Manaul MassTransferLab II 1617 v.2 1

1 Department of Chemical Engineering Mass Transfer Lab II
Indian Institute of Technology Roorkee Laboratory Manual
AUTUMN 2016
CHN-301 MASS TRANSFER LABII
List of Experiments
Sr. no. Title of the experiment
1. Packed bed distillation

2. Sieve plate distillation
3. Mass Transfer with and without chemical reaction
4 Batch drying
5 Diffusion of air
6. Batch Adsorption
Instructions
Students have to enter in the laboratory in LABORATORY COAT and SHOES. LOOSE
DRESS is not allowed in the laboratory.
An Index sheet will be provided from the lab on the first day of the experiment. Students
have to fill all experiments in sequence according to their turn. The dates of experiment
and report submission, and page numbers will be filled by the TA.
Students should bring a stapled report in A4 sheet (with the original observation data
sheet) of the experiment performed in the last turn.
Students must show a sample calculation for one data set (different for each team
member) and draw graphs manually on graph sheet.
Students should write the observations in the provided data sheets and get it signed by the
TA at the end of the experiment.
There will be a penalty for late submissions (75% and 50% of marks of the experiment
for late by one and two weeks, respectively) and students coming late would not be
permitted to enter in the laboratory.
Evaluation (PRE: 15 marks, PRS: 15 marks)
Report: 30 marks (Students will be continuously and individually graded based on their
contribution in performing experiments and the quality of report)
Oral quiz: 15 marks (Viva will be taken individually or in teams on any date of the
experiment)
1
2 Department of Chemical Engineering Date: _____________
Indian Institute of Technology Roorkee Page no.: __________
Experiment 1: Packed Bed Distillation
1. Objective
To operate the column under total reflux condition and estimate the minimum number of
theoretical stages required using both Fenskes equation and McCabe Thieles graphical
method.
2. Utility and Equipment

1. Packed bed column with reboiler, condenser and storage vessel
2. Test tubes for sampling
3. Electricity Supply: Single Phase, 220 V AC, 50 Hz, 6.5 kW with earth connection.
4. Water Supply. 2 LPM at 5m head.
5. Refractrometer for analysis.
3. Chemicals required
1. Distilled water
2. Methanol
4. Theory
The word distillation refers to the physical separation of a mixture into two or more fractions that
have different boiling points. In this method components of a solution are separated depending
upon distribution of the substances between a gas and a liquid phase, applied to cases where all
components are present in both phases. Distillation differs from absorption and stripping in that
the second fluid phase is usually created by thermal means (vaporization and condensation)
rather than by the introduction of a second phase that may contain an additional component or
components not present in the feed mixture. There are three main methods used in distillation
practice. These are: (a) differential distillation or simple distillation (b) flash or equilibrium
distillation, and (c) rectification.
2
Of these, rectification is much the most important, and it differs from the other two methods in
that part of the vapor is condensed and returned as liquid to the still, whereas, in the other
methods, vapor is either removed completely as such, or is condensed as product.
Continuous rectification or fractionation is a multistage countercurrent distillation operation

where contact of liquid and vapor phases can be achieved in two different ways:
1. Tray towers
2. Packed towers
Tray towers are vertical cylinders in which the liquid and gas are contacted in stepwise fashion
on trays or plates. Trays in the column can be designed as sieve tray, bubble cap tray and valve
trey.
Packed towers on the other hand are vertical columns filled with packing or devices of large
surface. The liquid is distributed over and trickles down through, the packed bed, exposing a
large surface to contact the gas. Packing in the tower may be arranged randomly or stacked in a
proper arrangement. Different types of random packings used in the packed bed ditillation
columns are: 1. Rasching ring, 2. Lessing ring, 3. Partition ring, 4. Berl saddles, 5. Intalox saddle
6. Tellerette, and 7. Pall ring.
The operation in the packed bed column can be analyzed using the operating line equation as for
the rectifying section of the continuous distillation:
(1)
+1 = +
+ 1 + 1
For the binary system:
2 = 1 1 (2a)
2 = 1 1 (2b)
Since the slope of the operating line is R/(R+1), the slope increases as the reflux increases, until
when reflux is infinite. Under total reflux condition the slope is 1. The operating line then
coincides with the 450 line. The numbers of plates are minimum at total reflux. Minimum
number of plates required can be calculated from the terminal concentration of xB and xD based
3
on the relative volatility of the components , which is defined in terms of equilibrium

concentrations:
1 /1 (3)
=
2 /2
Minimum number of theoretical plates required,
log[ (1 )/ (1 )] (4)
= 1

An ideal, mixture follows Raoults law, and the relative volatility is the ratio of vapor pressure.
Thus,
1 = 1 1 (5a)
2 = 2 2 (5b)
1 (5c)
1 =

2 (5d)
2 =

1 /1 1 (6)
= ==
2 /2 2
The final ratio does not change much over the range of temperature encountered in a typical
column, so the relative volatility is taken as constant.
5. Experimental Setup Description
The packed column is comprised of a cylindrical column packed with glass rasching rings. An
electrically heated reboiler is installed at the bottom of the column. The bottom product is
collected in the tank. The vapors formed at the top of the column are condensed using a shell and
tube type condenser by circulating cooling water. A tank with pump and Rotameter is provided
for circulation of cooling water. The condensate is collected in reflux drum and feedback to
column as reflux and part of it is collected as distillate in product receiving tank. The complete
column is insulated for minimizing the heat loss. The experimental setup for the packed bed
distillation column is shown in Figure 1.
4
Figure 1 Experimental setup of the packed bed distillation column.
6. Procedure
1. Fill the water in cooling water tank.
2. Fill the reboiler with Methanol-water solution. The total amount of solution should not be
less than 15 ltrs. The composition of solution should be in range of 15 to 25 % of
methanol by volume.
3. Set a process temperature for the process using the digital temperature controller (DTC).
The temperature range should be in range 85 to 95 C.
4. Start the heaters and cooling water pump.
5. Adjust the cooling water flow rate to a moderate value. Never fully close the bypass
valve.
6. Wait for 25-30 min. for the system to achieve steady state.
7. Now take out the samples from the bottom and distillate stream (by closing the timer for
short while).
8. Cool down the samples to room temperature and measure the refractive indices.
5
7. Observations
= ___________ (for CH3OH-H2O system)
R = ___________
RI of Feed (R.IF) = ___________
RI of Distillate (R.ID) = ___________
RI of Residue (R.IR) = ___________
8. Calculation
(i) From the calibration curve, corresponding mole fractions of CH3OH are:
xF = ____________
xD = ____________
xB = ____________
(ii) Calculation for minimum number of theoretical stages by Fenskes eqn.
(1 )

