Experiment No: 1

VAPOR LIQUID EQUILIBRIA

Aim:
To determine the vapor-liquid equilibrium curve for the ethanol-water mixture and
compare it with the VLE data.

Introduction:
Several chemical engineering processes which have mass transfer operations
taking place between different phases. The desired outcome is usually a change
in composition and hence the composition of a phase is the key parameter of
interest.

An equilibrium is said to be established in a system when no changes occur to the

macroscopic properties of a system with time. This implies a balance of all the
potentials which can cause a change. An isolated system of liquid and vapor will
initially show some changes in composition; this is because some molecules in a
phase will have sufficiently high velocities near the interface to enter the other
phase. Eventually both these fluxes will become equal and equilibrium will be
established.

Theory:

In this experiment, we consider liquid vapor system with two components. From
the Equilibrium Phase rule, the equilibrium state will be completely determined
when two independent variables are fixed. Hence at any given temperature and
pressure, the compositions of the components in the two phases will be fixed.
Examples of equilibrium curves for such a system are shown in Figure 1. The
curves shown are plotted at a constant pressure at different temperatures 𝑡 and
compositions of component 1 in the liquid and vapor phase as 𝑥𝑖 and 𝑦𝑖
respectively. The upper line in each represents the saturated vapor line also called
the bubble line and the lower line represents the saturated liquid line also called
the dew line.

Figure 2 shows the variation of 𝑦𝑖 with 𝑥𝑖 when one of the values is fixed at a
constant pressure. This xy behavior is theoretically modelled by laws such as
Raoult’s Law and Henry’s law.

-1-
Figure SEQ Figure \* ARABIC 1: txy diagrams at 1 atm: (a)
tetrahydrofuran(1)/carbon tetrachloride(2); (b) chloroform(1)/tetrahydrofuran(2); (c)
furan(1)/carbon tetrachloride(2); (d) ethanol(1)/ toluene(2) [1]

-2-
 Figure SEQ Figure \* ARABIC 2: xy diagrams at 1 atm: (a) (a)
tetrahydrofuran(1)/carbon tetrachloride(2); (b) chloroform(1)/tetrahydrofuran(2);
(c) furan(1)/carbon tetrachloride(2); (d) ethanol(1)/ toluene(2) [1]

Models:
Raoult’s Law:
This law states that the partial pressure (P1) of a component in the vapor phase is
equal to the vapor pressure (P1,vap) times the mole fraction (x1) of the component
in the liquid phase. That is,
𝑃1 = 𝑃1,𝑣𝑎𝑝 𝑥1
Using this with the Dalton’s Law of partial pressure yields

𝑦1 𝑃𝑡 = 𝑃1,𝑣𝑎𝑝 𝑥1

Where 𝑃𝑡 is the total pressure in the vapor phase.

Hence this gives a linear relationship between the two compositions at equilibrium.

-3-
Henry’s Law:
Henry’s law states that –
𝑃1 = 𝑥1 𝐻

Where H is Henry's constant.

With the Dalton’s Law, this gives-
𝑦1 𝑃𝑡 = 𝑥1 𝐻

Experimental Setup:

● The apparatus consists of a round bottom flask with three way open at the
top and opened at the bottom.
● A heating mantle of 1 liter capacity is provided to heat the reboiler
● A vapor rising and reflux and reflux tube with condensate and sampling is
connected to the reboiler
● A spiral glass tube condenser is provided to condense the vapor
● A overhead tank is provided to circulate condenser cooling water
● Two thermocouples are provided to measure the liquid and vapor
temperatures.

Figure SEQ Figure \* ARABIC 3: Schematic

-4-
Requirements:
● Ethanol
● Water
● Digital Refractometer

Experimental Procedure:
1. Preparation of Calibration Chart :-
● Measure 10 mole % of Water and 90 mole % of Ethanol and mix the
contents well. Find the refractive index of the mixture.
● Now prepare a mixture of 30 mole % of Water and 70 mole % of Ethanol
and find the refractive index.
● Thus change the concentration of mixture and estimate the refractive index
for various concentrations and tabulate them in Table No. 1
● The calibration chart once prepared can be used repeatedly.
2. Prepare a mixture of Water and Ethanol containing a 50 mole % of ethanol
with a volume of approximately 500 ml and feed it to the vapor liquid
equilibrium apparatus.
3. Heat the mixture gently to distill it. Recycle the vapor for at least half an hour
before any samples are taken, to allow equilibrium between liquid and vapor
phases to be obtained.
4. Then the liquid and vapor samples are taken at noted temperatures and
cooled to room temperature and their refractive index is found.
5. Add 100 ml of Water to the VLE apparatus and again allow equilibrium to
be attained (indicated by constant temperature) before the next set of
samples are taken.
6. Find the refractive index of the samples.
7. Tabulate them in table No. 2

Procedure to use the Refractometer:

1. Calibrate the refractometer by filling its sample well with a few drops of
distilled water and then pressing the zero button.
2. Now take a sample in a dropper and put 1-2 drops on the sample well of the
refractometer.
3. Close the cover of the sample well.
4. Now press the read button to get the reading of the refractive index.

-5-
Precautions:
● Close the mixture inlet valve before switching on the heater.
● Clean the sample well of the digital refractometer with dry tissue paper to
remove dust particles.

