INSTITUTE OF CHEMICAL TECHNOLOGY

(University under Section -3 of the UGC Act 1956)

Maharashtra Govts Elite Status and Centre of Excellence
Matunga, Mumbai 400019

Chemical Engineering Laboratory Manual
Academic Year: 2014-2015
Semester VII

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Safety rules and regulations to be followed in CE Laboratory
during practical

1. Students must wear decent proper clothing, clean aprons and shoes during
experimentations. Besides, the use of safety goggles and hand-gloves is advised.
2. Student must perform experiments in small groups and only under the supervision of
their teachers. No experiments should be done on holidays and outside working hours.
3. Students must make themselves familiar with the experimental procedures, which are
outlined in their manual, before starting any experiment.
4. Student must not leave their experiments unattended.
5. Students are advised to read the material safety data sheets for chemicals, which they
are handling.
6. All chemicals and glassware must be handled and stored with care.
7. Any problem noticed in any experimental set-up must be immediately reported to the
supervisor.
8. Any injury, that may possibly occur, must be immediately reported to the supervisor.
9. Eating or drinking water inside the laboratory is strictly prohibited.
10. The use of laptops and mobile phones inside the laboratory is strictly prohibited.
11. Computers in laboratory are not for personal use.
12. Discipline must be followed at all times inside the laboratory.


Strict action will be taken against those, who fail to adhere to these rules and regulations.





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INDEX
1 Characterization of solid suspension in mac 1
2 Characterization of gas liquid dispersion in mac 4
3 Hydrodynamics of packed extraction column 7
4 Gas absorption in packed column 11
5 Gas absorption with chemical reaction in bubble column 15
6 Gas absorption in mac 18
7 Spray extraction 22
8 Properties of copper disc dissolution 26
9 Solid dissolution with instantaneous reaction 28
10 Liquid liquid equilibrium 31
11 Kinetics of condensation polymerization 36
12 Kinetics of dehydration of tert. Butanol 39
13 Characterization of gas solid fluidization 43
14 Camphor balls 48
15 Gas induced impeller 50
16 Cooling tower 52
17 Chiller characterization 56
18 Gas chromatography 60
19 Process control experiments ##


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1. CHARACTERIZATION OF SOLID SUSPENSION IN MECHANICALLY AGITATED
CONTACTORS
Aim:
1. To study the particle behavior in process of solid suspension in stirred tank and to
observe the effect of type and size of impeller, clearance ration and amount of solid
concentration on the power required for complete-off-bottom suspension
2. To determine critical impeller speed for complete solid suspension.
Apparatus:
Radial flow and axial flow impellers of different sizes, solid resin, baffled tank and
tachometer
Procedure:
1. Fill the tank with water such that the height of water is equal to the diameter of the tank
2. Add 25 gram of resins
3. Start the motor and increase the speed of the disc type turbine impeller gradually for a
fixed clearance ratio.
4. Note down the critical speed at which complete-off-bottom suspension of particles
occurs. Also find weight to be added in tht pan for equilibrium.
5. Now keeping the same amount of resin find out the critical speed for different size of
impeller.
6. Repeat (3) to (5) for pitched blade turbine
7. Repeat (3) to (5) taking 50 and 60 g of resin.
8. Plot power consumed vs amount of resins. ln (critical speed) vs ln (amount of resin) and
PNc vs D/T for the impellers. Here PNc is the power consumed at critical speed.
Data:
1. Diameter of tank =
2. Diameter of impeller =
Power number of impeller Np
3. Six bladed turbine = 1.52

2 | P a g e

4. Six pitched (45
o
) blade turbine =5.05
5. Dead weight of the pan =
6. Distance of the application of the torque from the center of the vessel =

Observation table:

wt of resin
(gm)
wt in pan
(gm)
critical speed
(rpm)
D
i
s
c

t
u
r
b
i
n
e

D = 5 cm
5
10
15
20
D = 10 cm
5
10
15
20
P
i
t
c
h
e
d

b
l
a
d
e

t
u
r
b
i
n
e

D = 5 cm
5
10
15
20
D = 10 cm
5
10
15
20

Formulas:
1. Power calculated by power number method is given by:

2. Power calculated by Torque method is given by:

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Notations used
P - Power consumed, watt
NP - Impeller power number, dimensionless
NC - Impeller speed, rps
D - Diameter of impeller, m
- Torque
- Torque angular velocity

Graphs to be plotted:
1. Power consumed vs Amount of resin
2. ln (critical speed) vs ln(amount of resin)
3. PNc vs D/T

Conclusions and comments:














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2. CHARACTERIZATION OF GAS LIQUID DISPERSION IN MAC

Aim:
To study gas liquid dispersion and observe effects of gas flow rate, clearance and type of
impeller on critical impeller speed
Apparatus:
Tank, impeller of different types and sizes, tachometer, sparger, etc.
Procedure:
1. Fill the vessel with water up to a known height.
2. Select a particular impeller with its known diameter and position it at the center of
the vessel with a known clearance.
3. Adjust the gas sparger just beneath the eye (the center) of the impeller.
4. The gas is passed through the sparger with a known flow rate.
5. Start the motor of the impeller and adjust the impeller speed till the complete gas
dispersion just starts.
6. Note down this impeller speed with the help of tachometer.
7. Repeat the same procedure for various gas flow rates keeping other parameters
constant.
8. Similarly, find the variation of one of the following parameters with impeller speed:
- Type of impeller
- Impellor diameter
- Clearance
- Liquid volume
Precautions:
- Tachometer readings should be taken with care so that no inaccuracy occurs due to
vibrations etc.
- The sparger and the impeller must always be perpendicular to the base of the tank
so that no non uniformity in mixing occurs.


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Data:
Diameter of the tank =.. cm
Height of liquid in the tank = .. cm
Observation table:
1. Pitched blade turbine
Sr. No Gas flow rate
Vg (cc/s)
Critical speed Nc (rpm)
For three different clearances
1
2
3
4
5
2. Disc turbine
Sr. No Gas flow rate
Vg (cc/s)
Critical speed Nc (rpm)
For three different clearances
1
2
3
4
5

Formula:
Correlation for Critical Impeller Speed:
1. For disc turbine

cd
N =
2
25 . 0 5 . 0
) (
) ( * ) ( * 4
D
T Q
g

2. For pitched blade turbine

cd
N = * ) ( * ) ( * 143 . 2
88 . 1 06 . 1
D T (Vg)
0.35

Notations used
Ncd - critical impeller speed, rps
Qg - gas flow rate
T - diameter of the tank, m
D - diameter of impeller, m

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Vg - velocity, m/s

Graphs to be plotted:
Critical Impeller speed Vs. Gassing rate
Critical Impeller speed Vs. Liquid volume
Critical Impeller speed Vs. Clearance
Critical Impeller speed Vs. Impeller diameter
The above graphs can be plotted for different types of impellers.

Conclusions and comments:



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3. HYDRODYNAMICS OF PACKED EXTRACTION COLUMN
Aim:
To determine the variation of fractional phase hold-ups at varying dispersed and
continuous flow rates

Apparatus:
Packed tower, rotameters, storage tanks, overflow line, measuring cylinders, stopwatch

Procedure:
Part-I
1. Start dispersed and continuous phase flow rates after first filling up the column with
desired continuous phase.
There are two sets to be performed
1. Water as dispersed phase (interface at the bottom)
2. Organic as dispersed phase (interface at the top)
2. Maintain the continuous phase and dispersed phase flow rate to a particular value of
rotameter reading.
3. Allow steady state to be reached (Wait for ten minutes for steady state to be
obtained).
4. Close all inlets simultaneously. The dispersed phase will coalesces at the interface
because of which the position of the interface changes.
5. Note down the change in interface height on the scale attached on the column (if
organic phase is dispersed phase then area of the column x rise in interface level will
give the volume of the dispersed phase. Proper care should be taken during
measuring hold-up when water is dispersed phase) or drain the accumulated
dispersed phase till the original level is attained. Collect the drained phase and
measure its volume.
6. Repeat for different dispersed flow rates for the same continuous phase flow rate
(5-6 readings).