(1 )
=
ln
(iii) Calculate the minimum number of theoretical stages by using McCabe Thieles graphical
method.
(iv) Calculation for ideal number of theoretical stages with a desired reflux ratio:

Intercept =
+ 1
(v) Plot the equilibrium curve, and the operating line. Draw the stages as described in
McCabe Thieles method.
(vi) Overall efficiency of the packed bed distillation column at the prevailing operating
condition
100
=

6
Table 1 Calibration data for methanol Table 2 Equilibrium data for methanol and
concentration versus refractive index at 25 water system
0
C.
T (C) x y
Methanol Refractive 100 0 0
(vol. %) Index 96.4 0.02 0.134
10 1.3348 93.5 0.04 0.230
20 1.3363 91.2 0.06 0.304
30 1.3387 89.3 0.08 0.365
40 1.3401 87.7 0.10 0.418
50 1.3413 84.4 0.15 0.517
60 1.3417 81.7 0.20 0.579
70 1.3411 78.0 0.30 0.665
80 1.3387 75.3 0.40 0.729
90 1.3309 73.1 0.50 0.779
100 1.3282 71.2 0.60 0.825
69.3 0.70 0.870
67.5 0.80 0.915
66.0 0.90 0.958
65.0 0.95 0.979
64.5 1.00 1.000
1.344
1.340
Refrective index
1.336
1.332
1.328
1.324
0 20 40 60 80 100
Methanol (vol.%)
Figure 2 Calibration curve for refractive index vs composition of a methanol-water system at

ambient conditions.
7
9. Results and Discussions
(i) The minimum number of theoretical stages required using both Fenskes equation and
McCabe Thieles graphical method are _______ and _______, respectively.
(ii) Are the number of theoretical stages estimated using both approaches similar or
different? Give explanation for your findings with proper justification.
10. Nomenclature
T1 bottom temperature of column, 0C

T2 top temperature of column, 0C
T3 vapor temperature, 0C
T4 condensate temperature, 0C
T5 cold water inlet temperature, 0C
T6 cold water outlet temperature, 0C
H Height of packing, m
Relative volatility
Xf mole fraction of product in feed
XD mole fraction of product in distillate
XB mole fraction of product in residue
R reflux ratio
RIF refractive index of feed
RID refractive index of Distillate
RIB refractive index of residue
Nmin minimum number of theoretical stages
11. Precautions and Maintenance Instructions
(i) Heater should not be switched on before filling the feed into reboiler.
(ii) Always drain tanks and reboiler when experiment is over.
(iii) Always use clean water and ensure that there are no foreign particles in the flow streams.
8
12. References
(i) McCabe, WL, Smith, JC, Harriott, P, Unit Operations in Chemical Engineering, 5th
Edition, McGrawHills International Edition, pp. 810837.
(ii) Geankoplis, CJ, Transport Processes and Separation Process Principles, 4th ed.
Introduction to adsorption processes, Ch.12, pp. 760771, 2003.
(iii) Coulson & Richardson, Chemical Engineering Vol. 2, 4th edition, Asian Books Pvt. Lt.,
ND, 1991, Page: 451-454, 427-434.
(iv) Treybal, RE, Mass Transfer Operations, 3rd Edition, pp. 477485, 1981.
9
Experiment2: Sieve Plate Distillation
1. Objective
(i) To operate the column under total reflux condition and estimate the minimum number of
theoretical plates required.
(ii) To obtain T-x data under total reflux at steady state and compare it with theoretical value.
(iii) To estimate the theoritical number of stages at the operating conditions using both Fenske
and McCabe Thieles graphical method.

(i) Sieve plate column with reboiler, condenser and storage vessel
(ii) Test tubes for sampling
(iii) Electricity Supply: Single Phase, 220 V AC, 50 Hz, 6.5 kW with earth connection.
(iv) Water Supply. 2 LPM at 5m head.
(v) Refractrometer for analysis.
3. Distilled water
4. Methanol
4. Theory
The word distillation refers to the physical separation of a mixture into two or more fractions that
have different boiling points. In this method components of a solution are separated depending
upon distribution of the substances between a gas and a liquid phase, applied to cases where all
components are present in both phases. Distillation differs from absorption and stripping in that
the second fluid phase is usually created by thermal means (vaporization and condensation)
rather than by the introduction of a second phase that may contain an additional component or
components not present in the feed mixture. There are three main methods used in distillation
10
practice. These are: (a) differential distillation or simple distillation (b) flash or equilibrium
distillation, and (c) rectification.
Of these, rectification is much the most important, and it differs from the other two methods in
that part of the vapor is condensed and returned as liquid to the still, whereas, in the other
methods, vapor is either removed completely as such, or is condensed as product.
Continuous rectification or fractionation is a multistage countercurrent distillation operation

where contact of liquid and vapor phases can be achieved in two different ways:
3. Tray towers or sieve plates