Observations:
Table No: 01. Calibration Chart.

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

Table No. 2

S. No. Vapor Temperature Refractive Index

Vapor sample Liquid sample
(°C)

Table No. 3

-6-
 S. No. Refractive Index Mole fraction of Ethanol
Vapor Liquid Vapor Liquid

Table No.4

S. No. Temperature yc xc
T (oC)

Results:
Draw the graph for y1 vs x1 for experiment and compare with the original data from
literature.

Sources of errors:
Report the possible sources of error found in the experiment and the
observations. Discuss exactly how these affect the experimental data (i.e. will
the readings be larger or will they be smaller due to the presence of a particular
source).

Discussions:

-7-
The following topics need to be discussed in detail in the report.

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

2. Give a physical interpretation of your results.
3. Compare your results with those obtained from theory/literature. Justify
the differences in these, if any.
4. What is the Equilibrium Phase rule? What are the free and the dependent
variables in this experiment?
5. Define bubble point and dew point.
6. Describe in brief how the interactions between the components affect the
vapor liquid equilibrium.
7. Is it always possible to obtain a pure component using a distillation
process? Why/why not?

References:
J M Smith, H C Van Ness and M M Abbott, Introduction to Chemical Engineering
Thermodynamics, 7th Edition Tata McGraw Hill, pp. 276-317,

-8-
 Experiment No – 2
MASS TRANSFER
WITH AND WITHOUT CHEMICAL REACTION
(Solid – liquid system)
Aim:
1. To study the dissolution of benzoic acid in aq. NaOH solution
2. To calculate the enhancement factor comparing Mass Transfer Coefficient of with
and without chemical reaction dissolution.

Introduction:
The dissolution of a solid into a liquid is governed by Molecular Diffusion. But given that,
the Molecular Diffusion is a slow phenomenon, the rate of dissolution is increased by the
support of Bulk Mass Transfer in industrial applications.
Mass Transfer further depends upon the interactions of solid and liquid reactants and
can be stratified as with and without chemical reaction Mass Transfer. These interactions
can be elaborated by the Film Theory and the Boundary Layer Theory.

Theory:
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, B is the liquid phase reactant and nB is the stoichiometric coefficient
of B for the reaction. Assuming the reaction to be instantaneous so that A and B don’t
coexist. The mechanism of solid dissolution involves dissolution of A in the liquid followed
by its reaction with the species B at the reaction plane. B exists in the region from the
reaction plane to the bulk while A exists from the solid phase to the reaction plane. A
diffuses from solid phase to the reaction plane and B diffuses from the bulk liquid phase
to the reaction plane.
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 kr to the mass transfer coefficient
without reaction k, is given by
k r DA DB [ Bo ]
 film = = +
k DB D A n B [ A*] (1)
where [A*] is the (saturation) concentration of A at the solid-liquid interphase, [B0] is the
bulk concentration of B.
And for boundary layer model it is
1 2
k D  3
D  3
[ Bo ]
b = r =  A  +  B 
k  DB   DA  n B [ A*] (2)

Experimental Setup:

Setup Diagram
The apparatus consists of a reactor tank. The solvent in the form of a cylinder is dissolved
in the solvent present in the reactor with the help of a rotating rod. A water bath has been
provided with a stirrer and a heat source for maintaining the temperature of the reactor.

Materials Required:
1. Benzoic Acid
2. NaOH solution
3. Indicators (Phenolphthalein and Methyl Orange)
4. HCl

Experimental Procedure:
 1. Weigh the cylindrical steel rod, Wi.
2. Measure the dimensions of the steel rod.
3. Put the rod in the center of the die set and fill up Benzoic Acid till the top.
4. Close the die set and compress the cake.
5. Remove the cake and weigh it, Wf.
6. Prepare the benzoic acid cylinder first by using the dye set provided.
7. Measure the dimensions of the cake.
8. Fill the vessel with a known concentration de-ionized water and measure the
volume of deionized added (V).
9. Start the heater of the water bath and fix the dissolution temperature. Else conduct
the experiment at room temperature and measure the temperature.
10. Fix the Benzoic acid cake in the vessel containing deionized water and start the
motor and fix the rotational speed, (N, rpm).
11. Run the experiment for a known time interval of say 10 – 15 min.
12. Stop the motor and remove the benzoic acid cake.
13. Mix thoroughly the contents of the vessel and analyze it for dissolved Benzoic Acid
concentration by titrating against standard NaOH solution (use Phenolphthalein
indicator).
14. Repeat the steps for different concentrations of aqueous Benzoic Acid solution.
15. Repeat steps 1–14 using a known concentration aqueous NaOH solution in the
reactor. Analyze the samples for unreacted NaOH concentration by titrating
against standard HCl solution (use Methyl Orange indicator).

Precautions:
1. Fix the rod inside the die vertically to avoid deformation of Benzoic Acid
cylinder.