Part-II

Exchange the phases of part I i.e. make the dispersed phase of part I the continuous
phase and vice versa. Repeat the above procedure as given in part I

Data:
1. Column diameter =. m
2. Packed height = . m

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3. Density of organic phase = 834.4 kg/m
3
(for 2-ethylhexanol)
4. Interfacial tension= 10.9 dyne/cm
5. Voidage, k = 0.68
6. Effective volume = (/4)*d
2
*L*Voidage

Observation table:
Part I:
Continuous phase:
Dispersed phase:

No. Continuous phase Dispersed phase Interfacial
level
Vol
collecte
d
(cm)
Volume
collecte
d (ml)
Time
(sec)
Flow
rate
(ml/s
)
Volume
collecte
d (ml)
Time
(sec)
Flow
rate
(ml/s)
Initia
l
(cm)
Final
(cm)



Part II:
Continuous phase:
Dispersed phase:

No. Continuous phase Dispersed phase Interfacial
level
Vol
collecte
d
(cm)
Volume
collecte
d (ml)
Time
(sec)
Flow
rate
(ml/s
)
Volume
collecte
d (ml)
Time
(sec)
Flow
rate
(ml/s)
Initia
l
(cm)
Final
(cm)






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Sample calculations:
1. Check for dpacking > dFC
Where, dFC = 2.42*(/(P*g))
0.5


2. Effective volume = volume of packed colume *voidage
= (/4)*d
2
*L*voidage
3. Velocity of dispersed phase (Vd)
= (Volumetric flow rate /column cross section area)

4. Velocity of continuous phase (Vc)
Vc = (volumetric flow rate/ column cross section area)

5. Dispersed phase holdup (d)
d = (Dispersed phase volume/effective volume)

6. Plot a graph of (Vd+(k*Vc)/(1- d)) vs (k* d *(1- d)). The slope is k*Vo, knowing
packing Voidage (k), Calculate Vo

7. Calculate drop diameter by the following correlation:
|
|
.
|

\
|
|
|
.
|

\
|
A
=
d
d o
p
v
k v
g
d
c

o
5 . 0
92 . 0


8. Calculate interfacial area from the drop diameter
p
d
d
k
a
c 6
=


Notations:
dp - drop diameter
dpacking - packing size
dFC - critical size of packing (usually 1.27 cm or more)
d - dispersed phase holdup
o - Interfacial tension
- density difference of phases
Vc - velocity of continuous phase
Vd - velocity of dispersed phase
Vo - Characteristic droplet velocity



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Calculation table:

No Vc
(cm/sec)
Vd
(cm/sec)
(Vd+(k*Vc)/ (1- d)) (k* d * (1- d)) dp
(cm)
a

1
2
3
4
5
6


Results:

Conclusions and comments:

Graphs to be plotted:
1. d vs Vd for cases 1 and 2
2. (Vd+(k*Vc)/(1- d)) vs (k* d *(1- d))
3. a vs Vd





















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4. GAS ABSORPTION IN PACKED COLUMN

Aim:
To determine the effective interfacial area for gas liquid contacting in a packed column
employing a chemical reaction

Procedure:
1. Pass approximately 10% CO2-air mixture from the bottom of the column and keep it
constant throughout the experiment.
2. Start aqueous NaOH flow rate and maintain a liquid seal at the bottom (so that no
gas bypasses from bottom)
3. For a constant gas flow rate, vary liquid flow rate (1-5 cm
3
/s) for 5 different values
and take readings at the steady state.
4. Analyze outlet sample for Na2CO3 formed.
5. Take at least 5 readings for different NaOH flow rate

Method of analysis:
2NaOH +CO2 ---- > Na2CO3 +H2O
BaCl2 + Na2CO3 ---- > BaCO3 + 2 NaCl
a) Titrate a known volume of sample with HCl to find out total alkalinity (T1)
b) Titrate known volume of sample after adding excess of BaCl2 with HCl to find NaOH
concentration (T2)
Observations:
- Diameter of column= m
- Height of packing= m
- Normality of NaOH used= N
- Normality of HCl used = N
- Calibration of air rotameter: y (mL/min) = 0.881*x+1063
- Calibration of CO2 rotameter: y (mL/min) = 465.3*x + 392.7
- Diffusivity of CO2 in NaOH=DA=1.96*10
-9
m
2
/s
- Second order rate constant at 30
o
C = k2 =2*10
4
m
3
/(kmol.sec)

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- H - Henry's constant for CO2-buffer system = 0.0224 kmol/m
3
.atm

Observation Table:
Sr. No NaOH flow rate Titrate reading
T1, ml
Titrate reading
T2, ml
Normality of
NaOH by T2(N)
1
2
3
4
5
6

Calculations
The experiments involves computation of rate absorption (with reaction) of CO2 in aqueous
solutions of NaOH, as well as computation of solubility of CO2 in aqueous solutions of
NaOH+Na2CO3 . For these purposes, we need to calculate the following:
1. Inlet concentrations of NaOH (kmol/m
3
), (Note: initial concentration of Na2CO3 =
nil)
2. Outlet concentration of NaOH as the absorption (with reaction) proceeds (kmol/m
3
)
The above requirements are achieved as described here below:
1. Inlet concentrations of NaOH, i.e concentration of unreacted NaOH solution at the inlet
of packed column:
- Since NaOH is a strong base, titrate a known volume of unreacted NaOH solution
versus standard Oxalic acid, using Phenolphthalein as indicator
NNaOH-INLET = NOXALIC ACID * VOXALIC ACID / VNaOH-OUTLET
- Since equivalent weight = molecular weight in case of NaOH
[NaOH]INLET = NOXALIC ACID * VOXALIC ACID / VNaOH-OUTLET
2. Concentration of unreacted NaOH at the outlet of packed column
a) In order to find the concentration o unreacted NaOH at the outlet of packed column, then
it is titration versus standardized HCl, using Phenolphthalein as indicator (as above in 1.)
[NaOH]OUTLET = NHCl * VHCl / VNaOH-OUTLET

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b) In order to avoid interference of Na2CO3 in the titration, it is precipitated by reaction
with an excess of 10% aqueous solution of BaCl2
BaCl2 + Na2CO3 ---- > BaCO3 + 2 NaCl
3. Rate if absorption of CO2 in NaOH solution:
a) Rate if absorption of CO2 in NaOH solution can be fond from fall in [NaOH]. The reaction
of CO2 with NaOH is
2NaOH +CO2 ---- > Na2CO3 +H2O
- This means that 1 kmol of CO2 reacts with 2 kmol of NaOH
Therefore, rate of absorption per unit packed volume of packed column = RAa =
([NaOH]INLET - [NaOH]OUTLET)* NaOHflowrate / (2*Volumepacking) =
([NaOH]INLET - [NaOH]OUTLET)* NaOHflowrate / (2*(/4)*dcolumn
2
*Hpacking)
4. Determination of log mean partial pressure of CO2
-
Let inlet flow rate of CO2 =fCO2-in
Molar inlet flow rate (ideal gas law) =PV/RT= (1 atm* fCO2-in)/(0.082*303.15)
= nCO2-in kmol/s
Molar outlet flow rate of CO2 (ideal gas law) = nCO2-in - nCO2-reacted/absorbed
= nCO2-out kmol/s
- Similarly, Let flow rate of Air = fair
Since air does not react with NaOH,
Inlet flow rate of air = outlet flow rate of air
Flow rate of air (ideal gas law) = PV/RT= (1 atm* fair)/(0.082*303.15)
= nair kmol/s
(Partial pressure of CO2)inlet = (PPCO2)inlet = 1 atm* (nCO2-in/( nCO2-in + nair ))
=____________ * 101.325 kN/m
2

And (Partial pressure of CO2)outlet = (PPCO2)inlet = 1 atm* (nCO2-out/( nCO2-out + nair ))

14 | P a g e

=____________ * 101.325 kN/m
2


Log mean partial pressure of CO2 is given by:

5. Solubility if CO2 in NaOH
[A*] = H x

kmol/m
3

7. The G/L interdacial area is given as
a = (RAa)/([A*](DAK2 [NaOH])
0.5
) m
2
/m
3
of packings
[A*] - solubility of CO2 in NaOH
DA - Diffusivity of CO2 in NaOH solution = 1.96*10
-9
m
2
/s
K2 - second order reaction rate constant between CO2 and NaOH at 30
0
c = 2*10
4

m
3
/kmol.s

Graphs to be plotted:
1. a versus flow rate of NaOH

Results, Conclusions and comments:


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5. GAS ABSORPTION WITH CHEMICAL REACTION IN BUBBLE COLUMN:
Aim:
To determine the liquid side mass transfer co-efficient (kL.a) in a bubble column using the
theory of gas absorption with chemical reaction

Apparatus:
A cylindrical column, gas sparger, CO2 source, air compressor, rotameter, and titration
assembly

Chemicals:
Buffer solutions, NaOH (0.5 N), HCl (0.5 N), BaCl2 (0.5 N), Oxalic acid (0.2 N),
phenolphthalein indicator and methyl orange indicator

Procedure:
1. Charge 2 litre buffer solution and pass CO2- air mixture for 15 minutes. CO2 should
approximately be 10%.
2. Standardize the given NaOH and HCl solutions
3. At the end of 10 min, take out sufficient amount of sample for analysis
4. Titrate 10 ml of sample against 0.5 N HCl using methyl orange as indicator to get the
titration reading (T1)
5. Also titrate 10 ml of sample + 25 ml BaCl2 (0.2 N) + 25 ml NaOH against
phenolphthalein indicator to get the titration reading (T2)
6. Initial buffer solution (without CO2, blank) should be titrated in the same way as
mentioned in step 5.
7. Note down the rotameter readings for air and CO2 rotameter (exact values of flow
rate in cm
3
/s can be read from the graphs provided with the experimental setup
8. Also note down the dispersion height.

