Experiment 

No.‐1:  Measurement of Diffusivity of Carbon Tetrachloride in Air 
 
The schematics of the experimental set up is given below: 
 
 
 
 
 
 
 
 
 
 
 
 

 
 
Figure: (a) Experimental Schematics (b) Digital photograph of Experimental set up in MT Lab 
 
 
Following data are obtained from one such experiment.  Calculate diffusion coefficient of an 
organic  vapour  and  study  the  effect  of  temperature  on  the  diffusion  coefficient  using  the 
data.    If  you  need  additional  data,  get  the  data  from  the  handbook.    You  can  assume  any 
physical  data  related  to  the  experimental  set  up.  See  the  manual  for  additional 
help/hints/theories.  

T (℃   Time (sec)  Length(cm)  x0 ‐x(cm)  𝜃/𝑥 0 ‐x(s/cm)  

50  0  6.697  0  0 
100  6.630  0.067  1492.53 
200  6.570  0.060  3333.33 

60  0  6.685  0  0 
100  6.615  0.070  1428.57 
200  6.550  0.065  3076.92 

70  0  6.668  0  0 
100  6.603  0.065  1538.46 
200  6.543  0.060  3333.33 

  
Experiment No.‐2:  Verification of Rayleigh’s equation for batch distillation 
 
1.  The schematics of the experimental set up is given below: 
 

(a)

Feed Solution

 
 

(b)

 
Figure: (a) Experimental Schematics (b) Digital photograph of Experimental set up in MT Lab 
 
Following data are obtained from one such experiment.  Verify the Rayleigh’s equation for 
the following data found out after conducting a batch distillation for a binary liquid mixture.  
If you need additional data, get the data from the handbook.  You can assume any physical 
data related to the experimental set up. See the manual for additional help/hints/theories.  
 
 
 Table: Calibration data for toluene/acetone mixture 

Toluene concentration (%volume) Refractive index

0 1.352
20 1.3692
40 1.394
60 1.4323
80 1.4537
100 1.782
 
Refractive Index of distillate: 1.395 
Refractive index of residue: 1.384 

Submit the softcopy of the lab note book in the MS Teams platform.

 
Experiment No.‐3:  Sieve Plate Distillation Column 
1.  The schematics of the experimental set up is given below: 
 

(a)

 
 (b)

 
 
 
Figure: (a) Experimental Schematics (b) Digital photograph of Experimental set up in MT Lab 
 
Following data are obtained from one such experiment.  Please 
a. Calculate theoretical number of plates using Mc-Cabe Thiele’s method when
the column is operating in total reflux ratio.

b. Calculate the overall efficiency of the sieve plate distillation column.

 If you need additional data, get the data from the handbook.  You can assume any physical 
data related to the experimental set up. See the manual for additional help/hints/theories.  
Observation Table:  

T1(OC) T2 T3 T4 T5 T6 T7 T8 T9 T10
77 66 78.9 81.7 87.7 75.3 73.1 71.2 67.6 64.5
 

Refractive index

Reboiler 1.338
Distillate 1.363
Plate 1 1.3505
Plate 2 1.360
Plate 3 1.346
Plate 4 1.346
Plate 5 1.348
Plate 6 1.350
Plate 7 1.357
Plate 8 1.353
 
 
 
 
 
 
 
Required Information 
Data (Methanol‐ Water) 
Relative volatility α = 3.32 
Molecular weight of methanol MM = 32 g/mol 
Molecular weight of Water MW = 18 g/mol 
Actual number of plates NA = 8 
Enthalpy of feed HF = 0 kJ/kmol 
Specific heat of methanol CPA = 2721 J/kg K 
Specific heat of Water CPB = 4187 J/kg K 
Latent heat of vaporization of methanol λA = 104607 J/kg 
Latent heat of vaporization of Water λB = 2284 J/kg 
Density of methanol ρm = 0.803 g/cm3 
Density of Water ρw = 1.0 g/cm3 
Symbol used 
xD = Mole fraction of ethanol in distillate 
xB = Mole fraction of ethanol in residue 
R = Reflux ratio 
x = mole fraction of light key component in liquid phase 
y = mole fraction of light key component in vapour phase 
Conditions of the experiments 
Type of Plates: Sieve 
Number of Plates: 8 
Temperature: 77oC 
Table: Calibration curve

% Ethanol Refractive index

10 1.336
20 1.338
30 1.343
40 1.357
50 1.35
60 1.354

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Experiment No.‐7:  Studies on Batch Drying and Generation of Drying Curve 
 
1.  The schematics of the experimental set up is given below: 
 
 
(a) 

 
 
 

(b) 

 
 
Figure: (a) Experimental Schematics (b) Digital photograph of Experimental set up in MT Lab 
 
Following data  are obtained from one  such experiment.  Develop  the drying curve for the 
sample  provided.  If  you  need  additional  data,  get  the  data  from  the  handbook.    You  can 
assume any physical data related to the experimental set up. See the manual for additional 
help/hints/theories.  
 