4. Packed towers
Tray towers are vertical cylinders in which the liquid and gas are contacted in stepwise fashion
on trays or plates. Trays in the column can be designed as sieve tray, bubble cap tray and valve
trey.
Packed towers on the other hand are vertical columns filled with packing or devices of large
surface. The liquid is distributed over and trickles down through, the packed bed, exposing a
large surface to contact the gas. Packing in the tower may be arranged randomly or stacked in a
proper arrangement. Different types of random packings used in the packed bed ditillation
columns are: 1. Rasching ring, 2. Lessing ring, 3. Partition ring, 4. Berl saddles, 5. Intalox saddle
6. Tellerette, and 7. Pall ring.
The operation in the batch still and column can be analyzed using the operating line equation as
for the rectifying section of the continuous distillation:

+1 = + (1)
+ 1 + 1
For the binary system:
2 = 1 1 (2a)
2 = 1 1 (2b)
Since the slope of the operating line is R/(R+1), the slope increases as the reflux increases, until
when reflux is infinite. Under total reflux condition the slope is 1. The operating line then
11
coincides with the 450 line. The numbers of plates are minimum at total reflux. Minimum
number of plates required can be calculated from the terminal concentration of xB and xD based
on the relative volatility of the components , which is defined in terms of equilibrium
concentrations:
1 /1
= (3)
2 /2
Minimum number of theoretical plates required,
log[ (1 )/ (1 )]
= 1 (4)

An ideal, mixture follows Raoults law, and the relative volatility is the ratio of vapor pressure.
Thus,
1 = 1 1 (5a)
2 = 2 2 (5b)
1
1 = (5c)

2
2 = (5d)

1 /1 1
= == (6)
2 /2 2
The final ratio does not change much over the range of temperature encountered in a typical
column, so the relative volatility is taken as constant.
The sieve plate column is comprised of a cylindrical column with seven plates for mounting the
bubble caps. An electrically heated reboiler is installed at the bottom of the column. The bottom
product is collected in the tank. The vapors formed at the top of the column are condensed using
a shell and tube type condenser by circulating cooling water. A tank with pump and Rotameter is
provided for circulation of cooling water. The condensate is collected in reflux drum and
feedback to column as reflux and part of it is collected as distillate in product receiving tank. The
complete column is insulated for minimizing the heat loss. The experimental setup for the
packed bed distillation column is shown in Figure 1.
12
Figure 1 Experimental setup of the sieve plate distillation column.
6. Procedure
1. Fill the water in cooling water tank.
2. Fill the reboiler with Methanol-water solution. The total amount of solution should not be
less than 15 ltrs. The composition of solution should be in range of 15 to 25 % of
methanol by volume.
3. Set a process temperature for the process using the digital temperature controller (DTC).
The temperature range should be in range 85 to 95 C.
4. Start the heaters and cooling water pump.
5. Adjust the cooling water flow rate to a moderate value. Never fully close the bypass
valve.
6. Wait for 25-30 min. for the system to achieve steady state.
7. Now take out the samples from the bottom and distillate stream (by closing the timer for
short while).
8. Cool down the samples to room temperature and measure the refractive indices.
13
7. Observations
NA =7
= ___________ (for CH3OH-H2O system)
R = ___________
RI of Feed (R.IF) = ___________
RI of Distillate (R.ID) = ___________
RI of Residue (R.IR) = ___________
8. Calculations
(i) From the calibration curve, corresponding mole fractions of CH3OH are:
i. xF = ____________
ii. xD = ____________
iii. xB = ____________
(ii) Calculation for minimum number of theoretical stages by Fenskes eqn.
(1 )

(1 )
=
ln
(iii) Calculate the minimum number of theoretical stages by using McCabe Thieles graphical
method.
(iv) Calculation for ideal number of theoretical stages with a desired reflux ratio:

Intercept =
+ 1
(v) Plot the equilibrium curve, and the operating line. Draw the stages as described in
McCabe Thieles method.
(vi) Overall efficiency of the sieve plate distillation column at the prevailing operating
condition
100
=

14
Table 1 Calibration data for methanol Table 2 Equilibrium data for methanol and
concentration versus refractive index at 25 water system
0
C.
T (C) x y
Methanol Refractive 100 0 0
(vol. %) Index 96.4 0.02 0.134
10 1.3348 93.5 0.04 0.230
20 1.3363 91.2 0.06 0.304
30 1.3387 89.3 0.08 0.365
40 1.3401 87.7 0.10 0.418
50 1.3413 84.4 0.15 0.517
60 1.3417 81.7 0.20 0.579
70 1.3411 78.0 0.30 0.665
80 1.3387 75.3 0.40 0.729
90 1.3309 73.1 0.50 0.779
100 1.3282 71.2 0.60 0.825
69.3 0.70 0.870
67.5 0.80 0.915
66.0 0.90 0.958
65.0 0.95 0.979
64.5 1.00 1.000
1.344
1.340
Refrective index
1.336
1.332
1.328
1.324
0 20 40 60 80 100
Methanol (vol.%)
Figure 2 Calibration curve for refractive index vs composition of a methanol-water system at

ambient conditions.
15
16 Department of Chemical Engineering Date: ______________
Indian Institute of Technology Roorkee Page no.:___________
(i) The minimum number of theoretical stages required using both Fenskes equation and
McCabe Thieles graphical method are _______ and _______, respectively.
(ii) Are the number of theoretical stages estimated using both approaches similar or
different? Give explanation for your findings with proper justification.
10. Nomenclature
T1 bottom temperature of column, 0C