2. Wash the burettes and beakers before starting the experiment.

3. Assure proper mixing of samples before titration.

4. Speed of the stirrer should not be too high and must be equal for both the
parts.
Observations:
● For Mass Transfer without reaction
Temperature, T =
Speed of motor, rpm =
Diameter of Cake, Dav =
Length of Cake, Lav =
Diameter of rod, dr =
Length of rod, Lg =
Area of the cake, Aav =
Volume of water in the reactor, V =
Volume of sample taken for titration =

Concentration of NaOH (N2) =

Indicator =

S.No Time t, min Volume of Standard NaOH Concentration of Benzoic Acid

. used (V2), ml

● For Mass Transfer with reaction

Temperature, T =
Speed of motor, rpm =
Diameter of Cake, D´av =
Length of Cake, L´av =
Diameter of rod, d´r =
Length of rod, L´g ´ =
Area of the cake, A´av =
Volume of NaOH in the reactor, V´ =
Volume of sample taken for titration =

Concentration of HCl (N'2) =

 Initial Concentration of NaOH =
Indicator =

S.No Time t, min Volume of Standard HCl used Concentration of NaOH

. (V´2), ml

Calculations:
   
( )
Aav = Dav Lav + 2   Dav2 − d r2 
Average surface area =  4  

Ap = Dav Lav

For the dissolution without reaction, measure the benzoic acid concentration in
liquid at different times and the mass balance gives the following relation for
change in benzoic acid concentration with time.
 C 
t = − ln 1 −   
Aav
k
V   C * 
where, C* is the saturation concentration of Benzoic Acid in water at given temperature,
V is volume of the liquid and k is mass transfer coefficient without reaction.

Plot t vs ln[1-C/C*] and regress the data linearly. The slope of the regression line is
kAav
slope =
V
Mass transfer coefficient without reaction can be obtained from the value of the slope
and the known values of the volume of the liquid and the Aav.

Reaction
 C6H5COOH + NaOH → C6H5COONa + H2O
Formula Used:
C −O
R '= V'
T
where,
C = initial concentration of NaOH in the feed tank
O = Concentration of NaOH at time T.

R'
R=
Specific rate of dissolution Aav' (kmol/m2s)

The experimental value of the enhancement factor can then be calculated as given below:
R
exp =
kC *

where R is the specific rate of dissolution with reaction.

Result:
1. The value of the observed enhancement factor is …..
2. Compare the enhancement factor for mass transfer predicted by the film and
boundary layer models to the observed enhancement factor.

Discussion:
1. The effect of temperature on mass transfer coefficient.
2. Any five Industrial applications of dissolution reaction.
3. Additional inferences from the experiment.
4. Other methods used to measure concentration of solutions.

References:
1. Treybal, R.E, “Mass-Transfer Operations”, 3rd ed., McGraw-Hill, NY, 1981, Page
623-625, 632-636, 639-640.
2. Binay K. Dutta, “Principles of Mass Transfer and Separation Processes”, Prentice
Hall of India Pvt Ltd., ND, 2007, Page 630-636
3. Octave Levenspeil, “Chemical Reaction Engineering”, 3 rd ed., John Willey & Sons,
NY, 1999, Page 376-390
 Experiment No- 3
ADSORPTION IN PACKED BED
Aim:
To study Adsorption in a packed bed for a Solid-Liquid system and to find the
breakthrough curve and the length of unused bed.

Introduction:
Adsorption is a well-known mass transfer operation for solid-fluid contacting. A large
number of adsorption operations are present in chemical industries. The main purpose
of using adsorption operation in industry is to alter the concentration of mixtures and
solutions. It can be operated either with or without chemical reaction. For example,
Fuller’s Earth is used in leaching operation in vegetable oil manufacturing.

In adsorption, the molecules distribute themselves between two phases, one of which
is a solid the other can be liquid or gas. Adsorption suffers one drawback that the
capacity of the adsorbent for the adsorbate in question is limited. At intervals, the
adsorbent has to be removed from the process and regenerated, that is, restored to
its original condition.

Theory:
Adsorption is the selective transfer of a solute from a fluid phase to a batch of rigid
particles. The usual selectivity of an adsorbent between solute and carrier fluid or
between different solutes makes it possible to separate certain solutes from the carrier
or from one another.

It occurs when molecules diffusing in the fluid phase are held for a period of time by
attractive forces due to the adsorbent surface. The surface represents a gross
discontinuity in the structure of solid, and atoms at the surface have a residue of
molecular forces which are not satisfied by surrounding atoms like those in the body
of the structure. These residual or Vander Waal’s forces are common to all surfaces
and the only reason that certain solids are designated “adsorbents” is that they can be
manufactured in a highly porous form, giving rise to a large internal surface.

The Adsorption wave

Consider a binary solution, containing a strongly adsorbed solute at concentration C 0.