Data Provided 
Weight of empty petridish = 30.71 g 
Weight of dry sand = 50 g 
Amount of water = 10 ml 
Initial weight of wet sand = 90.02 g 
Temperature = 45⁰C 
Air flow rate = 7 m/s 
Diameter of the petridish = 7 cm 
 
 
Observation Table 

Time (min)  Weight  of  wet  Time (min)  Weight  of  wet 

sand (gram)  sand (gram) 
0  90.02  48  85.29 
3  89.73  51  85.01 
6  89.50  54  84.77 
9  89.19  57  84.45 
12  88.96  60  84.16 
15  88.65  63  83.68 
18  88.37  66  83.44 
21  88.08  69  83.21 
24  87.74  72 82.95
27  87.47  75 82.75
30  87.17  78 82.57
33  86.84  81 82.41
36  86.51  84 82.25
39  86.22  87 82.10
42  85.90  90  81.95 
45  85.58     
 

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 LIQUID-LIQUID EXTRACTION IN

A PACKED BED
OBJECTIVE:
To study the extraction of benzoic acid from toluene (dispersed phase) by ater (continuous
phase) in a packed bed.
AIM:
 To determine overall mass transfer coefficient based on continuous phase (water),Kwa.
 To determine overall mass transfer coefficient based on dispersed phase (toluene),Kta.
 To determine overall ‘Height of Transfer Unit’ based on continuous phase
(water),HTUow & based on dispersed phase (toluene), HTUot
 To determine Individual ‘Height of Transfer Unit’ based on continuous phase (water),
HTUw and dispersed phase (toluene), HTUt
INTRODUCTION:
Liquid extraction, sometimes called solvent extraction, is the separation of the constituents of
a liquid solution by contact with another insoluble liquid. If the substances constituting the
original solution distribute themselves differently between the two liquid phases, a certain
degree of separation will results, and this can be enhanced by use of multiple contacts or their
equivalent in the manner of gas absorption and distillation.
THEORY:
Towers filled with some random packing (say rasching rings) are widely used for extraction of
valuable chemicals from dilute solutions by liquid-liquid extraction. The packing provides a
larger extract area for mass transfer and also reduces the axial mixing to some extent.
The extraction rate in such columns depends on:
Choice of either continuous or dispersed phase
Packing and column variables
Velocity of the liquid phases in the tower
The tower performance is generally based on extraction rate data and evaluated in terms of
over all height of transfer unit, based on continuous phase, HTUow and the extraction factor
expressed in terms of flow rate ratios of the liquid phases, mVw/Vt These two variables are
plotted against each other on Cartesian co-ordinates. As suggested by Colburn, the slope and
intercept of such a plot would represent the resistance of the individual films as:
OVER ALL HEIGHT OF TRANSFER UNIT:
 mV 
HTU ow  HTU W  HTU t  w                   1
 Vt 

 V 
HTU ot  HTU t  HTU w  t                   2
 mVW 
Where, m is the slope of equilibrium curve, m = dCw/dCt

* Under certain conditions (e.g. low concentrations) m is a constant

V is the superficial velocity of the liquid phase based on empty cross section of the column,

subscript w for continuous phase (water) and t for dispersed phase (toluene).