Reactions:
Na2CO3 + H2O + CO2 2NaHCO3

NaHCO3 + NaOH Na2CO3 + H2O

Na2CO3 + BaCl2 NaCl +BaCO3

16 | P a g e

Observation data:
2. Air rotameter reading = cm
3
/sec
3. Carbon dioxide gas rotameter reading = cm
3
/sec
4. Amount of buffer taken in column = lit
5. Initial height of buffer in column (Hi)= cm
6. Diameter of column (D) = cm
7. Cross sectional area of column (A)= m
2

8. Reaction time= min
9. Henry's constant for CO2 = 2.82*10
-4
kmol/kN.m
10. Conc. of NaOH (N1) = N
11. Conc. of HCl (N2) = N


Analytical calculations:
The difference in the initial (standardization) and final (T2) reading gives the amount of
NaOH consumed and hence the bicarbonate concentration formed in the reaction is
determined using this we can find out the amount of CO2 absorbed
Dispersion height = cm
Titration reading (T1) = ml
Titration reading (T2) = ml


Observation table:
Sr. No Initial height,
cm
Final height,
cm
Titration
reading (T1),
ml

Titration
reading (T2),
ml

1
2
3
4
5
6


Calculations:
1. Volume of reaction mixture (V) = (/4)*d
2
*Ls
Where, Ls = dispersion height of buffer

2. Conc of NaOH (N3)
N3*V3 = N2*V2

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V3= Total volume taken in flask (25 ml BaCl2 + 25 ml of NaOH +10 ml sample)
N2, T2 = given in data
3. Conc. of NaOH reacted (N4) = (N1-N3)= gmole/lit.
4. Moles of NaOH reacted = nNaOH = (N4*V)= gmole
1 mole of NaOH reacted = 1 mole of Na2CO3 formed
5. Moles of Na2CO3 formed = nNa2CO3 = (N4*V)= gmole
6. Moles of CO2 absorbed (Q) = (moles of NaOH reacted)/ 2*t= gmole/sec
7. Reaction rate (Ra) = (N4/t)= gmole/lit.sec
8. Moles of (n-CO2) in = (CO2 flow rate)/ vol of air (V1) = gmole/sec
Volume of air at NTP:
1 gmole of air = 22414 cm
3
/gmole (V1)
9. Moles of air in = (n-air)in = (air flow rate)/ vol of air (V1)= gmole/sec
10. Moles of CO2 out = (n-CO2)out = (n-CO2)in -(n-CO2)abs (Q)= gmole/sec
11. P.P. of CO2 in= = (PPCO2)in = 1 atm* ((n-CO2)in /((n-CO2)in + (n-air)in))= atm
12. P.P. of CO2 out= = (PPCO2)in = 1 atm* ((n-CO2)out /((n-CO2)out + (n-air)in))=
atm
13. Finding out H
I-(NaOH)= Ci =(Cin+Cout)/2 = (N1+N3)/2= gmole/lit
I-(Na2CO3)=1.5*( n-CO2)abs (Q) = gmole/lit
Log10 (H/Hw) = - (Ks*I)= - {(Ks)NaOH* INaOH + (Ks)Na2CO3* INa2CO3}
Hw = 2.82*10
-4
kmole/kN.m
H = kmole/kN.m

14.

15. [A*] = H x

16. [KLa] = [Ra]/[A*]= sec
-1


Results, conclusions and comments:

18 | P a g e

6. GAS ABSORPTION IN MECHNICALLY AGITATED CONTACTOR

Aim:
To determine the mass transfer co-efficient (kL.a) in mechanically agitated contactor using
chemical method
Procedure:
1. Charge suitable amount of buffer solution in MAC (H/D =1 approx.) the quantity charged
should be noted
2. Pass air-CO2 mixture for 15 minutes at suitable speed of revolution. CO2 should
approximately be 10%.
3. Note dispersion height. Clear liquid height etc.
4. Analyze initial and final samples
5. repeat for 5 different rpm in the range 500-1200 rpm at constant gas flow rate.

Analytical procedure:

Na2CO3 + H2O + CO2 2NaHCO3

NaHCO3 + NaOH Na2CO3 + H2O

Na2CO3 + BaCl2 NaCl +BaCO3

a. 10 ml sample + 25 ml NaOH + 25 ml BaCl2 against 0.5 N HCl with phenolphthalein (T2)
b. 25 ml 0.5 N NaOH vs HCl-Blank (T1)
c. 10 ml sample against HCl with methyl orange (T)

Sample volume may be adjusted to get T readings in the range 10-20
Analytical calculations:
T gives total alkalinity. From T1 and T2 volumes of NaOH consumed and hence bicarbonate
concentration is found. Hence, bicarbonate concentration is calculated.

19 | P a g e


Data presentation:
Tabulate for each rpm the amount of buffer solution charged, the gas flow rate, the time of
agitation and the titration reading
Data: For [CO3
2-
]/[HCO3
-
]= 2
K2[Bo] =1.2 sec
-1

DAK2[Bo] =1.6*10
-5
(cm/sec)
2

Diameter of MAC: D =
Observations:
Initial height of buffer solution (H) = cm
CO2 flow rate= cm
3
/sec
Air flow rate= cm
3
/sec
Reaction time= sec
Blank titration reading of buffer solution= gmole/lit

Observation table:
Sr. No Speed, rpm Titration reading,
ml
Titration reading,
ml


Calculations:
NaOH reacted =(a-T2) *0.5/25 (mol/lit)
Moles of NaOH reacted = volume *NaOH reacted
= (/4)*D
2
*H*NaOH reacted (moles)

1 mole of NaOH reacted = 1 mole of Na2CO3 formed

20 | P a g e

Ra= (moles of Na2CO3 formed)/(reaction time*volume)
2 moles of NaOH = 1 mole of CO2
Moles of CO2 absorbed = (moles of NaOH reacted)/ 2*(reaction time)
Moles of CO2 in (n-CO2) in = (CO2 flow rate)/ vol of CO2 per mole
= (CO2 flow rate)/22400
Moles of air in = (n-air)in = (air flow rate)/ vol of air per mole
= (air flow rate)/22400
Moles of CO2 out = (n-CO2)out = (n-CO2)in -(n-CO2)abs
P.P. of CO2 = 1 atm* ((n-CO2)out /((n-CO2)out + (n-air)in))
For Na2CO3,
I= 3Ci=3/2*moles of CO2 adsorbed
(Ks)Na2CO3 = 0.094 m
3
/kg
For NaOH,
I=Ci= moles of CO2 adsorbed
(Ks)NaOH = 0.137 m
3
/kg
Log10 (H/Hw) = - (Ks*I)= - {(Ks)NaOH* INaOH + (Ks)Na2CO3* INa2CO3}
Hw = 2.82*10
-4
kmole/kN.m
H=
[A*] = H x PP of CO2
[KLa] = [Ra]/[A*]
Estimate power input per unit volume using the following equation:

Np= power number=5
D= impeller diameter

21 | P a g e

T= tank diameter
N= rps
Graphs:
1. Plot a graph of KLa vs rpm and comment on the effect of rpm on KLa
2. report the effect of rpm on dractiona; gas holdup
3. Plot a graph of Po/V vs rpm and comment on the effect of rpm on Po/V
Results:
Conclusion
Comments





















22 | P a g e

7. SPRAY EXTRACTION

Aim : To study the hydrodynamics of a liquid-liquid spray column and determine the
overall mass transfer coefficient.