The fluid is to be passed continuously upward through a relatively deep bed of
adsorbent initially free of adsorbate. The lowermost layer of solid, in contact with the
strong solution entering, at first adsorbs solute rapidly and effectively, and what little
solute is left in the solution is substantially all removed by the layers of solid in the
upper part of the bed. The effluent from top of the bed is practically solute free, as at
Ca in the upper part of the adjacent figure.
 Figure 1: Adsorption wave

The distribution of adsorbate in the solid bed is indicated in the sketch in the lower part
of this figure at a, where the relative density of the horizontal lines in the bed is meant
to indicate the relative concentration of adsorbate. The lowermost layer of the bed is
practically saturated, and the bulk of the adsorption takes place over a relative narrow
adsorption zone called the mass transfer zone (MTZ). As solution continues to flow,
the adsorption zone moves upward as a wave, at a rate ordinarily very much slower
than the linear velocity of the fluid flowing through the bed. At a later time, as at b in
the figure, roughly half the bed is saturated with solute, but the effluent concentration
Cb is still substantially zero. At c in the figure the upper portion of the adsorption zone
has just reached the top of the bed, and the concentration of solute in the effluent has
suddenly risen to an appreciable value Cc for the first time. At this point of time, the
MTZ has ‘broken through’ the length of the bed and hence the concentration of the
solute in the effluent rises. This point is called the Breakpoint. The solute concentration
in the effluent now rises rapidly as the adsorption zone passes through the top of the
bed and at d has substantially reached the initial value Co. The portion of the effluent
concentration curve between positions c and d is termed the Breakthrough curve. If
the solution continues to flow, little additional adsorption takes place since the bed is
for all practical purposes entirely in equilibrium with the feed solution.
Length of Unused Bed Calculation
The Length of Unused Bed (LUB) is given by the length of the mass transfer zone.
The LUB allows us to scale-up the breakthrough curve’s data based on laboratory
columns for the same particle size and velocity.
Consider figure 2. If the mass transfer rate were infinitely rapid, the Breakthrough
curve would be the vertical line at θs, which can be located so that the shaded areas
are equal. The adsorption zone of the figure can then be idealized as reduced to a
plane, with the length of bed Zs upstream of the plane at concentration Yt and the
length Z-Zs downstream equal to the length of unused bed (LUB). At Breakthrough,
the length of the bed is taken to be the sum of LUB and the length saturated with solute
in equilibrium with the feed stream.

Figure 2: Breakthrough Curve (Ref. to Treybal, Mass Transfer Operation)

If V=velocity of advancement of the “adsorption plane”, then at breakthrough

𝑍𝐵 = 𝑉𝜃𝐵
Also 𝑍 = 𝑉𝜃𝑆
Therefore 𝐿𝑈𝐵 = 𝑍 − 𝑍𝑠 = 𝑉𝜃𝑆 − 𝑉𝜃𝐵 = 𝑍(𝜃𝑆 − 𝜃𝐵 )/𝜃𝑆

θB = Time when the colour of product starts changing rapidly

θS = Time required for idealized breakthrough
Experimental Setup:
The apparatus is provided for the process of adsorption in packed columns with solid
phase being static & fluid phase is flowing. For flow of fluid a pump & rotameter is
provided. Three borosilicate columns are provided having different diameters &
lengths. At the inlet of the column, valves are provided to feed only one column at a
time. Valves are provided at the bottom of columns & liquid tanks to drain out after
running the apparatus. Filters are provided before the column drain valves to prevent
the charcoal from draining.

Figure 3: Setup diagram

Requirements:

1. Electricity supply: Single phase, 220 V, 50 Hz, 5-15 Amp socket with earth
connection
2. Water supply
3. Colorimeter or Spectrophotometer
4. Chemical required: KMnO4
5. Test tubes, Measuring cylinders
Experimental Procedure:

1. Check that all the valves are properly closed.

2. Calibrate the rotameter.
3. Check that activated charcoal is filled in all the columns.
4. Prepare 20 litre solution of KMnO4 in water.
5. The coloured KMnO4 solution should not be too concentrated.
6. Fill the coloured solution in the feed tank (upper tank).
7. Open the valve of the column to be operated.
8. Start the pump and fix a minimum flow rate using rotameter.
9. Take the samples of the output from the column after fixed time intervals.
10. Take water as the reference sample in the colorimeter.
11. Now measure the optical density of different samples with respect to the
reference sample.
12. Prepare a calibration curve of different concentrations and their respective
optical densities.
13. Find the concentration of colour in the liquid from the prepared calibration
curve.
14. Note down the flow rate, time and concentration.
15. Run the experiment till the change in colour output liquid becomes almost
stable
16. Stop the pump and close the valve of the column.
17. Repeat the experiment for the second and third column.

Precautions:

1. Before starting the pump, ensure that the bypass valve is fully closed &
Rotameter is properly closed.
2. Before starting the apparatus check whether the drain valve of all the columns
is properly closed.
3. Make sure that there is no leakage from the bottom of the column.
4. Only one feed valve must be open at a time.
5. The apparatus should be drained off as soon as possible as the color of liquid
would clot over the inner surfaces of the apparatus, making the apparatus yield
incorrect results.

Observations:

Height of column1 (Z1) = 1m

Height of column 2 (Z2) = 0.5m
Height of column 3 (Z3) = 0.3m
Flow rate (F) = ------ LPH

Prepare a calibration curve of the different concentrations of solute and their

respective optical densities as figure 4. Measure the optical density 𝐼𝜃 of solution at
the outlet at different times 𝜃 and find the concentration 𝐶𝜃 from the calibration chart
for the three columns.