T2 top temperature of column, 0C
T3 vapor temperature, 0C
T4 condensate temperature, 0C
T5 cold water inlet temperature, 0C
T6 cold water outlet temperature, 0C
H Height of packing, m
Relative volatility
Xf mole fraction of product in feed
XD mole fraction of product in distillate
XB mole fraction of product in residue
R reflux ratio
RIF refractive index of feed
RID refractive index of Distillate
RIB refractive index of residue
Nmin minimum number of theoretical stages
(iv) Heater should not be switched on before filling the feed into reboiler.
(v) Always drain tanks and reboiler when experiment is over.
(vi) Always use clean water and ensure that there are no foreign particles in the flow streams.
16
Indian Institute of Technology Roorkee Page no.:___________
12. References
(v) McCabe, WL, Smith, JC, Harriott, P, Unit Operations in Chemical Engineering, 5th
(vi) Geankoplis, CJ, Transport Processes and Separation Process Principles, 4th ed.
(vii) Coulson & Richardson, Chemical Engineering Vol. 2, 4th edition, Asian Books Pvt. Lt.,
ND, 1991, Page: 451-454, 427-434.
(viii) Treybal, RE, Mass Transfer Operations, 3rd Edition, pp. 477485, 1981.
17
18 Department of Chemical Engineering Date: _______________
Indian Institute of Technology Roorkee Page no.: ____________
Experiment 3: Mass Transfer with and without Chemical Reaction
1. Objective
To compare the observed enhancement factor for mass transfer with those predicted by the
film theory and boundary layer models.

1. Experimental setup for mass transfer with and without chemical reactions (hot bath,
stirrer)
2. Test tubes for sampling
3. Electricity Supply: Single Phase, 220 V AC, 50 Hz, 6.5 kW with earth connection.
4. Water Supply. 2 LPM at 5m head.
5. Glassware for sample analysis (Conical flask, Measuring cylinder, burette, pipette, etc.).
6. Stopwatch
1. Benzoic acid 500 gm
2. NaOH pellet 10gm
3. N/10 HCl 200 ml
4. N/10 HCl 200 ml
5. Phenolphthalein indicator few drops
4. Theory
Solid liquid mass transfer plays an important role in some industrial operations. The dissolution
may occur with or without chemical reaction. In case dissolution is accompanied by solid liquid
reaction, it is desirable to know the enhancement in the rate of mass transfer due to chemical
reaction. In the present experiment we aim at finding the enhancement in the rate of dissolution
due to simultaneous reaction and compare it with the enhancement predicted on the basis of the
film and boundary layer models.
18
The dissolution of benzoic acid in aq. NaOH solution gives the idea about the enhancement in
the rate of dissolution due to simultaneous reaction and compares it with the enhancement
predicted on the basis of the film and boundary layer models. The dissolution of a solid in a
solution accompanied with instantaneous chemical reaction can be expressed as
A+nB B Product
where A is the solid and B is the liquid phase reactant. Assuming the reaction to be instantaneous
so that A and B dont coexist. The mechanism of solid dissolution involves: dissolution of A in
liquid followed by its reaction with species B diffusion from the bulk liquid phase at a reaction
plane. The reaction scheme for reaction between benzoic acid and sodium hydroxide is shown
below:
Reaction : C6H5COOH + NaOH C6H5COONa + H2O
If the film model is applied to this situation, the enhancement factor, , defined as the ratio of
the solid liquid mass transfer coefficient with reaction, k, to the mass transfer coefficient without
reaction, k ,given by:
[0 ]
() = + (1)
( )
And for boundary layer theory
1 2
3 3 [0 ]
() = + (2)
( )
The set up consists of a reactor, in which solid cylinder of benzoic acid is placed and is stirred by
means of a variable speed mixer. Baffles are also provided. Then reactor is made of S.S.304. a
peltilizer is provided to make the solid cylinder of benzoic acid. Constant temperature water
bath arrangement is provided to conduct the experiment at various temperatures. The
experimental setup described above is shown in Figure 1.
19
Figure 1 Experimental setup for mass transfer with and without chemical reaction.
6. Procedure
(i) Prepare the benzoic acid cylinder using a die.
(ii) Record the dimensions of the benzoic acid cylinder.
(iii) Fill the vessel with aq. NaOH solution of known concentration up to 2/3rd of vessel.
Record the volume of aq. NaOH solution added (V).
(iv) Start the water bath and fix the dissolution temperature, wait till the aq. solution
attains the desired temperature (T).
(v) Now fix the benzoic acid cylinder inside the vessel containing aq. NaOH solution and
start the motor at a fixed rotational speed (N rpm)
(vi) Run the experiment for 10 min.
(vii) Stop the motor and remove benzoic acid cylinder.
(viii) Mix thoroughly the contents of vessel and analyze it for un-reacted NaOH
concentration by titrating against standard HCl solution.
(ix) Measure benzoic acid cylinder dimensions again.
(x) Repeat steps 1 to 9 for different concentrations of aq. NaOH solutions.
20
(xi) Repeat steps 1 to 8 using de-ionised water. This run may be carried for about 45 to 60
minutes duration. During this period small samples (5 ml) should be withdrawn at
regular intervals of 10 minutes and analysed for dissolved benzoic acid by titrating
against 0.02 Kmol/m3 NaOH solution.
7. Observations
7.1 Data
CR* = 3.07 k mole/m3
C* = 0.069 k mole/m3
drod = 0.00842 m
DA = 1.04 10-9 m2/sec
DB = 4.1 X 10-9 m2/sec
nB = 1
7.2 Observations
T = ________ OC
DI = ________ m
Df = ________ m
Li = ________ m
Lf = ________ m
N = ________ rpm
7.3 Observation tables
Table 1 Mass Transfer without Chemical Reaction
S. No. t, min V, ml
21
Table 2 Mass Transfer with Chemical Reaction
S. No. t, min V, ml
8. Calculations
8.1 Mass transfer without chemical reaction

1 1
a. = , k mole/m3 = ______________

b. Estimate the values of (1 CW/C*) and ln(1 CW/C*) at different time
Table 3 Mass Transfer without Chemical Reaction
S. No. t, min CW, k mole/m3

1 1

c. Plot a graph between t and ln[1CW/C*].
d. Slope = ______________
e. Estimate rate constant:
2 2 )
= + 2 ( , 2 = _________ 2
4
+
= , = _________
2
+
= , = _________
2