Procedure :
1. Fill the column with methyl isobutyl ketone (MIBK) to such an height that the tips of the
dispersed phase (water) nozzles dip into the continuous (MIBK) phase. The system will
extract pure MIBK into the dispersed water phase.
2. Constant water flow rate is maintained and outlet from the column is so maintained
that the interface in the column remains at a constant level. Note this level.
3. Allow the column to operate in steady state for ten minutes and then collect 30-40 ml of
the outlet water phase sample.
4. Close inlet and outlet of column simultaneously and note the rise in the level of
interface. Knowing the column diameter the dispersed phase holdup is calculated.
5. The interface is brought to original level and the next value of dispersed flow is
experimented with in the same manner.
6. Analysis of MIBK in extract aqeous phase
7. Take at least 6 readings for different water flow rates
The analysis is done as follows:
Reaction of ketone with hydroxylamine is used to determine MIBK concentration.
R - C - R' + NH2OH.HCl -----> R - C - R' + HCl + H2O
|| ||
O NOH
The free HCl is used for RR' CO determination.


23 | P a g e

Procedure for analysis
5 ml of sample is mixed to 25 ml standard hydroxylamine hydrochloride solution. The
mixture is refluxed for about thirty minutes on a steam bath with intermittent shaking. The
refluxed liquid is titrated against standard NaOH using bromophenol blue as an indicator.
End point is yellow to green to a final blue. A blank titration of standard hydroxylamine
solution is also done. The difference in readings can give the MIBK concentration in the
sample taken
The set of readings on superficial dispersed phase velocity (vc = 0), dispersed phase
fractional holdup and outlet MIBK concentration (ci = 0) are used for further calculations.

Data presentation :
For each value of the dispersed phase flow rate, note down the initial and final level
of the interface, which should correspond to the fractional holdup. Measure the flow rates
and tabulate the corresponding titre reading.
Data :
Density of MIBK : 600 kg / m
3

Density of water : 1000 kg / m
3

Viscosity of MIBK : 0.58 x 10
-3
Pa.s
Viscosity of water : 0.95 x 10
-3
Pa.s
Interfacial tension (o) : 10 dynes/cm

Calculations :
1. Determine the dispersed phase holdup cd, dispersed phase velocity (vd) and slip velocity
vs for each flow rate.
a) Cross section area of column = /4*D
2
=_____m
2

b) dispersed phase velocity, vd = (volumetric flow rate)/(cross-sectional area)
= ______ m/s

24 | P a g e

c) continuous phase velocity is zero
vs = dispersed phase velocity (vd)/ cd

2. Make a plot of vs against cd and determine the extrapolated value of uT (y-intercept :
vs at cd = 0 ).
3. Estimate average droplet diameter (dp) to find the volume of a single drop (VF) by trial
and error (a non-linear algebraic equation to be solved by any numerical method - eg.
Newton - Raphson).
(a) VF from correlation:
VF + 4.11 (10
-4
) VF
2/3
( D . vn
2
/ A ) = 21(10
-4
) (o . DN /A) + 1.069 (10
-2
).
(DN
0.747
. vn
0.365
. C
0.186
/ A )
1.5


where VF = volume of single drop
vn = velocity of dispersed phase through the nozzle
DN = diameter of the nozzle

(b) Calculate average droplet diameter (dp)
dp = [(6/t) VF ]
1 / 3
4. Estimate the available specific interfacial area 'a' for each reading.
a = (6 cd ) / dp
5. Calculate the log mean concentration gradient as follows :
Let C - MIBK conc. in outlet stream, kmol/m
3

Ci - inlet concentration of MIBK = 0
C * - saturation conc. of MIBK in water, kmol/m
3
= 0.1899 kmol/m
3

6. Find the volumetric rate of mass transfer
RA a = (C - Ci) . QD /V
where QD = volumetric flow rate of dispersed phase (water)
V = contactor volume

25 | P a g e

7. Volumetric Mass transfer coefficient for dispersed phase
kd a = RA a / ( ACLM )
8. Continuous phase mass transfer coefficient and dispersed phase mass transfer
coefficients can also be estimated by the following correlations for spray columns.
kc = 0.725 [ dp vs c / c ]
- 0.43
. [ c / (c . Dc) ]
- 0.58
. [ vs (1-cd) ]
kd = 0.00375 UT / [ 1 + d / c ]
9. Overall mass transfer coefficient for the dispersed phase can then be estimated, since "a"
has earlier been estimated.
1 = 1 1
------- ------ + -------
Kd a kc a kd a

Graphs :
1. Plot "a" and predicted kd vs. experimental dispersed phase velocity (vd) on a single
graph.
2. Plot the mass transfer coefficients vs. dispersed phase velocity on a log-log scale.

Results, Conclusions and Comments:










26 | P a g e

8. COPPER DISC IN ACIDIFIED POTASSIUM DICHROMATE

Aim

To determine solid-liquid mass transfer coefficient, ksl and study the effect of speed of
agitation.


Procedure
1. Take 400 cc of acidified dichromate solution and rotate Cu disc in it for 15 mins. at
known rpm.
2. Analyze initial and final solution for dichromate conc.
3. Note down disc dimensions before and after run.
4. Repeat for 5 rpm in the range 300 to 1200 rpm.
Analysis:
1. Blank- 25 ml 0.2 N FeSO4, acidify with 25 ml 4N H2SO4 vs. std. K2Cr2O7 (0.1N) + indicator
--- ( Tb)

2. 10 ml sample + 25 ml 4N H2SO4 + 25 ml 0.2N FeSO4 + 2ml n-phenyl anthranilic acid
indicator vs. std. K2Cr2O7. End point pale green to reddish brown( Tf ).

3. Repeat (2) with 10 ml of unreacted acidified potassium dichromate soln. ( Ti )

Caution
Keep the titrated flask (blank reading) for comparison and titrate for the same shade as the
end point. When green color changes to reddish brown, stop addition of dichromate from
the burette.

Data Presentation
Tabulate the disc dimensions before and after, titration reading Tf and rpm for each
reading.

Speed, rpm Titrate reading, ml Disc diameter, mm



27 | P a g e

Calculations

1. Calculate [ Bi ]
[ Bi ] = [K2Cr2O7] std ( Tb Ti ) / sample volume , gmeq./ lit

2. Calculate [ Bf ]
[ Bf ] = [K2Cr2O7] std ( Tb Tf ) / sample volume , gmeq./ lit

3. From eqn. (2), find the value of k sl in cm/s.

4. From initial and final conc. of dichromate, calculate the rate of the reaction, RA a in
gmole/cm
3
s.

5. Compare k sl with the predicted value:

( Sh ) ( Sc )
1
[ 0.565/ Sc
2/3
] = 0.62 ( Re )
0.5

where Sh = ( K sl d / D ) d = disc diameter
Sc = ( / D ) D = 9.07 x 10
-6
cm
2
/s
Re = ( d
2
N / ) = 1.19 x water N = rps
6.

Bi and Bf are initial and final concentrations of B, respectively
Ksl = sol-liq mass transfer coefficient
Results

Tabulate k sl predicted and experimental and experimental for each rpm. Plot a graph N vs.
k sl and comment. Also plot a graph of k sl predicted vs. experimental and comment on the
match between the two.
Comment on effect of N on k sl and match between k sl experimental and predicted.








28 | P a g e

9. SOLID DISSOLUTION WITH INSTANTANEOUS REACTION

Aim:
To study solid dissolution with instantaneous reaction and predict enhancement obtain
due to reaction

Procedure:
1. Measure the dimensions of benzoic acid cylinder and rotate it at a low speeds in
aqueous NaOH solution (300 ml) in a beaker for 10 min
2. After 10 min immediately remove benzoic acid cylinder from the solution and titrate
NaOH sample.
3. Measure the cylinder dimensions
4. Repeat for 5 NaOH concentrations 0.1 to 0.5 N
5. To find out physical dissolution rate benzoic acid cylinder is rotated at the same rpm in
200 ml of water for 30 min. samples are withdrawn (5 ml) for every 5 min time interval
and analyzed for acid content. Add 5ml of makeup water when you withdraw the
sample.