Rate of mass transfer from dispersed phase to the continuous phase is defined as:

N   
 C w*1  C w1  C w* 2  C w2 
 K w aV 

   
 ln C w1  C w1 / C w2  C w2 
* *

N  C1  C 2 
 K w aV  
  lnC1 / C 2  
The capacity coefficient based on continuous phase (water), Kwa, is thus defined as:
N
KW a                  3
V CW ln

C w1  C w2
Where, C w ln 
 C w1 
ln 
 C w 2 
Similarly, the capacity coefficient based on dispersed phase (toluene), Kta, is defined as:
N
Kt a                  4
V C t ln

As per Chilton and Colburn, the over all height of transfer unit based on continuous phase
(water), HTUow is defined as:
Vw
HTU ow                 5
K wa
And the over all height of transfer unit based on dispersed phase (toluene), HTUot
is defined as:
Vt
HTU ot                 6
Kt a

DESCRIPTION:
The set up consists of two feed tank. In this system two different liquids are used in which the
one is heavier (water) which is used as solvent and the other is lighter in which the solute is
present (toluene). The heavier liquid is inserted from the top and the lighter from the bottom.
The interface maintained in the column between the lighter phase and the heavier phase at the
top of the column can be adjust up or down as necessary by regulating the arrangement
provided at the water stream leaving the column. Flow rate of both the liquids is measured by
the rotameters provided. The samples are taken from the top for lighter liquid and bottom for
heavier liquid.
UTILITIES REQUIRED:
1. Compressed Air Supply @ 0.5 CFM at 2 Bar,.
2. Drain required.
3. Laboratory Glassware.
4. Weighing Balance (least count + 1 gm)
5. CHEMICALS REQUIRED:
Toluene = 20 L
Benzoic acid = 488 gm
Distilled water = 20 L
N/5 NaOH in alcohol = 500 ml
N/20 NaOH in water = 500 ml
Phenolphthalein as indicator = 10 ml
EXPERIMENTAL PROCEDURE:
1. Prepare a mixture of Toluene and Benzoic Acid as a feed mixture, with the
concentration of Benzoic Acid 488gm in 20Ltrs (i.e. N/5).
2. Fill the column with the continuous phase (water).
3. Allow the dispersed phase (toluene + benzoic acid) to enter from the bottom of the
column at some minimum flow rate.
4. Adjust the Rotameter readings for Continuous and dispersed phase to same values.
5. The interface between the lighter phase and the heavier phase at the top of the column
must be worked up or down as necessary by adjusting the sliding arrangement provided
in the water stream leaving the column. The position of the interface is to be maintained
 at about 1 inch above the point of introduction of the heavier liquid (water) into the
column.
6. Take the first observation after the steady state has been established i.e. after ≈ 10to 20
minutes.
7. Collect known amount of sample of Extract(water) and raffinate (Tolune).
8. Titrate the sample of tolune against N/5 NaOH in alcohol using phenolphthalein as
indicator.
9. Titrate the sample of water against N/20 NaOH in water using phenolphthalein as
indicator.
10. Repeat the experiment for different flow rate of liquids.

OBSERVATION & CALCULATION:

DATA:
Dc = 0.045 m
Z = 0.75 m
NTT,NTB = ----------------(for Tolune)
NWB = ----------------(for Water)

Equilibrium data for Benzoic Acid - Toluene – Water

Cw, g mole/L Ct, g mole/L
0.0000 0.0000
0.0016 0.0080
0.0064 0.0336
0.0080 0.0673
0.00961 0.08811
0.011211 0.12015
0.012816 0.14097
0.01442 0.17301
The equilibrium data can be represented by:
Cw
 H  0.2015  1.4273C t  4.3672C t2
CT

And
C w  0.0745C t 0.0019

Or slope of the equilibrium line can be assumed to be constant at

dC w
m  0.0745
dC t

OBSERVATION TABLE:
S.No. Qt, LPH Qw, LPH V1, ml VTT, ml VTB, ml VWB, ml

CALCULATION:
A) CONCENTRATION OF BENZOIC ACID IN TOLUENE:
1) At bottom: (feed concentration)
N TBVTB
N1   ______________ gmol / L
V1
Ct1= CF = N1 g mole/L
2) Similarly At Top:
N TT VTT
N1   __________ ____ gmol / L
V1
Ct2= N1 g mole/L
 A1  C t1 C t 2 Qt  __________ ____ gmol / h

B) CONCENTRATION OF BENZOIC ACID IN WATER:

1) At Top:
Cw2= 0
 N WBVWB
N1   ______________ gmol / L
V1

Cw1 = N1 g mole/L
 A2  C w1 C w 2 Q w  __________ ____ gmol / h

N A1  A2
   ______________ gmol / h
 2
OVERALL MASS TRANSFER COEFFICIENT BASED ON DISPERSED
PHASE:
Kt a
At bottom:
C 
H1   w 
using equilibrium data
 C t  atCt Ct 1