Calibration Table:

Concentration Optical Density

Observation Table:
Time (θ) Optical Density (Iθ) Concentration (Cθ)

Plot a curve between θ & Cθ and find 𝜃𝑆 and 𝜃𝐵

Calculations:
 B + T
S =
2

  
Z 1 − B 
Length of unused bed =   S 

Results:
Plot the breakthrough curve for the three packed bed columns. From these find 𝜃𝑆
and 𝜃𝐵 and find the length of the unused bed in all the cases.
Sources of errors:
Report the possible sources of error found in the experiment and the observations.
Discuss exactly how these affect the experimental data (i.e. will the readings be
larger or will they be smaller due to the presence of a particular source).

Discussion:
The following topics need to be discussed in detail in the report.
1. What is the conclusion of the experiment? Is the objective fulfilled?
2. Give a physical interpretation of your results.
3. Compare your results with those obtained from theory/literature. Justify the
differences in these, if any.
4. Provide any additional suitable inference.
5. What is the mechanism or steps for adsorption to occur? Compare the rate
constants of these steps to the superficial velocity and describe how the velocity
of the propagation of adsorption-plane depends on these.

References:
1. Treybal, R.E, “Mass-Transfer Operations”, 3rd ed., McGraw-Hill, NY, 1981,
Page 623-625, 632-636, 639-640.
2. Binay K. Dutta, “Principles of Mass Transfer and Separation Processes”,
Prentice Hall of India Pvt Ltd., ND, 2007, Page 630-636
 Experiment No- 4

WETTED WALL COLUMN

Aim:
To calculate the gas phase mass transfer coefficient in a wetted wall column using air-
water system.

Introduction:
A wetted wall column is essentially a vertical tube with means of admitting liquid at the
top and causing it to flow downwards along the inside wall of the tube, under the influence
of gravity and means of admitting gas to the inside of the tube, where it flows through the
tower in contact with the liquid. In absence of ripple formation at the liquid surface, the
interfacial area is known and form drag is absent.

Theory:
Mass transfer from a flowing gas to a falling liquid film is encountered in a number of
practical situations. The wetted wall tower is a classical model experimental set-up for
measuring the mass transfer coefficient. The mass transfer data obtained in such a
column also throw light on the mechanism of mass transfer in a system of similar
geometry and flow conditions. The wetted wall column is a vertical tube or pipe provided
with an arrangement for liquid feeding and withdrawal. The gas flow up through the
column and the liquid flows down as a film (which may have a calm or rippling surface
depending upon the film Reynolds number). Most of the experiment reported on the
wetted wall column involve evaporation of pure liquid in flowing stream of air and other
gases. In an experiment on evaporation of water in air, for example, the average mass
flux can be calculated from the known area of the wetted section of the wall, the total rate
of mass transfer (calculated from the flow rate of air and the moisture content at the inlet
and at the exit of the column), and the average driving force. The driving force at any
section is the difference between the vapor pressures of water at the prevailing
temperature and the partial pressure of moisture in the bulk air. Since the area of gas-
liquid contact is known and the liquid film is visible. A large number of mass transfer
correlations for the wetted wall column is available.
The above literature may be written in the mathematical form:

W
KG =
A.PLM
Wetted area A =  DL

QA ( Pw1 − Pw2 )
W=
Water evaporation rate P

Pw1 − Pw 2
PLM =
P
ln w1
Log mean pressure difference Pw 2

Experimental Setup:
The set-up consists of a glass column. Water tank is provided with a FHP pump for
circulation of water. A rotameter is provided to control the water flow rate. A heating
chamber is provided with a heater. Temperature sensors are provided to measure the
temperature of air and water.
 Schematic of wetted wall column

Requirements:
● Electrical Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amp combined socket
with earth connection.
● Water Supply.
● Floor Drain Required.
● Compressed Air Supply: @ 4 CFM at 2 bar.

Experimental Procedure:
1. Close all the valves.
2. Ensure that switches given on the panel are at OFF position.
3. Fill the water tank with water.
4. Switch ON the power supply.
 5. Switch ON the heater.
6. Open the air inlet valve and set the air flow rate.
7. Feed water to the column by opening and adjusting the water inlet valve and
bypass valve at the rate which completes the wetting of the column with
minimum ripple formation is visible.
8. Note down the dry bulb temperature and wet bulb temperature of air and water at
inlet and outlet at regular intervals.
9. Flow rate of water and air is also noted down.

Precautions:
● For condenser, the cold water supply should be constant.
● Don’t switch ON the blower at low voltage.
● Air should be moisture free.
● Wet bulb temperature apparatus should be properly connected with water.

Observations:
● Data
Diameter of the column d = 45 mm
Length of the column L = 1000 mm
Total operating pressure P = 1.013 bar
Density of air ρ = 1.205 kg/m3
Molecular weight of water MW = 18 g/mole
Molecular weight of air MA = 29 g/mole

● Observation table
S. No. T1 T2 T3 T4 T5 T6 Water flow rate Air flow rate
FW (LPH) FA (LPM)
Where
T1 = Inlet temperature of water (°C)
T2 = Outlet temperature of water (°C)
T3 = Inlet dry bulb temperature of air (°C)
T4 = Inlet wet bulb temperature of air (°C)
T5 = Outlet dry bulb temperature of air (°C)
T6 = Outlet wet bulb temperature of air (°C)

Calculations:
To calculate the humidity (Y1 & Y2) of air at temperature (T3 & T4) and (T5 & T6)
respectively by psychrometric chart.
Inlet Absolute Humidity of Air Y1 = ___________
Outlet Absolute Humidity of Air Y2 = ___________