Note:
1. Analyze 10 ml sample of aq. NaOH before and after the experiment vs 0.5 N HCl
2. Physical dissolution titration 10 ml blank sample vs 0.02 N NaOH

Observation table:
A) For dissolution with reaction:
Sr. No NaOH, N Initital
diameter,
cm
Final
diameter,
cm
Titration
reading, ml
Amount of
sample, ml
1
2
3
4
5


29 | P a g e



B) For physical dissolution:
Time, min Titration reading,
ml
Sample amount, ml Cumulative time,
min
10
20
30
40

Data:
Diffusivity of benzoic acid = 1.04 * 10
-9
m
2
/sec
Solubility of benzoic acid = 0.01639 gmol/lit

Sample calculations:
A) Dissolution with reaction
To find the M.T.C. in presence of chemical reaction
a) Find the normality of NaOH solution after reaction
Change in normality = Initial normality of NaOH- Normality after reaction
Ra=( Change in normality*volume of NaOH taken)/ (time of reaction in sec)
= gmole/sec
a = cm
2

RAa = Ra/a gmole/sec.cm
2

k = RAa/[A*] cm/sec
[A*] = interface conc., i.e. solubility of benzoic acid in NaOH at time t

B) For physical dissolution
[A*] = [Aw]= 1.63*10
-5
gmole/cm
3

[Aw] = solubility of benzoic acid in water
[Ao]= bulk conc. Of benzoic acid in water or maximum solubility of benzoic acid in water

30 | P a g e

Plot graph of -ln(1-[A0]/[AW]) vs time
Mass transfer without chemical reaction (Ko) = slope *volume of water/ area of cylinder =
C) Enhancement factor:
| = K /K
O

theoretical enhancement factor:
1. by stagnant film theory

2. by boundary layer theory

Where,
DA= DBZ-ACID =1.04 X 10
-9
m
2
/s
DB = DOH =4.1 X10
-9
m
2
/ s
Results:
Plot graph of |,

vs [Bo]/[A*]
Comment on results wrt |, predicted and experimental











31 | P a g e

10. LIQUID-LIQUID EXTRACTION
Aim:
To construct a ternary liquid-liquid equilibrium diagram for the system Toulene-Acetic
acid--Water.

Apparatus and chemicals:
Conical flask, beaker, burette, measuring cylinder, pipette, acetic acid, toluene, water,
phenolphthalein, 2 N alcoholic KOH etc

Procedure:
1) Prepare mixtures of acetic acid and toluene of the following compositions in clean dry
flasks:
Acetic acid (ml) 0 10 30 45 60
Toulene (ml) 100 90 70 55 35

2) Add water slowly from a burette with intense stirring, into each of these mixtures till
turbidity appears and persists for some moments after stopping the stirring. Note the
water volume added. These ternary compositions are the equilibrium points.
3) Repeat (2) for different composition as given in table
4) Prepare another set of mixture of same composition as in the above table but replacing
toluene with water. Add toluene dropwise instead of water and find in the same manner
set of 5 equilibrium compositions.
5) To determine tie lines make 4 mixtures as follows:

Acetic acid(ml) 10 20 30 40
Toulene (ml) 95 90 85 80
Water(ml) 95 90 85 80

a) Take the mixtures in four different separating bottles. Shake vigorously for 10
minutes and allow settling into two layers

32 | P a g e

b) Separate the two layers and the volume and weight of each layer separately.
c) Titrate each layer with aqueous/alcoholic solutions of alkali of suitable strength
to determine acid concentration in the two phases. Calculate the weight fractions
of acid in the two phases.

6) Construct a ternary equilibrium diagram on a ternary graph paper or on ordinary graph
paper using weight fractions as the concentration units.
7) Construct the tie lines (four) on the ternary diagram and then an approximate
distribution curve.
8) Tabulate your observations as follows:

a) Water added to a mixture of toluene and acetic acid
Sr No. Volume of Acetic
acid Taken(ml)
Volume of toluene
taken(ml)
Volume of water
added (ml)
1
2
3
4
5


b) Toluene added to a mixture of water and acetic acid
Sr No. Volume of Acetic
acid Taken(ml)
Volume of water
taken(ml)
Volume of toluene
added (ml)
1
2
3
4
5




33 | P a g e

c) Observations for two phases in separating bottles:
For aqueous layer
Separating
bottle no.
Weight(gms) Volume Va
(ml)
Volume of solution
taken for titration
Vt(ml)
Burette
reading
T1(ml)
1
2
3
4


For organic layer
Separating
bottle no.
Weight(gms) Volume Vo
(ml)
Volume of solution
taken for titration
Vt(ml)
Burette
reading
T2(ml)
1
2
3
4


Prepare a spreadsheet of calculated data as shown below:
a) For water added to (acetic acid+ toluene) mixture
b) For toluene added to (acetic acid + water) mixture
c) For the separating bottles

Data Required:
Density of Acetic acid = 1.049 gms/ml
Density of Toulene = 0.866 gms/ml
Density of Water = 1.000 gms/ml



34 | P a g e


Calculations:
1) Calculate the compositions in terms of weight fractions for the three components. These
are to be used for plotting the solubility curve.
Weight of the component = (density x volume) of the component
For a given mixture calculate the weights of all three components & then find the weight
fractions as:
Weight of acetic acid
Weight fraction of acetic acid =
Sum of weights of acetic acid, toluene and water

2) Calculate the weight fractions of acetic acid in the aqueous and organic layers in each
separating bottle. These are the equilibrium compositions and represent the end points of
the tie lines.
For the aqueous layer which is titrated against alkali:
Acetic acid = alcoholic KOH
N1V1= N2V2
N1Vt = N2T1
Find the strength of acetic acid in aqueous layer (N1)
1000 ml contains (N1 x 60) gms of acetic acid
Va ml contains ? gms of acetic acid

Wt of acid in aq. layer
Weight fraction of acid in aqueous layer =
Wt of aq. layer

Similar calculations for organic layer:
Acetic acid = alcoholic KOH
N1V1= N2V2
N1Vt = N2T2
Find the strength of acetic acid in organic layer (N1)
1000 ml contains (N1 x 60) gms of acetic acid
V0 ml contains ? gms of acetic acid

35 | P a g e


3) Calculation for distribution coefficient (D):
D= (wt. fraction in org. phase)/ (wt fraction in aq. Phase)


(a)Ternary Diagram (b) Distribution Curve



A













B L K C

Figure 1: (a)Ternary Diagram and (b) Distribution Curve


Results:
Conclusions:
Comments:








36 | P a g e

11. KINETICS OF CONDENSATION POLYMERIZATION

Aim:
To study the kinetics of condensation polymerization using the reaction of Ethylene Glycol
and Adipic Acid.

Procedure:
1. Take 25ml of benzene alcohol solution in a 100 ml clean flask. Weigh the
same.(Take about 8-9 samples)
2. Weigh one mole of ethylene glycol and adipic acid separately. Charge the two in the
reactor vessel and start the stirrer.(Note that the reaction is carried out at 180
o
C.
The temperature of the bath is automatically controlled by the Jumo thermometer).
3. Start the stop watch as soon as the reaction mixture is charged in the reactor vessel
i.e. take this as a zero time.
4. After every 5 minutes switch off the stirrer and pipette out 3-4 ml of mixture from
the reactor and immediately put it into the known initial weight of benzene alcohol
samples prepared in step one. Weigh these samples flask after adding the reaction
mixture.
(Note: There is difficulty while withdrawing the sample from the reactor vessel.
Since the reaction mixture coagulate in the pipette. Hence it is advisable to keep
the pipette in the hot water bath before removing the sample).
5. Repeat the same procedure and continue for 45 minutes withdrawing the sample
after every 5 minutes.
6. Titrate the samples against 2N alcoholic KOH solution using phenolphthalein as the
indicator.

37 | P a g e

Observation table:

Obs
No.
Time
(min)
Initial
weight
of
sample
(Kg)
Final
weight
of
sample
(Kg)
Titration
reading
(ml)
Conc.
(gmol/lit)
d/dt (conc)
(gmol/lit.s)
ln (d/dt
(conc))
ln
(conc)
1
2
3
4
5
6

Sample calculations:
1. To find the concentration of unreacted adipic acid:
N1V1=N2V2
N1=C1N
CA= C1/2 gmol/lit
N1=Normality of acid, N2= Normality of KOH, V1= volume of acid, V2= Volume of KOH

2. First plot the graph of CA vs time to get the (dCA/dt)t
Then plot the graph of ln (dCA/dt) vs ln (CA)
3. To find degree of polymerization
1. Assume density of reaction mixture = 1 g/cc
Wt. of reactants= 146+62= 208 g
Volume of reactants = 208 cc
2. Total volume withdrawn = X cc
Total volume remaining = (208-X) cc
3. Moles of acid remaining = NA= Conc.*(208-X/1000)= Y moles

38 | P a g e

4. Moles of ester group formed (NE)= (1-Y) moles
5. Degree of polymerization (P) = (NE/NA)=
6. Average degree of polymerization = (Xn)= 1/(1-P)

Results:
- Order of reaction with respect to Adipic acid =
- Rate constant for the reaction=
- Degree of polyemerization=
- Acerage degree of polymerization=

Conclusion:


Comments:

















39 | P a g e

12. KINETICS OF DEHYDRADTION OF TERT-BUTANOL

Aim:
To ascertain the kinetics of the dehydration of tertiary butanol to gaseous iso butylene
using an acid catalyst.

