝑆ℎ = 𝐷𝐴
= 𝐷𝐴
=2
4. Briefly describe the analogy between heat transfer and mass transfer.
● For mass transfer, the Nussel number (Nu, ratio of convective to conductive
heat transfer) is called Sherwood number(Sh). The Prandtl number (Pr) for
mass transfer is equivalent to the Schmidt number(Sc) as we have mass
diffusivity instead of thermal diffusivity.
1. While measuring the diameter of the naphthalene ball, several readings with
different orientations can be recorded and then these can be averaged to get
accurate results
2. We can keep good track of temperature readings for both air and the
naphthalene sphere.
Sources of Error:
● As the gas starts flowing through the sphere ball it will alter the shape of the
ball and also because of surrounding irregularities and this all will
subsequently result in the difference in the measurement of diameter of the
sphere.
● As we are measuring the mass of the sphere using the weight measuring
machine which can involve human error.
● There will also be the existence of a parallax effect while taking the readings
of the height of manometric fluid in both legs of the manometer.
● Naphthalene balls have different air flow throughout the surface.
Precautions:
● The mean diameter of the naphthalene ball can be measured by multiplying
the diameter of two mutually perpendicular surfaces.
● Be cautious while suspending the naphthalene ball and starting the
timer.small delay can alter results.
● Never touch the outer surface of the heater.
B. DIFFUSION COEFFICIENT
Objective:
To find the diffusion coefficient of Acetone vapour in air using Stefan’s Tube
apparatus.
Experimental Setup:
The setup consists of a diffusion cell and inside the diffusion cell there exists a
central vertical glass tube ,which is opened from the top and closed from the
bottom.which is also packed/surrounded by another glass tube.The air , which is
entered into the cell, flows up around the tube through the annular between the glass
tube and the surroundings and escapes from the topside of the tube.
FIGURE 2 - Schematic diagram of Stefan’s tube
Requirements:
● Acetone.
● Stefan Tube.
● Cathetometer.
● Compressed air supply.
Theory:
Diffusion is a process that results from the random motion of molecules that
culminates in a net flow of matter from a region of high concentration to a region of
low concentration.
Generally there are two types of diffusion - diffusion of one species through another
species which is non diffusing or stagnant and the other is the case of equimolar
counter diffusion
Ficks law –
𝑑𝐶𝐴
𝑗𝐴 = − 𝐷𝐴 𝑑𝑧
Where jA is the molecular flux of species A with respect to an observer that moves
with average molar velocity, DA is the diffusivity of species A in a mixture and CA is
the concentration of the species A in mixture
Stefan’s tube is used to enumerate the molecular diffusion coefficient of vapour in

gas. This consists of a vertical tube filled with acetone while air is passed over the
top of the tube. A stagnant film of evaporated acetone vapours is formed present
above the liquid surface inside the tube. The diffusion coefficient is calculated by
tabulating the liquid level after specified intervals of time.
Assume that z is the liquid level from the top end of the tube, air has a partial
pressure pA2 , then the vapours of acetone can be assumed to pass through the
stagnant gas film of thickness z. It can be noted that the partial pressure of acetone
in the gas adjacent to the interface is equal to the vapour pressure of acetone at the
temperature at which experiment is conducted, let it be pA1.
If quasi steady state model is assumed (despite the fact that this is a transient
diffusion case), the steady state diffusion of A through stagnant B at a given z is
given by the following expression
𝐷𝐴𝐵 𝑃 (𝑃𝐴1−𝑃𝐴2)
𝑁𝐴 = 𝑅𝑇𝑧 𝑃𝐵𝑀
where,
DAB is the molecular diffusion coefficient of A in B
P is the total pressure
R is the universal gas constant
T is the temperature on absolute scale
PBM the log mean of PB1= P-PA1 & PB2 = P-PA2
Let the density of the liquid A be ⍴ then,

⍴ 𝑑𝑧
𝑁𝐴 = 𝑀𝐴 𝑑𝑡
where MA is the molecular weight of A

Now manipulating the above two expressions and removing NA we get
𝑅𝑇𝑃𝐵𝑀⍴ 𝑧𝑑𝑧
𝐷𝐴𝐵𝑑𝑡 = 𝑃 (𝑃𝐴1 − 𝑃𝐴2) 𝑀𝐴
Integrate the above expressions with the boundary conditions @t = 0 – z = z1 and