= , / = _________ /

22
8.2 Mass transfer with chemical reaction

1 1
a. = , k mole/m3 = ______________

b. Estimate the values of (1 CW/C*) and ln(1 CW/CR*) at different time
Table 4 Mass Transfer with Chemical Reaction
S. No. t, min CW, k mole/m3

1 1

c. Plot a graph between t and ln[1CW/CR*].
d. Slope = ______________
e. Estimate rate constant:
2 2 )
= + 2 ( , 2 = _________ 2
4
+
= , = _________
2
+
= , = _________
2

= , / = _________ /

8.3 Estimate the theoretical enhancement factor

= = _________

[0 ]
() = + = _________
( )
1 2
3 3 [0 ]
() = + = _________
( )
23

1. The values for mass transfer enhancement factor estimated using film theory and
boundary layer model, and from experiments are as follows:
= _________
() = _________
() = _________
2. What do you understand from the enhancement factor values obtained in the present
experiment?
10. Nomenclature
Aav = Average surface area of benzoic acid cylinder, m2
B0 = Initial concentration of benzoic acid in liquid, k mol/m3
CW = Concentration of sample, k mole/m3
CR* = Solubility of benzoic acid in water with reaction, k mole/m3
C* = Solubility of benzoic acid in water without reaction, k mole/m3
Di = Initial diameter, m
Df = Final diameter, m
Dav = Average diameter of benzoic acid cylinder, m
drod = Rod diameter, m
DA , DB = Diffusivity, m2/sec
k = Mass transfer coefficient without reaction, m/min
kr = Mass transfer coefficient with reaction, m/min
Lav = Average length of benzoic acid cylinder, m
Li = Initial length, m
Lf = Final length, m
N1 = Concentration of N/10 NaOH used for titration, k mole/m3
24
nB = Number of moles of NaOH taking part in chemical reaction.
t = Time, min
T = Operating temperature, OC
V = Volume of sample taken, m3
V1 = Volume of N/10 NaOH used for titration, m3
exp = Experimental enhancement factor.
theo(f) = Theoretical enhancement factor for film layer
theo(B) = Theoretical enhancement factor for boundary layer
11. Precautions
(i) Measure accurately the volume of water.

(ii) Always use clean water and good quality chemicals and standard solution for
titration.
(iii) Use electronic balance for weighing of chemicals. Dont mix the droppers of
different chemicals.
(iv) Handle the chemicals carefully.
12. References:
(i) Perry, R.H., Chilton, The Chemical Engineers Handbook, 5th ed., McGraw-Hill, NY,
1977, Page 4.38-4.41.
(ii) Octave Levenspiel, Chemical Reaction Engineering, 3rd ed, John wiley & Sons, NY,
1999, Page 384-385, 391.
25
Indian Institute of Technology Roorkee Page no.: ___________
Experiment4: Batch Drying of Solid Material
1. Objective
a. To study the rate of drying of solid material in a batch drier under constant drying
condition and draw drying curve.
b. To determine the critical moisture content in the material.
c. To determine the fraction of total drying time required during constant and falling rate
period.

(i) Heating Chamber with Heater
(ii) Water
(iii) Sample (hard board piece)
(iv) Thermometer, and
(v) Stop Watch
3. Theory
The term 'drying' applies to the transfer of liquid from wet solid into the unsaturated gas
phase. The main external variables involve in drying process are gas flow rate, its temperature
and vapour content in the gas phase. When these variables are kept constant over the entire
drying operation, it is called constant drying conditions. The rate of drying may be determined
for a sample of substance by suspending it in a cabinet duct, in a stream of gas, form a balance.
The weight of drying material may then be measured as a function of time. From the data
obtained, a curve of moisture content as a function of time may be plotted. Rate of drying is
defined as

= (1)

It may also be obtained from the curve either by measuring the slope of the tangents drawn to
the curve or by determining from the curve small changes in moisture content X for
26
corresponding small changes in time , and may plotted as a function of moisture content. There
are usually two major part in the rate of drying curve , a period of constant rate and other that of
falling rate.
If a solid is initially very wet, the surface will be covered with a thin film of liquid, then it is
exposed to relatively dry gas. Evaporation will take place from the surface only and rate is
controlled by diffusion of vapour from surface. Since all the condition remain constant, rate will
be constant during this period. However, since the solid and the liquid surface are usually colder
than the ultimate surface temperature, evaporation rate will be higher during the initial
adjustment period.
Beyond a certain moisture content, i.e. critical moisture content, the drying though is
controlled still by surface evaporation but the available wetted surface become dry. Beyond this
stage drying is controlled by the diffusion of moisture through the solid pores and the rate of
drying fall even more rapidly than before. Ultimately when the liquid content of the solid has
fallen to the equilibrium value for the prevailing gas vapour content drying stops.
The experimental set-up consists of a chamber, a balance at the top of the chamber and an
electric heater below in the chamber. Wet sample(wet hard board piece) is suspended from the
balance in the side chamber. During the experimentation, sample is dried under natural
circulation of hot air from bottom to top through the chamber. A thermometer is placed in the
chamber to measure the drying temperature and the temperature in the chamber is controlled by
varying the heater supply voltage by means of a variac.
5. Procedure
1. Note down the dry weight of the sample by the balance
2. Soak the sample in water so that it become completely wet and wipe out all adhering
water, if any, from the surface.
3. Note down the weight of the wet sample using weight balance.
4. Bring the temperature of the chamber to a steady value, of above 65-75C, and
maintain it throughout the operation through variac attached.
27
5. Suspend the wet sample from the balance in the chamber and note down the time history
of the weight of the sample till the weight become steady.
6. Observations and Calculations

Ls (weight of drying Sample) =
A (Surface Area) =
Sl. no. T (C) Time(t) Weight of Moisture Drying

sample content rate
(gm)
--- --- --- --- --- ---
--- --- --- --- --- ---
--- --- --- --- --- ---

(i) Weight of the sample v/s time is shown in Figure ___ and it can be seen that ______
(ii) Moisture content v/s time is shown in Figure ___ and it can be seen that ______
(iii) Drying rate curve is shown in Figure ___, marked with various zones of drying.
(iv) The critical moisture content is __________.
(v) The fraction of moisture evaporated and the fraction of total drying time required during
constant and falling rate period are ___ and ___, respectively, which suggest that _____.
8. Nomenclature
N rate of drying wt. of the moisture evaporated/(unit time)(unit surface area)

Ls weight of dry sample
time (s)
X moisture content of the sample wt. of the moisture/unit wt. of the dry sample.