Procedure:
1. Heat the reaction vessel with 80 ml t-butanol to 80
o
C.
2. After a constant bath temperature is achieved, charge 5 gm of resin in 20 ml of t-butanol
through a funnel and addition nozzle. Close the nozzle immediately so that the system
becomes air tight (Wet the soap film meter before adding the catalyst).
3. Start the stop watch immediately after adding the catalyst. Measure the evolution rate
after suitable interval of film (Initial readings are important for determining the
reaction kinetics). The observation consists of instantaneous evolution rate of
isobutylene gas and cumulative time.
4. Measure the evolution of isobutylene gas for about 45 minutes.

Sample Calculation:
The reaction may be represented as
A ----------> C + B
(t BuOH) (Water) (Isobutylene)
The reactant, t-Butenol is in the liquid form and the products formed are isobutylene gas
and water. Here the temperature of the reaction mixture is maintained at 80
0
C and
therefore along with the gaseous products some of the water formed escapes as water
vapor.
1. First calculate the volume of the gas evolved in the section of the soap film meter
pertaining to the fixed length considered (eg. 10 cm or 15 cm) at any t:
G cm
3
= cross sectional area x (10 or 15)
2. Calculate the vapor pressure of water at room temperature given by Ps in mmHg

40 | P a g e

3. Assuming ideal gas law. Calculate the number of moles n, in G ml of the gas. Convert G to
m3 for consistent units, and assume pressure to be 101.325 KPa
4. The moles of isobutylene gas at any t are given by:
B' gmoles= (760-Ps)*n/760
5. Now, the rate of evolution of isobutylene gas at any instant t is given by

Where t is the mean time for gas evolution for the fixed length of soap film meter.
Calculate dB/dt at all measured mean evolution times corresponding to the particular
cumulative time. Plot a graph of dB/dt vs t (cumulative).
6. Calculate by area measurement, the total amount of B evolved from t=0 to different
times, t.
7. At any time t then, amount of unreacted t-Butanol is given by:
A. gmoles= (100ml*A/MwA)-B
Where, A is the density and MwA, the molecular weight of t-Butanol
8. Amount of water vapor at any instant is given by:
C gmoles = B (Ps/ (760-Ps))
9. The total volume of the reaction mixture at any instant is that occupied by the unreacted
t- Butanol and water left behind after some of it has escaped as vapor.
V = (A MwA / A) + ( [ B-C] MwC / A)
10. The rate and order of the reaction is found out by taking into account the water
concentration which is stoichiometrically equal to the amount of isobutylene formed, hence
the conc of water at any instant is given by
Cc gmoles/ml = B/V

41 | P a g e

Estimate values of Cc at various times t and plot a graph pf Cc versus t. Obtain values of
dB/dt at different instants of time-t
11. The rate of appearance of c for changing volumes is

Calculate the values of m and k from the plot of

vs ln Cc
Observation table:
5 cm 10
cm
15
cm
20
cm
Cumulative
time, t
B'/t B A C V
1
2
3
4
5

Ca Cc dA/dt ln Ca ln(-dA/dt/v) dC/dt ln(Cc) ln(dC/dt/V)
1
2
3
4
5

Similarly carry out the calculations for the order wrt C


42 | P a g e

Results:
The order of the reaction with respect to A is found out to be . While that with respect to
C is ..
Conclustions
Comments

















43 | P a g e

13. CHARACTERIZATION OF GAS-SOLID FLUIDIZATION
Aim:
To study the fluidization of solid particles by gas (air) and to determine the minimum
fluidization velocity of the system.
Equipments:
Chloroform manometer, vertical column, orifice meter, chlorobenzene, manometer, pump
Procedure:
1. Attach an anemometer at the top of gas-solid fluidization column.
2. Start the blower and adjust the valve for constant flow rate.
3. Connect a chloroform manometer across the inlet and the outlet of the fluidization
column.
4. Increase the flow rates in steps of 0.1 m/s.
5. For each value of gas flow rate note down the mean height of the packed bed [(min.ht
+ max.ht. + 2*avg.ht. )/4] and the liquid levels in the two manometric limbs.
6. After attaining the maximum flow rate start decreasing the flow rate and again
measure the mean height of the bed and the fluid levels in the two manometric limbs.
7. Calculate AP/L
8. Plot AP/L vs u.
9. Plot log cl vs log u.

Precautions:
1. On increasing flow rates, care should be taken that decrease of flow rate does not take
place
2. Before taking the height in the manometer, we should wait for the manometer liquid to
stabilize.
3. While fluidization takes place, sometimes the solid gets stuck to the side of column.
Hence we should tap the side of the column lightly to ensure that the all solid particles are
fluidized
4. Care should be taken that the column is vertical.

44 | P a g e


Data:
Diameter of the particle = 0.7661 mm
Density of particle = 1.36 gm/cc
Viscosity of air = 0.185*10
-4
Pa-sec
Density of air at 303
0
k =1.171 kg/m
3
Sphericity of the particle = 1
Density of Cloroform= 1487 kg/m
3

Density of Chlorobenzene = 1107 kg/m
3

Diameter of orifice = 5 mm
Diameter of pipe = 15.2 mm
Inside diameter of column= 3.34 cm
Co = 0.6

Observation table:
1. For increasing flow rate:
Sr. No Manometer
across orifice
Manometer across
bed
Height of bed, cm Mean bed
height, L (cm)
H1, cm H2, cm H3, cm H4, cm Hmin Hmax Havg


2. For decreasing flow rate:
Sr. No Manometer
across orifice
Manometer across
bed
Height of bed, cm Mean bed
height, L (cm)
H1, cm H2, cm H3, cm H4, cm Hmin Hmax Havg






45 | P a g e

FORMULAE:
1. U1A1=U2A2
Where;
U1=velocity of air at the top as recorded by the anemometer
A1=cross-sectional area of the top
U2=velocity at the bed
A2=cross-sectional area of the bed

From, this formula we calculate actual velocity in the column knowing the velocity at the
top.
2.

]
* ) (
max ) / (
[ 1
g
L P
S
mf
mf

c

A
=

This value of
mf
c
is substituted in the Erguns equation and it will result in a quadratic
equation, one of its root is value of minimum fluidization velocity.
3.

L L
mf mf
* ) 1 ( * ) 1 ( c c =

This equation calculates c at any length L after fluidization.

Graphs:
1. The plot of P/L vs u gives two intersecting lines for increasing and decreasing flow
rates. The point of intersection gives Vom and (P/L)max
2. The plot of P vs u gives a increasing trend in P at the beginning and later becomes
constant. Vom projected onto the y-axis gives Pmax
3. The plot of log vs log u gives a straight line and intercept on y-axis gives log(uT)

Sample calculations:
H1 = 25.9 cm, H2= 24.2 cm, H3 = 28.3 cm, H4= 23.2 cm, L = 10.1 cm
i. AH1-2 = H1-H2 = 1.7 cm
ii. AH3-4 = H3-H3 = 5.1 cm

46 | P a g e

iii. APorifice = AH1-2 x A x g =1.7 x 0.01x 1487 x 9.81 = 247.99 N/m
2

iv. APbed = AH3-4 x A x g = 5.1 x 0.01 x (1107-1.514)x 9.81 = 553.09 N/m
2

v. Velocity in orifice = Vorifice = Vom =
A

= 10.92 m/s
vi. Velocity in column = u = Vo x (Aorifice/ Acolumn)= 10.92 x (0.482
2
/3.34
2
)= 0.22 m/s
vii. Calculate (AP/L)bed = (553.09/0.101) = 5476.14 N/m
2

viii. Plot AP/L vs u
ix. Plot AP vs u
From graph,
Find (AP)max = 710 N/m
2
, Lmax = 0.10 m, Vom = 0.325 m/s, (AP/Lmf)max = 6.825 x 10
3
N/m
3


x.
]
* ) (
max ) / (
[ 1
g
L P
S
mf
mf

c

A
=

]
81 . 9 * ) 514 . 1 1360 (
10 x 6.825
[ 1
3

=
mf
c = 0.51
xi
L L
mf mf
* ) 1 ( * ) 1 ( c c =

(1-0.51) x 0.1 = (1-)*L
= 0.51
Calculate , for various values of L

xii. plot log() vs log u
Log (uT)= intercept
This gives us (uT) graphically

xii.
2 2
3
* *
) 1 (
*
* 150
) ( *
P S
mf
mf
S
OM D
g
V u

~
c
c

= 0.591 m/s

47 | P a g e

Theorotically, uT = Vom *8.33 *
3
) 1 (
mf
mf
c
c
= 21.718 m/s
Results:
1. uT = . m/s (theoretically)
1. uT = . m/s (graphically)
3. Vom = .. m/s

Comments:







48 | P a g e

14. CAMPHOR BALL
Aim:
To study the variation of mass transfer coefficient as a function of flow rate of air for the
vaporization of camphor ball in a packed bed.