@t = t – z = z2
2 2
𝑅 𝑇 𝑃𝐵𝑀 (𝑧2 − 𝑧 1) 𝝆
𝐷𝐴𝐵 = 2 𝑃 (𝑃𝐴1 − 𝑃𝐴2) 𝑀𝐴 𝑡
Procedure:
1. Take the vertical glass tube, fill it with acetone liquid up to the top of the
vertical tube, and place it in the cell.
2. At first, the length of z1 should be measured by focusing the cathetometer at
the top end of the tube and also at the liquid surface.
3. At a very low and steady rate, the air(B) started to flow and maintain.
Simultaneously the stopwatch also started. A schematic diagram for the same
is shown in the experimental setup.
4. Every 30 minutes, record the height of the acetone in the tube and tabulate
the results.
Method:
Observations:
Temperature = 23 oC = 296 K
Universal Gas Constant = 8.314 m3-Pa/mol-K
Molecular weight of Acetone = 58.08 g/mol = 0.05808 kg/mol
Initial Height of the liquid ‘z1’ = 25.967 cm
Final Height of the liquid ‘z2’ = 25.425 cm
Time taken = 120 minutes
Density of Acetone (ρ) = 0.7857 g/cm3 = 785.7 kg/m3
Observation Table:
Time (min) Level of Acetone (cm)

0 25.967
30 25.858
60 25.756
90 25.568
120 25.425
Calculations:
𝑃𝐴 = Partial pressure of Acetone at air-liquid contact point = Vapour pressure of

1
Acetone at 296 K
Partial Pressure of Acetone at 296 K can be calculated using Clausius-Clapeyron

equation:-
𝑙𝑛 ( ) 𝑃1
𝑃2
=
∆𝐻𝑣𝑎𝑝
𝑅 ( 1
𝑇2
−
1
𝑇1 )
We know that,
Normal boiling point of Acetone = 56 oC = 329 K

Partial Pressure of Acetone at 56 oC = 101325 Pa
Therefore,
P2 = 101325 Pa
T2 = 329 K
T1 = 296 K ( Temperature at which Partial Pressure will be calculated)
∆𝐻𝑣𝑎𝑝 of Acetone = 2.91 x 10 4 J/mol
R = 8.314 J/mol-K
( )
𝑃𝐴 4
𝑙𝑛 1
101325
=
2.91 𝑥 10
8.314 ( 1
329
−
1
296 )
𝑙𝑛(𝑃𝐴 ) = 10. 3400
1
(10.3400)
𝑃𝐴 = 𝑒 = 30946. 03 𝑃𝑎
1
Assume that the velocity of air above the tube is such that acetone vapours reaching
the tube's top are carried away by air, leaving a minimal partial pressure of acetone.
Therefore, 𝑃𝐴 = Partial pressure of Acetone in bulk air = 0

2
Diffusion coefficient of Acetone in air can be calculated by:-

2 2
𝑅𝑇𝑃𝐵𝑀(𝑧2 −𝑧1 ) ρ
𝐷𝐴𝐵 = 2𝑃𝑀𝐴(𝑃𝐴 − 𝑃𝐴 ) 𝑡
1 2
Where,
Density of Acetone ( ρ) = 785.7 kg/m3

Ambient pressure (𝑃) = 101325 Pa = 1 atm
Temperature (𝑇) = 296 K
Molecular weight of Acetone ( 𝑀𝐴) = 0.05808 kg/mol
𝑃𝐴 = 30946. 03 𝑃𝑎
1
𝑃𝐴 = 0 𝑃𝑎
2
t = Time period of 30 minutes
Now,
𝑃 = 𝑃𝐴 + 𝑃𝐵 = 𝑃𝐴 + 𝑃𝐵 = 101325 𝑃𝑎 = 1 𝑎𝑡𝑚
1 1 2 2
𝑃𝐵 = 𝑃 − 𝑃𝐴 = 101325 − 0 = 101325 𝑃𝑎
2 2
𝑃𝐵 = 𝑃 − 𝑃𝐴 = 101325 − 30946. 03 = 70378. 97 𝑃𝑎

1 1
(𝑃𝐵 −𝑃𝐵 )
Log Mean Pressure of air, PBM = 2 1
( )
𝑃𝐵
2
𝑙𝑛 𝑃𝐵
1
(70378.97 − 101325)
𝑃𝐵𝑀 = = 84914.23 Pa
𝑙𝑛 ( 70378.97
101325 )
For time period 0 - 30 minutes
𝑡 = 30 𝑚𝑖𝑛 = 1800 sec

𝑧1 = 25.967 cm = 0.25967 m
𝑧2 = 25.858 cm = 0.25858 m
2 2
𝑅𝑇𝑃𝐵𝑀(𝑧2 −𝑧1 ) ρ
𝐷𝐴𝐵 = 2𝑃𝑀𝐴(𝑃𝐴 − 𝑃𝐴 ) 𝑡
1 2
Using constants as given above :-