Partial pressure of water in inlet air

PY1
Pw1 =
1 + Y1 (bar)

Partial pressure of water in outlet air

PY2
Pw 2 =
1 + Y2 (bar)

T1  = T1 + 273 (K)

T2  = T2 + 273 (K)

Vapor pressure of water in inlet air

3984.923
11.96481−
Pwv1 =e T10 −39.724
(bar)

Vapor pressure of water in inlet air

 3984.923
11.96481−
Pwv2 =e T20 −39.724
(bar)

Pw1 = Pwv1 − Pw1 (bar)

Pw 2 = Pwv2 − Pw 2 (bar)
Pw1 − Pw 2
PLM =
P
ln w1
Pw 2 (bar)

Wetted area A =  dL (m2)

F
QA =
Mass flow rate of water 1000  60 (kg/sec)

QA ( Pw1 − Pw2 )
W=
Rate of evaporation of water P (kg/sec)
W
KG =
Mass transfer coefficient A  PLM (kg/m2-bar-sec)

Results:
The value of the gas phase mass transfer coefficient in the wetted wall column is ____.

Sources of errors:
Report the possible sources of error found in the experiment and the observations.
Discuss exactly how these affect the experimental data (i.e. will the readings be larger or
will they be smaller due to the presence of a particular source).

Discussions:
1. What is the conclusion of the experiment? Is the objective fulfilled?
2. Give a physical interpretation of your results.
3. Define dry bulb and wet bulb temperatures.
4. Will variation in the temperature of inlet water give different results? If yes, then
give reasons.
References:
1. Treybal, Robert E. (1981). Mass Transfer Operations. 3rd Ed. NY: McGraw-Hill.
pp 70-72.
2. Dutta K. Binay (2007). Principles of Mass Transfer and Separation Processes.
ND: Prentice Hall of India Pvt. Ltd. pp 91, 101, 510-515.
 Experiment No.- 4B

Aim:

• To calculate the rate of drying.

• To calculate the critical moisture content.

• To plot the graph of time vs moisture content.

• To plot the graph of time vs rate of drying.

• To plot the graph of moisture content vs rate of drying.

Introduction:

In many cases, drying of materials is the final operation in the manufacturing

process, carried out immediately prior to packaging or dispatch. Drying refers to the
final removal of water, and the operation often follows evaporation, filtration or
crystallization. Drying is carried out for one or more of the following reason:

1. To reduce the cost of transport.

2. To make a material more suitable for handling.

3. To provide definite properties.

4. To remove moisture this may otherwise lead to corrosion.

Theory:

Drying of solids is considered to occur in two stages, a constant rate period followed
by a falling rate period. In the constant rate period, the rate of drying corresponds to
the removal of water from the surface of the solid. The falling rate period
corresponds to the removal of water from the interior of the solid. The rate in either
case is dependent on:

1. The solid characteristics.

2. Tray material.
 The rate of drying can be determined for a sample of a substance by suspending it over
an electronic balance in the duct. The weight of the drying sample can then be measured as
a function of time.

Let weight of dry solid is ws, weight of wet solid is ww and weight of solid after drying
w then moisture content can be calculated by:
𝑊𝑤−𝑊
𝑋𝑡 = 𝑊

Free moisture content x is:

x = x * −xt

Where x * is equilibrium moisture content

Drying rate can be calculated by:

N = − ws × Δx
A × Δt Δt is time difference.

Where Δx is moisture content difference

and

The exposure of the sample to air of constant temperature, humidity, and velocity
constitutes drying under constant drying conditions.

Rate of drying curve:

From the data obtained during such a test, a curve of moisture content as a function of
time can be plotted. This will be useful directly in determining the time required for drying
larger batches under the same drying conditions. Much information can be obtained if
the data are converted into rates of drying, expressed as N and plotted against moisture
content as shown in the following figure:

N
Xe x xc
 Determine the critical moisture contents, xc (this is the point at which falling rate is
start) from the above graph. Xe is equilibrium moisture content (at this point no more
drying is possible).

Experimental setup:

The set up consists of an insulated chamber fitted with heater. Inside the chamber a
tray is attached directly to an electronic weighing balance, which is fitted on the
bottom, outside the chamber. Temperature controller fitted in the set up maintains the
required temperature in the controller.

Requirements:

Electricity Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amp combined
socket with earth connection, Bench Area Required: 0.75m x 1m, Drying
solids: sand/asbestos/silica

Experimental procedure:

Starting procedure:

● Prepare a mixture of known weight of sand and water (30% - 50% water).
● Note down the weight of sand only.

● Fill the tray inside the chamber with the above prepare mixture.

● Ensure that switches given on the panel are at OFF position.

● Set the temperature of heater (max.110 oC).

● Note down the temperature.

● Put tray in the chamber.

● Switch ON the main power supply.

● Start the stopwatch.

● Record the balance reading with time after every 3-5 minute interval.

● Record the above reading till three consecutive balance readings are unchanged.

● Repeat the experiment for different solid material.

Closing procedure:

● When experiment is over switch OFF the main power supply.

● Remove the solid dry material from tray and clean the tray properly.