Apparatus:
Glass column, Rotameter, mini compressor, weighing balance, etc.

Procedure:
1. Weight the camphor balls and pack them in the column.
2. Pass metered air for known time till a measurable difference in the weight of balls is
observed
3. Find the loss in weight of the balls and the flow rate of air.
4. Repeat the experiment for different flow rates for air.
5. Cover the complete range of the rotameter.
6. Verify the proposed equation by plotting log Kg vs log G.
7. Determine the slope and the intercept of this plot and compare it with the proposed
equation.
8. Also indicate the nature of JD Vs NRe curve.
9. Repeat the experiment with different bed height and particle diameter.
10. Indicate the effect of particle size on the mass transfer coefficient.

Data:
1. Diffusivity of camphor ball in air - 0.078 cm
2
/sec
2. Density of air - 1.29 kg/m
3

3. Viscosity of air - 1.31 x 10-5 m
2
/s
4. Molecular weight of Camphor -
5. Vapor pressure of camphor is given by Antoine type
log Ps = 6.845-(1606.529/187.2-t)


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Observation:
Diameter of column =
Diameter of camphor ball =
Number of balls =

Observation table:
Sr.
No.
Loss in weight
(gm)
Time,
sec
Flow rate G Kg JD NRe


Sample calculations:
1. Find the surface ara of the ball
A= [*d*h + 2 (/4 *d
2
)] * no. of balls
2. Find the Kg by using equation
Kg (Ps-Po) = Ws/(Ms*A)
Plot a graph of log Kg vs log G
3. Find out the bed voidage ()
= (total vol. of column - vol. of balls)/(total volume of column)
Find the Reynolds Number
NRe = Dp*v*/
Where,
Dp - diameter of the ball, m = equivalent diameter
v - Superficial mass velocity, kg/s
- Viscosity of air
- Density of the air
Find the JD by the following equation
JD = (0.4548/)*NRe
-0.4069

Plot a graph of JD Vs NRe

Results, Conclusion and comments:

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15. GAS INDUCED IMPELLER
Aim:
i. Measure the critical speed for onset of gas induction at different submergence.
ii. Measure the gas hold-up at different rpm above the critical rpm for different
submergence.
Equipment:
Gas inducing mixer, variable frequency drive, cylindrical container, measuring tape

Procedure:
Instructions to use the variable frequency drive (VFD):
1. Switch ON the power supply to the VFD.
2. Press the GREEN button on the lid of the drive.
3. Open the lid and ensure that the panel is in EXT mode.
4. Press the PU/EXT(white) button, observe the panel to be in PU mode and adjust the
frequency to be supplied to the motor of the mixer. Check the meter reading to be in
its minimum value i.e. 3.
5. Press the RUN (green) button to start the motor. Rotate the knob to adjust the
frequency to get the desired rpm of the motor.
6. Once measurements are performed, reduce the rpm to its minimum value.
7. To pause the motor, press the STOP/RESET (red) button.
8. To stop the motor first press the STOP/RESET (red) button, then the EXT (white)
button and then close the lid and press the red button on the lid before switching
OFF the supply to the drive.
Experimental Procedure:
1. Fill the tank with water till the marked level and ensure that there is no leakage.
2. Adjust the height of the mixer such that the impeller issubmerged in water.
3. Start the VFD and increase the frequency of the VFD till you see the onset of
entrainment of gas in the liquid, which is observed when continuous stream of gas is
seen in the liquid coming out from the impeller casing. The corresponding rpm
(using the calibration chart of the motor or tachometer) of the frequency is the
critical rpm for onset at that submergence.
4. Now increase the frequency of the VFD and note the gas hold-up. Do this for 5-6
different rpm above the critical rpm. Now, pause the VFD.

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5. Increase the submergence of the impellers until maximum submergence so that we
can observe onset at 4-5 different submergences.
6. Repeat instruction 3 and 4 for the different submergences.
7. Note down the following for each submergence:
a. Submergence: _________ cm.
b. Initial liquid height HL: _________ cm.
c. Critical frequency: _________; hence critical rpm NCG: _________.
VFD Reading Total height of
liquid HD(cm)

Calculations:
With the noted readings, calculate the hold-up of the gasfor each submergence.
VFD Reading Motor Speed
(rpm) N
N-NCG %Gas Hold-up
G

% Hold-up of gas G = (HD HL) / HD
N = 57 x VFD reading
Draw graphs to observe the following:
1. NCG vs. Submergence
2. G vs. N
3. G vs. (N-N0)
Conclusion and comments:



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16. COOLING TOWER ANALYSIS
Aim:
For a cooling tower, find:
i. Number of transfer units,
ii. Height of a transfer unit,
iii. Overall gas side mass transfer coefficient.
Apparatus:
Cooling tower, fan, thermometers, Hygrometer, water heater, buckets.


















Fan

Water out
T
L2
, L
Air in
T
G2
, G
2
, %RH-2



Cooling
tower

Air out
TG1, G1, %RH1

Water in
T
L1
, L


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The heat balance over the column gives the operating line is given by

The total sensible heat transfer from liquid bulk to interface = latent heat to vaporize the
liquid + sensible heat change in gas
Height of the column Z = NTU*HTU
Number of transfer units (NTU) =

Height of a transfer unit (HTU) =

GS: Gas flow rate per unit cross-section (kg/m
2
-s)
HY: Enthalpy of air along with water vapour (kJ/kg dry air)
KY: Overall gas side mass transfer coefficient (kg/m
2
-s-H)
H: Humidity (kg water vapour/ kg dry air)
TL: Liquid temperature (K)
HY*: Saturated gas Enthalpy (KJ/kg dry air)

Procedure:
1. Switch on the heater, to heat the inlet water to about 50
o
C, which would take ~20mins.
In the time being plot the equilibrium curve (HY vs. TL).
2. Adjust the liquid flow-rate (keep as small as possible).Measure the flow rate using a
measuring cylinder.
3. Switch on the fan at full speed (regulator).
4. Note down the temperature of inlet water (TL1).
5. Take a mug and collect the water coming down from the column and measure its
temperature (TL2).
6. Find the humidity (%RH1) and temperature (TG1) of the ambient air.
Note: Response time of the hygrometer is 30 sec. Please be patient for the reading.
Dont touch the tip of the hygrometer or blow air into it by mouth and dontallowdirect
water contact.
7. Find the humidity (%RH1) and temperature (TG1) of the outlet air.
8. Vary the fan speed and repeat steps 4-7 at same liquid flow-rate.



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Data:
0= 2501.4 kJ/kg
Cp air = 1.005 kJ/kg-K
Cp water vapour = 1.88 kJ/kg-K

Observations:
Height of the column: _________ cm.
Diameter of column: __________ cm.

Obs.
No.
Fan
speed
Inlet
water
temp.
TL1 (K)
Outlet
water
temp.
TL2 (K)
%RH1 %RH2 Outlet Gas
temp.TG1(K)
Inlet
Gas
temp
TG2(K)
Liquid
Flow-
rate
L (ml/s)


Calculations:
1. From volume flow-rate L (ml/s) calculate mass flow-rate L(ml/s)*1(g/ml); hence
calculate mass flux (kg/m
2
s).
2. Calculate the Gas flow rate per cross-sectional area by energy balance:

3. Plot the equilibrium curve and the operating curve. Divide the range between the inlet
and outlet temperatures into adequate intervals. At each temperature, find the
corresponding enthalpy HY on the operating line and the HY* on the equilibrium curve.
Note: We are evaluating the overall gas side transfer co-efficient, hence the tie-lines are
vertical.
4. Evaluate the integral

. This is the gas-phase enthalpy transfer units(NTU).