(i) Heater should not be switched on before filling the sample into chamber.
(ii) Always use clean water and ensure that there are no foreign particles in it.
28
10. References
1. Treybal, RE, Mass Transfer Operations, 3rd Edition, 1981.
2. Geankoplis, CJ, Transport Processes and Separation Process Principles, 4th ed.
29
Experiment 5: Vapor In Air Diffusion
1. Objective
To study the effect of temperature on the diffusion coefficient.
2. Utilities and Equipment
(i) T-tube for sampling

(ii) Water bath
(iii) Electricity Supply: Single Phase, 220 V AC, 50 Hz, 0.6 kW with earth connection.
(iv) Bench area required: 1.2 m x 0.75 m
(v) Air or vacuum pump
(vi) Digital Temperature Controller
(i) Distilled water

(ii) Carbon tetrachloride (CCl4)
(iii) Organic liquids (Ethanol, Toluene, Acetone, Hexane)
4. Theory
If two gases are inter-diffusing with continual supply of fresh gas and removal of products of
diffusion, this diffusion reaches an equilibrium state with constant concentration gradients. This
is known as steady state diffusion. If there is no flow in either direction at steady state, the rates
of diffusion of A and B, NA and NB are equal but have opposite sign. According to Daltons law,
the total concentration of two components CA and CB is constant.
30

= (1)

Then using the integrated form of the Ficks diffusion equation as follows:

= (1 2 ) = = ( 1 ) (2)
2
where PA1 and PA2 are partial pressures of A at the boundaries of the zone of diffusion and x is
the distance over which diffusion occurs.
In case where gas A is diffusing through stagnant gas B (non-diffusing) the flow carries both
components in proportions to their partial pressure. The total transfer of A is the sum of its
proportion of the flow and the transfer by diffusion

= (3)

= 1 + (4)

2
= (5)
0 1
and
2
= ln (6)
1
This is the expression used for the experimental determination of vapor diffusion coefficients in
gases by evaporation from a liquid surface in a narrow bore tube and measuring the fall of level
of this surface. The distance of the liquid surface below the open end of the tube is measured
before and after evaporation over a definite period. If variation in level is small, then arithmetic
mean of these two readings is taken as the value of x. In case there is appreciable change of
level, the value of x is determined by integration between initial and final readings of level. The
rate of evaporation is thus given by:
2 1
= ln = (7)
1
Integration of these expression yields:
31
2 2
ln( ) = (8)
1 1 0 1
2 22 12 (9)
ln( ) =
1 1 2
Therefore,
1 22 12 (10)
= ( )

ln( 2 ) 2
1
Other form of this equation that is convenient to use is:
( 2 02 ) (11)
= ( )
2 (1 2 )
In terms of concentration the expression for D is:
2 (12)
( 2 02 ) =

1 2 (13)
=

ln 1
2
Usually, x0 will not be measured accurately nor is the effective distance for diffusion x, at time .
Accurate values of (x x0) are available and the equation for diffusion coefficient can be written
as:
(14)
= ( 0 ) +
0 2 0
A graph between /(x - x0) vs (x x0) should yield a straight line with slope
(15)
=
2
(16)
=
2
The total concentration is determined as:
(17)
=

32
Then
(18)
=

CB1 shall be equal to CT and
2 = (19)
Evaluation of vapor pressure of CCl4
The relationship between temperature and vapor pressure is formulated from the graph shown
below in Perrys hand book in the form of a second order polynomial equation.
150
Vapor Pressure
100 y = 0.019x2 - 0.2519x + 7.5239
50
0
0 20 40 60 80 100
Temperature, OC
Figure 1 vapor pressure versus temperature
Vapor Pressure (VP) = 0.019 T2 0.2519 T + 7.5239 (20)

Effect of temperature and pressure on coefficient of diffusion, D is expressed as:
1.5 (21)
=

D can be determined by drawing a curve of P Vs. T
33
5. Experimental Setup
Figure 1 Vapor in air diffusion
The equipment consists of a T tube made of glass, placed in a constant temperature water bath.
Temperature of the bath is controlled by Digital Temperature Controller. Air Pump is used to
supply the air that is allowed to pass through the T tube. Volatile component is filled in the T
tube and air is passed over it by the pump and change in the level is seen by sliding microscope.
6. Procedure
(i) Clean the apparatus and make it free from dust.