Precautions:

● Never run the apparatus if the power supply is less than 180 volts and above than 230
volts.
● Never switch on mains power supply before ensuring that all the ON/OFF switches
given on the panel are at OFF position.
● If the electric panel is not showing the input on the mains light, check the main supply.

● If D.T.I display ‘1’ on display board it means sensors connection are not OK tight it.

● If switch of the heater is ON but temperature can’t rise but panel LED is ON it means
heater had burned replace it.
Observations:

T = °C

ws = kg

ww = kg

Observation table:

Sno. t (min) w (kg)

Calculations:

𝑊𝑤−𝑊
𝑋𝑡 = 𝑊

where,
Ww-initial weight of wet solid
xt*-equilibrium free moisture content
W-weight of solid after drying at any time t

x = xt * −xt

Δx = xn − xo

Δ t = tn − to
Calculation Table: 1

Sno. t (min) ∆t (min) x ∆x

−𝑤𝑠×⧍𝑥
N= 𝐴×⧍𝑡

where,
A-area of tray
N-rate of drying
ws-initial weight of
dry solid

Calculation table: 2

Sno. N (kg/s m2) t (min) x

Results:

● Plot the graph of N vs t.

● Plot the graph of x vs t

● Plot the graph of N vs x and determine xc

Sources of errors:

Report the possible sources of error found in the experiment and the observations. Discuss
exactly how these affect the experimental data (i.e. Will the readings be larger or will they be
smaller due to the presence of a particular source).

Discussion:

● What are the various factors which affects the rate of drying?

● Discuss the uses of drying operation.

● Discuss the impact of opening the door of jacket during the experiment.

● Suggest some ways to lower the time of drying.

References:

● McCabe, Warren L. Smith, Julian C. Harriott, Peter (2005). Unit Operations of

Chemical Engineering. 7th Ed. NY: McGraw-Hill. pp 804-812.

● Coulson, J M & Richardson, J F (1991). Chemical Engineering Vol-2. 4th Ed. ND:
Asian Books Pvt. Ltd. pp 690, 693-697.

● Dutta K. Binay (2007). Principles of Mass Transfer and Separation Processes.

SOLID IN AIR DIFFUSION
(KCMT-132)
 Foreword
Welcome to the fast growing family of K.C. product owners. We appreciate your interest in us
and thank you for buying our product.

You have chosen the finest quality product in the market which is produced using latest techniques
and has underwent strict quality control tests. It is a product that we are proud to build and you
are proud to own it.

Our products are easy to understand and operate. They are excellent for students who are trying to
gain practical knowledge through experiments.

However your comfort and safety are important to us, so we want you have an understanding of
proper procedure to use the equipment. For the purpose, we urge you to read and follow the step-
by-step operating instructions and safety precautions in this manual. It will ensure that your
favourite product delivers reliable, superior performance year after year.

This manual includes information for all options available on this model. Therefore, you may find
some information that does not apply to your equipment.

All information, specifications and illustrations in this manual are those in effect at the time of
printing. We reserve the right to change specifications or design at any time without notice.

Customer satisfaction is our primary concern. Feel Free to contact us for any assistance. So what
are you waiting for, roll up your sleeves and let us get down to work!

K.C. Engineers Ltd.

 Important Information About This Manual

Reminder for Safety

Modification on Equipment:

This equipment should not be modified. Modification could affect its performance, safety or
disturbance. In addition damage or performance problems resulting from modification may not be
covered under warranties.

Precautions and Maintenance:

This is used to indicate the presence of a hazard that could cause minor or moderate personal injury
or damage to your equipment. To avoid or reduce the risk, the procedures must be followed
carefully.
 Contents
1. Objective …………………………………… 1

2. Aim …………………………………… 1

3. Introduction …………………………………… 1

4. Theory …………………………………… 1

5. Description …………………………………… 2

6. Utilities Required …………………………………… 2

7. Experimental Procedure …………………………………… 2

8. Observation & Calculation …………………………………… 3

9. Nomenclature …………………………………… 4

10. Precautions & Maintenance Instructions …………………………………… 4

11. Troubleshooting …………………………………… 5

12. References …………………………………… 6

13. Block Diagram …………………………………… 7

K.C. Engineers Limited, Ambala SOLID IN AIR DIFFUSION APPARATUS

(Rev. 1)
 SOLID IN AIR DIFFUSION APPARATUS
(VAPORIZATION OF NAPHTHALENE)
1. OBJECTIVE:
To study the vaporization of naphthalene in air.

2. AIM:
2.1 To calculate the mass transfer coefficient for vaporization of naphthalene in air
using a packed bed of spherical particles of naphthalene.

2.2 To plot (Sh / Sc)1/3 vs. Re on a log-log graph .

3. INTRODUCTION:
Diffusivity values for solids are lower than liquids and gases. Diffusion plays a major role
in catalysts and is important to chemical engineers for matallor lists; diffusion at atoms
within the solids is of more importance.

4. THEORY:
For component A (naphthalene) diffusing through non-diffusing B (air) at ambient
temperature, with diffusivity coefficient D AB in packed bed of sphere particle.

Then mass transfer coefficient can be calculated by following correlation:

DP V
Re =
ν

Where Re is Reynolds number, D P , V and ν are particle diameter, velocity of air and
kinematics viscosity of air.