C t1  C t1  C w1 / H 1   __________ ____ gmol / L

At Top:
C 
H2   w 
using equilibrium data
 C t  atCt C t 2

C t 2  C t 2  C w 2 / H 2   __________ ____ gmol / L

C t 2  C t1
Ct ln   ______________ gmol / L
lnC t 2 / C t1 

V DC2 Z  ______________ ml
4
N /
Kt a   ______________
V C t ln

C w1  H 1C t1  C w1  __________ ____ gmol / L

C w 2  H 2 C t 2  C w 2  __________ ____ gmol / L

C w2  C wt1
C w ln   ______________ gmol / L
lnC w2 / C w1 
N /
K wa   ______________
V C w ln


AC  DC2  ______________ m 2
4
OVER ALL HEIGHT OF TRANSFER UNIT BASED ON CONTINUOUS
PHASE:
Qw
Vw   ______________ m / h
AC

Vw
HTU ow  ______________ m
KW a

OVER ALL HEIGHT OF TRANSFER UNIT BASED ON DISPERSED

PHASE:
Qt
Vt   ______________ m / h
AC

Vt
HTU ot  ______________ m
Kt a

Vw
Plot the graph (HTU)ow vs. on a simple graph. Determine the slope & intercept.
Vt
HTUt = Slope of graph = --------- m
HTUw = Intercept of graph = --------- m
NOMENCLATURE:
A1 = Amount of benzoic acid extracted by water, g mol/h
A2 =Amount of benzoic acid recovered by water, g mol/h
Ac =Column cross sectional area, m2
Cw1 =Concentration of benzoic acid in water at bottom, g mol/L
Cw2 =Concentration of benzoic acid in water at top, g mol/L
Ct1 =Concentration of benzoic acid in toluene at bottom, g mol/L
Ct2 =Concentration of benzoic acid in toluene at top, g mol/L
Cw =Equilibrium solute (benzoic acid) concentration in water phase, gmol/L
CF =Concentration of benzoic acid in feed. g mol/L
Ct =Equilibrium solute (benzoic acid) concentration in toluene phase, gmol/L
Dc =Column diameter, m
H =Equilibrium distribution coefficient,H1,H2 (CW / CT)
HTUw = Individual height of transfer unit based on continuous phase(water), m
HTUt =Individual height of transfer unit based on dispersed phase (toluene), m
HTUow=Overall height of transfer unit based on continuous phase (water), m
 HTUot=Overall height of transfer unit based on dispersed phase (toluene), m
Kw a =Overall mass transfer coefficient based on continuous phase
Kt a =Overall mass transfer coefficient based on dispersed phase
N/θ =Average amount of Benzoic acid recovered, g mol/h
N1 =Normality of sample
NTT,NTB =Normality of NaOH used(for Tolune).
NWB =Normality of NaOH used(for Water).
Qt =Volumetric flow rate of toluene, LPH.
Qw =Volumetric flow rate of water, LPH.
V1 =Volume of sample, ml
VTT =Volume of NaOH used in titration of top sample for Tolune, ml
VTB =Volume of NaOH used in titration of bottom sample for Tolune, ml
VWB = Volume of NaOH used in titration of bottom sample for Water, ml
V =Effective volume of packed section, ml
Vt =Superficial velocity of water phase, LPH/m2
Vw =Superficial velocity of toluene phase, LPH/m2
Z =Packed height, m

PRECAUTIONS & MAINTENANCE INSTRUCTIONS:

1. Interface should not be disturbed during the experiment.
2. Don’t exceed the flow rate above 15 LPH.
3. Always use clean water & ensure that there are no foreign particles in it.
4. Always clean the column feed tanks & collecting tanks properly after experiment is
over.
5. Never use feed tanks to store the chemicals used in the experiment.
6. Always drain the column once before running the experiment on desired second flow
rates.
TROUBLESHOOTING:
1. If any type of suspended particles are come in the Rotameter. Remove the Rotameter
clean the tube and fit that at its place.
2. If there is any leakage tight that part or remove that and refix that again after wrapping
Teflon tape.
3. If Rotameter fluctuating more than average tight control knob of it.
REFERENCES:

1. Coulson & Richardson’s, “Chemical Engineering”Vol-2, 4th ed, Asian Books Pvt.

Ltd, ND, 1998, Page 519-520, 584-591.

2. Binay K.Dutta, “Principles of Mass Transfer and Separation Processes”, Prentice Hall

of India Pvt Ltd., ND, 2007, Page 128-132, 455-456.