(ii) Fill 3/4th of water bath with water.
(iii) Set the water bath temperature at the desired level (up to 50 0C) and wait till the bath
attains the set temperature. Note the steady state temperature of the bath.
(iv) Fill the test-tube with CCl4 up to within two centimeters of the top of capillary leg. Note
down the initial diffusion height of liquid in the capillary.
(v) Make the connection with the air or vacuum pump and allow a gentle current of air to
flow over the capillary.
(vi) Record the height of liquid in the capillary after every 30 minutes.
(vii) Repeat the steps 1 to 5 for different water bath temperatures.
(viii) Use different organic liquids like ethanol, toluene, acetone, hexane etc. and tabulate the
results.
34
7. Observations
Data:
P = ____________ kN/m2
R = ____________ kN-m/k mol- K

L = ____________ kg/m3
MA = ____________ kg/k mol
T = ____________ K
xo = ____________ cm
Observation Table:
S. No. , sec x, cm
8. Calculations
(xo x), cm /(xo x), sec/cm
35
(i) Plot of (xo x) vs. / (xo x) from the graph and find the slope S, sec/cm2
(ii) VP = 0.019 T2 0.2519 T + 7.5239, kN/m2
(iii) CT = P/RT, k mol/m3
(iv) CA = [VP/P] * CT, k mol/m3
(v) CB1 = CT, k mol/m3
(vi) CB2 = CB1 * (1 CA), k mol/m3
(vii) CBM = (CB1 CB2) / ln (CB1/CB2), k mol/m3
(viii) DAB = L CBM / (2 MA CA CT S), m2/s
9. Results and Discussion
The diffusivity of CCl4-water system is _____________ m2/s
10. Nomenclature
CA Molar concentration of A, k mol/m3
CB Molar concentration of B, k mol/m3
CT Total molar concentration, k mol/m3
CBM Log mean concentration of CCl4, k mol/m3
DAB Diffusion coefficient, m2/s
MA Molecular weight of CCl4, kg/k mol
P Total pressure, k N/m2
R Universal gas constant, k N-m/k mol-K
S Slope of graph, sec/cm
T Operating temperature, K
36
VP Vapor pressure of evaporating liquid, k N/m2
x Final height from the top end of the tube after time , cm
xo Initial height from the top end of the tube, cm
xo x Drop in liquid (CCl4) level in time , cm
Time of evaporation, sec
L Density of CCl4, kg/m3
11. Precautions
(i) Carbon tetrachloride (CCl4) should be colorless.

(ii) Dont switch on the heater before filling the water in the bath.
(iii) Microscope focus should be clear, if not adjust that.
12. References
(i) Mccabe, Smith, Unit Operations of Chemical Engineering, 7th edition, McGraw-Hill,
NY, 2005, Page 528, 531-532.
(ii) Binay K. Dutta, Principles of Mass Transfer and Separation Processes, Prentice Hall of
India Pvt Ltd., ND, 2007, Page 11-15.
37
38 Department of Chemical Engineering Date : _____________
Experiment 6: Kinetic Study in Batch Adsorption
1. Objective
To study the adsorption phenomena and to study the batch kinetics for adsorption of Indigo
carmine dye on activated carbon.
2. Utility and Equipments

1. Conical flask: 250 ml (6 numbers)
2. Measuring cylinder: 1000 ml, 100 ml (1 number each)
3. Pipette : 10 ml (2 numbers)
4. Volumetric flask: 1L (1 number)
5. Test tubes (7) and test tube stand
6. Spatula: (1 number)
7. Spectrophotometer with quartz cuvette
8. Weighing balance
9. Shaker
1. Distilled water
2. Dye (Indigo carmine)
3. Activated charcoal
4. Theory
Adsorption is a process that occurs when a gas or liquid solute (the adsorbate) accumulates on
the surface of a solid surface (adsorbent), forming a molecular or atomic film. The term sorption
encompasses both adsorption and absorption processes, while desorption is the reverse process.
Adsorption is operative in most natural physical, biological and chemical systems and is widely
used in water purification.
38
Adsorption is a consequence of surface energy. In a bulk material all the bonding requirements
such as activated charcoal, synthetic resins and water purification. The different types of
adsorption processes are as follows:
1. Physi-sorption or physical adsorption is a type of adsorption in which the adsorbate

adheres to the surface only through Vander Waals (weak intermolecular) interactions,
which are also responsible for the non-ideal behavior of real gases.
2. Chemi-sorption is a type of adsorption whereby a molecule adheres to a surface through
the formation of a chemical bond, as opposed to the Vander Waals forces, which causes
physi-sorption.
4.1 Batch Kinetic study
Two kinetic models, viz. pseudo-first-order and pseudo-second-order are widely used to
investigate the adsorption process of Indigo carmine dye onto activated carbon.
Pseudo-first-order model: In the logarithmic form the kinetic equation can be expressed as:

10 =
2.303
(1)
This equation is known as Lagergren equation.
Pseudo-second-order model: This model can be represented as
1 1
= +
2 2
(2)
where qe and qt are adsorption capacity at equilibrium and at time t respectively in mg of
adsorbate per g of adsorbent respectively.
In practice, activated carbon is used as an adsorbent for the adsorption of mainly organic
compounds along with some larger molecular weight inorganic compounds such as iodine and
mercury.
39
Activated carbon also called activated charcoal or activated coal is a general term that includes
carbon material mostly derived from charcoal. For all three variations of the name activated is
sometimes substituted by active. It is a material with an exceptionally high surface area. Just
one gram of activated carbon has a surface approximately 500 m2. The three main physical
carbon types are granular, powder and extruded (pellet). All three types of activated carbons can
give properties tailored to the application. Activated carbon is frequently used in number of
applications such as food production, medicine, pharmacy, military, etc, in pharmacy activated
charcoal is considered to be the most effective single agent available as an emergency
decontaminating gastrointestinal tract, it is used after a person swallows or absorbs almost any
toxic drug or chemical.
5. Procedure
1. Prepare a stock solution of dye containing 1000 ppm (or mg/L). To prepare the solution
dissolve 1 gm dye in one liter of water. Use 1 L volumetric flask.
2. Take 5 ml from stock solution and mix it with water to make 500 ml of solution (100
mg/L). Use 250 ml volumetric flask.
3. Take 350 ml from 100 g/L solution and add water to make it 700 ml solution (i.e. 50
mg/L).
4. Take 100 ml sample of 10 mg/L in 250 ml flask and add 2 g/100ml of activated carbon to
each.
5. Place the series of samples in a shaker at temperature 30 oC which is rotating at 263 rpm.
6. Take absorbance readings at 608 nm, using UV spectrophotometer, of samples at definite
times. Before checking the absorbance of a given solution mixture, filter the solution.
6. Observations
50 /
= 2
1
where A1 is the absorbance of 50 mg/L solution and A2 is the absorbance of sample at different
time interval.
40
Table1: Concentration of Dye before and after adsorption