2 2
8.314 𝑥 296 𝑥 84914.23 𝑥 ((0.25967) −(0.25858) ) 𝑥 785.7
𝐷𝐴𝐵 = 2 𝑥 101325 𝑥 0.05808 𝑥 (30946.03 − 0) 𝑥 1800
DAB = 1.41 x 10-4 m2/sec

DAB for every 30 min time interval
Time Interval Time (seconds) Z1 (m) Z2 (m) DAB

0 - 30 min 1800 0.25967 0.25858 1.4147E-04
30 - 60 min 3600 0.25858 0.25756 6.5921E-05
60 - 90 min 5400 0.25756 0.25568 8.0546E-05
90 - 120 min 7200 0.25568 0.25425 4.5654E-05
Average 8.3397E-05
Average Diffusion Coefficient of Acetone in Air

−5
(14.147 + 6.5921 + 8.0546 + 4.5654) × 10 −5 2
𝐷𝐴𝐵 = 4
= 8. 3397 × 10 𝑚 /𝑠
Results:
The Diffusion Coefficient of Acetone in Air at 23 oC is 8.34 x 10-5 m2/sec
1. Calculate the expected diffusion coefficient using the Chapman-Enskog

equation and compare with the experimental diffusivity.
● The Chapman-Enskog equation is given by:-
−7 3/2 1 1
1.858 𝑥 10 𝑇 𝑀𝐴
+ 𝑀𝐵
𝐷𝐴𝐵 = 2 m2/sec
𝑃 (σ𝐴𝐵) Ω𝐷
T = absolute Temperature in K
MA, MB = molecular weights of A and B
P = total pressure in atm
σ𝐴𝐵 = characteristic length parameter of binary in Å
Ω𝐷 = collision integral , 𝑓 ( )
𝑘𝑇
ε𝐴𝐵
Given, (following data is taken from B.K. Dutta Principal of Mass

transfer and separation processes)
T = 296 K
MA = 58.08 g/mol, MB = 28.97 g/mol
P = 1 atm
σ𝐴𝐵 = 4.155 Å
Ω𝐷 = 1.23
Therefore, Theoretical value of the Diffusion Coefficient calculated from

the Chapman-Enskog equation is 1.013 x 10-5 m2/sec and the
Experimental value of Diffusion Coefficient is 8.34 x 10-5 m2/sec.
The experimental and theoretical value are of the same order but
experimental value is higher than theoretical which leads to high error.
The experimental value differs from the Theoretical value because the
flow rate above the tube is less than the required flow rate. We
believed that the physical properties of acetone do not change with
temperature, however this is not always the case.
2. Write about the effect of air flow rate and temperature on diffusion
coefficient. What should be the optimum air flow rate?
● If the airflow rate is increased, the diffusion constant will increase and
as the air velocity increases, we can deduce that the reynolds number
will increase as well, which would increase sherwood number and in
turn mass transfer coefficient, so finally 𝐷𝐴𝐵 increases and also 𝐷𝐴𝐵
increases as the temperature is increased as 𝐷𝐴𝐵 is proportional to T1.5.
3. Give any five differences between the mass transfer coefficient and the
diffusion coefficient.
● The major differences between mass transfer coefficient and diffusion
coefficient are enlisted below:
1. Mass Transfer coefficient is the ratio of molar flux to conc./
partial pressure/ mole fraction difference (as driving force) while
diffusion coefficient is the ratio of molecular flux w.r.t. Observer
moving with molar average velocity to conc. gradient.
2. Mass Transfer coeff. is rate based while diffusion coeff. is
equilibrium based.
3. Mass Transfer coefficient has units of m/s whereas diffusion
coefficient has units of m²/s.
4. In mass transfer coefficients all these are considered Mass
transfer by diffusion, convection and phase change while in the
second case only by diffusion is considered.
5. 10⁻⁰²m/s is the general value for mass transfer coefficient
whereas 10⁻⁰⁵ m2/s for the diffusion coefficient.
4. Give any five inferences from the experiment.
● The rate of diffusion and mass transfer increases as air is blown over
the acetone glass tube. As a result, the diffusion coefficient's value will
rise.
● As the diffusion coefficient is a function of temperature, changes in
temperature have an impact on its value.
● The relative volatility of acetone is affected by pressure, which changes
the diffusion coefficient value.
● Diffusion coefficient and Mass transfer coefficient differ in many ways
and cannot be assumed to be the same.
● The Boundary Layer Theory (BLT) provides correct MTC values
despite several assumptions.
5. List five industrial uses of the experiment.