5. We know height of the column (Z) so now HTU=Z/NTU
6. HTU=GS/KYa; hence find Kya.

Obs.
No.
TL HY Hy* Hy*-Hy ( Hy*-Hy)
-1
dHy/( Hy*-Hy)





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Graphs:
Plot HY vs. TL (equilibrium line and operating line)

Conclusions and comments:



























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17. CHILLER CHARACTERISTICS

1. Aim: To estimate the coefficient of performance of the chiller
2. Equipment: Chiller, thermocouple, heating coils, clamp meter.
3. Theory:








A chiller removes heat from a liquid viavapour-compression or absorption refrigeration
cycles. Refrigeration is the cooling of a system below the temperature of its surroundings.
The working fluid in a refrigeration cycle is called a refrigerant. The refrigerant used in this
chiller is Freon-22 (chlorodifluoromethane). In refrigeration cycle, the refrigerant is first
compressed reversibly and adiabatically in process 1 2 (compressor), where the work
input per kg of refrigerant is Wc.It is then condensed reversibly in the process 2 3
(condenser) where the heat rejection is Q1, the refrigerant then expands reversibly and
adiabatically in the process 3 4 (throttling device) where the work output is WE, and
finally it absorbs heat Q2 reversibly by evaporation from the surroundings in the process 4
1 (evaporator).
Therefore, C.O.P ref =

Where, Refrigeration effect = (h1-h4)
Compression power = (h2-h1)
( = flow rate of the refrigerant)
x =dryness fraction=



Condenser
Evaporator
Compressor Throttling Device
1
2
3
4

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4. Procedure:
1. Switch on the power supply to the chiller and the heat load.
2. Switch on the MAIN, PUMP and COOL switches on the chiller.
3. Insert the fixed thermocouple inside the first evaporator coil.
4. Adjust the temperature of the evaporator coil using the SET button to 17
o
C.
5. Wait till the displayed temperature of the thermocouple is steady for over 15
minutes (i.e. steady state is reached).
6. Now, measure the following temperatures:
a. Evaporator outlet.
b. Compressor outlet.
c. Condenser outlet.
d. Water temperature.
7. Measure the current in the heaters and evaluate the heat load (assuming power
factor =1).
8. Repeat the steps 4-7 for two or three different set temperatures of the chiller.
9. Once done with experimentation, power off all the switches.
Precautions:
1. Dont put your fingers near the compressor fan.
2. Dont immerse your hand in the water tank.
3. The heater coil should not touch any part of the evaporator coils and the walls of the
tank.
4. Ensure that the heater coil is immersed up to the marked level, and dont remove it
out of the tank during the experiment.
5. Switch ON and OFF the switches carefully; use a wooden stick for your safety.
6. Plot a graph of pressure versus enthalpy for each set point.
5. Data:
Refrigerant: R 22 (Chlorodifluoromethane)
Pc= 49.7 bar
Tc= 369.3 K
= 0.221
Triple point = 233.15 K
Flow rate (manufacturer specification) = 6.93m
3
/hr.

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Density of vapour: 40.7 kg/m
3
.

Formulae:
Peng Robinson EOS:

Assumptions:
i. Saturated vapour leaves the evaporator.
ii. An ideal refrigeration cycle is in operation.
Use the Peng Robinson equation of state to find
i. The saturation pressure at the required temperatures.
ii. Enthalpies of the fluid wherever required.
iii. To calculate the latent heat of vaporisation at the triple point (Hint: Clausius-
Clapeyron equation)

6. Observations and Calculations:
Set Temperature: _____
o
C.
Point Nature of
the fluid
Temperature
(
o
C)
Pressure
(Using EOS)
(bar)
hf
(using EOS)
(kJ/kg)
hg
(using EOS)
(kJ/kg)
Enthalpy
(using EOS)

59 | P a g e

1
2
3
4

C.O.P. = _______
x3= _______
x4= _______

7. Conclusions and comments:




















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18. GAS CHROMATOGRAPHY (GC):
Aim:
To determine concentrations of unknown solvent in a given mixture using gas
chromatograph

Apparatus:
GC unit, 10 ml syringe

Chemicals:
Methanol, ethanol, propanol

Theory:
A Gas Chromatograph is used to detect the components based on the selective affinity of
components towards the adsorbent materials.
A basic chromatography instrument consists of the following:
1. A sample port or injector port for introduction and vaporization of the sample;
2. A separating column, consisting of metal tubing packed with a solid material coated
with a stationary absorbing liquid;
3. A carrier gas, usually N2 or He, to sweep the sample through the column;
4. Flow control equipment to maintain a constant flow of carrier gas through the
column;
5. The detector for measuring the quantity of a separated component;
6. Ovens and heaters for temperature control of the column, detector and injector;
7. An integrator or integrator/strip chart recorder combination to provide permanent
record of the analysis.
The sample is introduced in the liquid/gas form with the help of GC syringe into the
injection port, it gets vaporized at injection port then passes through column with the help
of continuously flowing carrier stream (mobile phase), mainly H2 (for TCD), and gets

61 | P a g e

separated/detected at the detection port with suitable temperature programming. We
visualize this on computer in the form of peaks. Carrier medium can be liquid (e.g. HPLC) or
gas (e.g. GC) for the ease of separation/detection, if it is gas then called gas chromatography
otherwise called liquid chromatography.

Fig: Experimental setup for Gas Chromatograph

Different chemical constituents of the sample travel through the column at different rates
depending upon,
1. Physical properties
2. Chemical properties, and
3. Interaction with a specific column filling (stationary phase).
As the chemicals exit the end of the column, they are detected and identified electronically.
The function of the stationary phase in the column is to separate different components,
causing each one to exit the column at a different time (retention time). Other parameters
that can be used to alter the order or time of retention are the carrier gas flow rate, and the
temperature. Physical Components involve inlet port, Adsorption column, detector port,
flow controller (to control the flow of carrier gas), etc.

Two types of columns are used in GC:
Packed columns are 1.5 - 10 m in length and have an internal diameter of 2 - 4 mm. The
tubing is usually made of stainless steel or glass and contains a packing of finely divided,
inert, solid support material (eg. diatomaceous earth) that is coated with a liquid or solid

62 | P a g e

stationary phase. The nature of the coating material determines what type of materials will
be most strongly adsorbed.
Capillary columns have a very small internal diameter, on the order of a few tenths of
millimeters, and lengths between 25-60 meters are common. The inner column walls are
coated with the active materials (WCOT columns).
Some columns are quasi solid filled with many parallel micro pores (PLOT columns). Most
capillary columns are made of fused silica with a polyimide outer coating. These columns
are flexible, so a very long column can be wound into a small coil.
Temperature dependence of molecular adsorption and of the rate of progression along
the column necessitates a careful control of the column temperature to within a few tenths
of a degree for precise work. Reducing the temperature produces the greatest level of
separation, but can result in very long elution times.
The choice of carrier gas (mobile phase) is important, with hydrogen being the most
efficient and providing the best separation. However, helium has a larger range of flow
rates that are comparable to hydrogen in efficiency, with the added advantage that helium
is non-flammable, and works with a greater number of detectors. Therefore, helium is the
most common carrier gas used.

Detectors
A number of detectors are used in gas chromatography. The most common are the Flame
ionization detector (FID) and the thermal conductivity detector (TCD). While TCDs are
essentially universal and can be used to detect any component other than the carrier gas
(as long as their thermal conductivities are different than that of the carrier gas, at detector
temperature), FIDs are sensitive primarily to hydrocarbons, and are more sensitive to them
than TCD. Both detectors are also quite robust. Since TCD is non-destructive, it can be
operated in-series before an FID (destructive), thus providing complementary detection of
the same eluents

Flame Ionization Detector (FID)
The detector is very sensitive towards organic molecules, but relative insensitive to a few
small molecules e.g. N2, NOx, H2S, CO, CO2, H2O. If proper amounts of hydrogen/airare

63 | P a g e

mixed, the combustion does not afford any ions. If other components are introduced that
contain carbon atoms cations are produced in the effluent stream. The more carbon atoms
are in the molecule, the more fragments are formed and the more sensitive the detector is
for this compound (-- > response factor). However, due to the fact that the sample is burnt
(pyrolysis), this technique is not suitable for preparative GC. In addition, several gases are
usually required to operate a FID: hydrogen, oxygen (compressed air), and carrier gas.

Thermal Conductivity Detector (TCD)
This detector is less sensitive than the FID, but is well suited for preparative applications,
because the sample is not destroyed. It is based on the comparison of two gas streams, one
containing only the carrier gas, the other one the carrier gas and the compound. Naturally,
a carrier gas with a high thermal conductivity e.g. helium or hydrogen is used in order to
maximize the temperature difference (and therefore the difference in resistance) between
two thin tungsten wires. The large surface-to-mass ratio permits a fast equilibration to a
steady state. The temperature difference between the reference cell and the sample cell
filaments is monitored by a Wheatstone bridge circuit.

Electron-capture Detectors (ECD)
Electron-capture detectors (ECD) are highly selective detectors commonly used for
detecting environmental samples as the device selectively detects organic compounds
with moieties such as halogens, peroxides, quinones and nitro groups and gives little to no
response for all other compounds. Therefore, this method is best suited in applications
where traces quantities of chemicals such as pesticides are to be detected and other
chromatographic methods are unfeasible.

Procedure:
Lab assistant will help you in explaining the procedure

Conclusion
Comments