Time (min) Concentration of Dye in the Concentration of Dye in the
Distilled water (mg/L); Co =10 Distilled water (mg/L); Co = 50
Absorbance Concentration Absorbance Concentration
0
10
20
30
60
90
7. Calculations
1. Determine mg of dye adsorbed per gram of adsorbent (m) according to the following
equation:
( )
=
1000
where, Co is concentration of dye before adsorption (mg/L), C is concentration of dye at
time t (min) during adsorption (mg/L), g is adsorbent dosing to the flask (g/l), V is
volume of dye solution taken in the flask (ml), q is adsorption capacity or adsorbent
loading (mg of solute adsorbed/g of adsorbent).
2. Calculate q for each sample and with the help of graph between q (mg/g) vs time and C
(mg/L) vs time for a particular sample (for example 20 mg/L) calculate equilibrium
values of qe and Ce.
3. Fit the experimental data to the specified kinetic adsorption models.
4. Report the best fit with the help of regression coefficient (R2) value.
5. Report the kinetic model constants.
6. Calculate adsorption capacity (q) at different time:
Table 2: Calculation of adsorption Capacity (q)

S.No Time (min) Conc.(mg/L) q (mg/g)
1 0
2 10
3 20
4 30
5 60
6 90
41
7. Calculate equilibrium values of Ce and qe obtained from Table 2 for respective samples
for Co value.
(Note: If water is getting black during the mixing with charcoal then subtract the absorbance of
charcoal from the absorbance of the respective die solution to have the actual absorbance of die
in the charcoal)

(i) The best fit kinetic model has been found as model. Kinetic constants of
models are found as ________ at _____ oC and ________ rpm.
9. Precaution
(i) Filter the sample before taking readings in spectrophotometer

(ii) The adsorbent should be oven dried.
(iii) Filter the solution before checking the absorbance of a given solution mixture.
10. References
(i) McCabe, WL, Smith, JC, Harriott, P, Unit Operations in Chemical Engineering, 5th
(ii) Geankoplis, CJ, Transport Processes and Separation Process Principles, 4th ed.
Introduction to adsorption processes, Ch.12, pp. 760-771, 2003.
(iii) Seader, JD, Henley, EJ, Separation Process Principles, dsorption, Ion Exchange,
Chromatography, Ch 15, pp. 778789, 794806, 820824, 1998.
42

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1 Department of Chemical Engineering Mass Transfer Lab II

Indian Institute of Technology Roorkee Laboratory Manual

CHN-301 MASS TRANSFER LABII

Sr. no. Title of the experiment

1. Packed bed distillation

Evaluation (PRE: 15 marks, PRS: 15 marks)

Experiment 1: Packed Bed Distillation

2. Utility and Equipment

Continuous rectification or fractionation is a multistage countercurrent distillation operation

on the relative volatility of the components , which is defined in terms of equilibrium

5. Experimental Setup Description

Figure 1 Experimental setup of the packed bed distillation column.

= ___________ (for CH3OH-H2O system)

RI of Feed (R.IF) = ___________

RI of Distillate (R.ID) = ___________

RI of Residue (R.IR) = ___________

Figure 2 Calibration curve for refractive index vs composition of a methanol-water system at

9. Results and Discussions

T1 bottom temperature of column, 0C

11. Precautions and Maintenance Instructions

Experiment2: Sieve Plate Distillation

2. Utility and Equipment

Continuous rectification or fractionation is a multistage countercurrent distillation operation

3. Tray towers or sieve plates

5. Experimental Setup Description

Figure 1 Experimental setup of the sieve plate distillation column.

= ___________ (for CH3OH-H2O system)

RI of Feed (R.IF) = ___________

RI of Distillate (R.ID) = ___________

RI of Residue (R.IR) = ___________

Figure 2 Calibration curve for refractive index vs composition of a methanol-water system at

9. Results and Discussions

T1 bottom temperature of column, 0C

11. Precautions and Maintenance Instructions

Experiment 3: Mass Transfer with and without Chemical Reaction

2. Utility and Equipment

Reaction : C6H5COOH + NaOH C6H5COONa + H2O

5. Experimental Setup Description

DA = 1.04 10-9 m2/sec

DB = 4.1 X 10-9 m2/sec

7.3 Observation tables

Table 1 Mass Transfer without Chemical Reaction

Table 2 Mass Transfer with Chemical Reaction

8.1 Mass transfer without chemical reaction

b. Estimate the values of (1 CW/C*) and ln(1 CW/C*) at different time

Table 3 Mass Transfer without Chemical Reaction

S. No. t, min CW, k mole/m3

c. Plot a graph between t and ln[1CW/C*].

e. Estimate rate constant:

8.2 Mass transfer with chemical reaction

b. Estimate the values of (1 CW/C*) and ln(1 CW/CR*) at different time

Table 4 Mass Transfer with Chemical Reaction

S. No. t, min CW, k mole/m3

c. Plot a graph between t and ln[1CW/CR*].

e. Estimate rate constant:

8.3 Estimate the theoretical enhancement factor

9. Results and Discussions

Aav = Average surface area of benzoic acid cylinder, m2

B0 = Initial concentration of benzoic acid in liquid, k mol/m3

CW = Concentration of sample, k mole/m3

CR* = Solubility of benzoic acid in water with reaction, k mole/m3

C* = Solubility of benzoic acid in water without reaction, k mole/m3

Dav = Average diameter of benzoic acid cylinder, m

drod = Rod diameter, m

b. Estimate the values of (1 CW/C) and ln(1 CW/C) at different time

b. Estimate the values of (1 CW/C) and ln(1 CW/CR) at different time