● Some industrial applications of this experiment are:
1. For cleaning catalysts to remove waste after the reaction stages,
to increase the efficiency of catalysis.
2. Mass transfer is used to transfer unwanted materials from any
solution and hence purify the solution.
3. With the complete knowledge of mass transfer, chemical
reactors are designed.
4. It is exploited to treat corrosive, high energy, nuclear wastes in
the industry which are produced as a by-product.
5. Mass transfer and absorption are also used to purify gases in
the industry.
1. Adding a temperature controller can be a boon as it will increase the precision
of our experiment.
2. The flowrate should be kept constant throughout the experiment, a orifice
metre and a controller could be added to ensure this.
3. We should avoid using air bubbles in the experiment because this will
increase the effective length of the column, causing our measurements to be
hampered.
4. A constant temperature water bath can be placed just outside the glass tube
filled with acetone, with air flowing in a horizontal manner just above the tube
entrance. Inside the glass tube, it will retain a steady temperature.
Sources of Error:
● Cathetometer might not be placed horizontally.
● As we know that the temperature is not constant then there might be some
error in calculating partial pressure of acetone.
● There is always some parallax error while taking readings on a vernier scale
through the convex lens.
● There could be a zero inaccuracy in the cathode metre’s reading equipment.
Precautions:
● Zero scale of cathetometer.
● Verify your reading by rechecking it.
● Clean all the apparatus properly, specially convex lenses.
● For correct reading take measurement after every 30 minutes.
● Take care while filling acetone in the glass tube.

CLP302 - MT (SG 6) - Merged (1) 2

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

CLP302 - MT (SG 6) - Merged (1) 2

Uploaded by

Copyright:

Available Formats

CLP302: Mass Transfer and Fluid Particle Mechanics Lab

Semester II: 2021 - 2022

Experiment Name Vapour Liquid Equilibria

Group Day Tuesday

Date / day of submission Tuesday, 7th February 2022

Date / day of common doubt Tuesday, 1st February 2022

Names of group members Hemant Prakash Singh (2019CH70172)

Name of lab instructor Prof. A.N. Bhaskarwar

Marks (to be filled by instructor/TA)

Figure-1: Experimental setup

Experiment setup based procedure

Procedure to use the refractometer

Calibration Chart of Water and Ethanol mixture

S.No. Mole % of Ethanol Mole % of Water Refractive Index

Vapour Liquid Equilibrium

86.4 1.3592 1.3376

For example, at T = 85.3 oC,

Vapour Liquid Equilibrium

85.3 1.3589 0.95 1.3395 0.04

86.7 1.3586 0.8 1.3387 0.032

The T-x-y data is shown in a separate table below:

Vapour Liquid Equilibrium

85.3 0.95 0.04

86.7 0.8 0.032

Temperature(℃) 𝑥𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 x error(%)

86.4 0.1024 0.024 76.59

85.3 0.1238 0.04 67.68

86.7 0.0966 0.032 66.87

Temperature(℃) 𝑦𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 y error(%)

86.4 0.4445 1 124.97

85.3 0.4704 0.955 103.01

86.7 0.4375 0.8 82.85

The main reasons for this error are:

Discussion and Conclusion:

1. What is the conclusion of the experiment? Is the objective fulfilled?

2. Give a physical interpretation of your results.

3. Compare your results with those obtained from theory/literature. Justify

5. Define bubble point and dew point.

6. Describe in brief how the interactions between the components affect

Experiment Name Mass transfer with and without chemical

Group Day Tuesday

Date / day of submission Tuesday, 18th January 2022

Date / day of common doubt Tuesday, 11th January 2022

Names of group members Hemant Prakash Singh (2019CH70172)

Name of lab instructor Prof. A.N. Bhaskarwar

Marks (to be filled by instructor/TA)

where [A* ] is the (saturation) concentration of A at the solid-liquid interphase, [Bo] is

If boundary layer model is used then

For Mass Transfer without reaction

Time (min) Volume of Std. NaOH used for 10 ml of soln (V2)

For Mass Transfer with reaction

Time (min) Volume of Std HCl used for 10 ml of soln (V'2)

● Mass Transfer without Chemical Reaction

Average surface area of Cake

Solubility of benzoic acid in water at 50 ℃ is

Volume of Std. NaOH

10 8.3 600 0.0083 0.1217 0.1298

● Mass Transfer with Chemical Reaction

Average surface area of Cake

To calculate Concentration of NaOH at time (T), we will use mole balance

𝑁'1 × 𝑉'1 = 𝑁'2 × 𝑉'2

Solubility of benzoic acid in water at 50 ℃ is

Specific rate of dissolution