ν
Sc =
D AB

Where Sc is Schmidt number.

In case of mass transfer in packed bed, Sherwood number can be calculated by using
following correlation.

K.C. Engineers Limited, Ambala SOLID IN AIR DIFFUSION APPARATUS

Page No. 1 of 7 (Rev. 1)
 𝑆𝑆ℎ = 0.61 Ф 𝑅𝑅𝑅𝑅 0.59 𝑆𝑆𝑆𝑆 0.3 ; 50<Re< 1000
Where Sh is Sherwood number, Ф is sphericity (0.91 for spherical particle)

Sh × D AB
kc =
DP

k c is experimental mass transfer coefficient.

5. DESCRIPTION:
The equipment is fitted with a vertical glass column with a mesh near the base of column
to hold the spherical balls. Spherical balls of known diameter are filled in the column to
make a packed bed. Air is allowed to pass through the silica gel member. From the
bottom of the column, dry air is allowed to enter in the packed bed. Rotameter is
provided to measure the flow rate of air.

6. UTILITIES REQUIRED:
6.1 Electricity Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amp combined socket
with earth connection.

6.2 Compressed Air Supply: @ 4 CFM at 2 bar.

6.3 Weighing Balance: 0.01 gm resolution.

6.4 Solid spherical balls of naphthalene.

7. EXPERIMENTAL PROCEDURE:

7.1 STARTING PROCEDURE:

7.1.1 Weigh the known number naphthalene balls and Record the average
diameter of the naphthalene ball.

7.1.2 Pack the glass tube with naphthalene balls up to a height of about 15-17
cm of column.

7.1.3 Connect the air line from the compressor to the valve V 2 at the base of the
column.

7.1.4 Note the ambient temperature.

K.C. Engineers Limited, Ambala SOLID IN AIR DIFFUSION APPARATUS

Page No. 2 of 7 (Rev. 1)
 7.1.5 Open the valve V 1 and set the flow rate of air.

7.1.6 Allow the air to flow through the packed bed for a fixed time (say minimum
60 min).

7.1.7 Remove the balls from packed column and weigh them.

7.1.8 Record the flow rate of air.

7.1.9 Repeat the experiment for different flow rate of air.

7.2 CLOSING PROCEDURE:

7.2.1 Remove the connection of compressed air supply.

8. OBSERVATION & CALCULATION:

8.1 DATA:
Ambient temperature, T = 20 oC
Dynamic viscosity of the air,µ = 1.82*10-5 kg/ms
Kinematic viscosity of the air, ν = 1.506*10-5 m2/s
Average diameter of the sphere D P = _____ m
Number of balls, n = _____
Diameter of the column D c = 0.050 m
Porosity, ɛ = 0.5
Diffusivity coefficient D AB = 5.81*10-6 m2/s
Density of air, ρ A = 1.205 kg/m3
Molecular weight of naphthalene, M P = 128.175 kg/mol
Sphericity, Ф = 0.91

8.2 OBSERVATION TABLE:

S.No. Q(LPM) t e , (min) W i (gm) W f (gm)

K.C. Engineers Limited, Ambala SOLID IN AIR DIFFUSION APPARATUS

Page No. 3 of 7 (Rev. 1)
 8.3 CALCULATIONS:

π 2 2
Ac = Dc (m )
4

Q
V= (m/s)
( Ac × 1000 × 60)

𝐴𝐴𝑆𝑆 = 𝑛𝑛 𝜋𝜋 𝐷𝐷𝑃𝑃 2 (m2)

DP Vρ A
Re =
6 µφ (1 − ε )

ν
Sc =
DAB

𝑆𝑆ℎ = 0.61 Ф 𝑅𝑅𝑅𝑅 0.59 𝑆𝑆𝑆𝑆 0.3

Sh × DAB
kc = (m/s)
DP

CALCULATION TABLE:

S.No. Re Sc Sh kc (Sh/Sc)1/3
1. 170.38 2.59 15.31 0.00475 1.807
2. 139.40 2.594 13.6 0.0042 1.7374
3. 108.42 2.59 11.73 0.0036 1.6536

Plot the graph of (Sh/Sc)1/3 vs. (Re) on a log-log paper.

9. NOMENCLATURE:

Nom Column Heading Units Type

Ac Cross sectional area of column m2 Calculated
2
As Total surface area of naphthalene balls m Calculated
2
D AB Diffusivity coefficient m /s Given
Dc Diameter of column m Given

K.C. Engineers Limited, Ambala SOLID IN AIR DIFFUSION APPARATUS

Page No. 4 of 7 (Rev. 1)
 Dp Average diameter of the sphere m Measured
Kc Experimental Mass transfer coefficient m/s Calculated
MP Molecular weight of naphthalene Kg/mol Given
*
n Number of balls Measured
Q Flow rate of air LPM Measured
*
Re Reynolds number Calculated
*
Sc Schmidt number Calculated
*
Sh Sherwood number Calculated
o
T Ambient temperature C Given
V Velocity of air m/s Calculated
µ Dynamic viscosity of the air kg/m-s Given
ν Kinematic viscosity of the air m2/s Given
ɛ Porosity *
Given
ρA Density of air Kg/m3 Given
Ф Sphericity *
Given

* Symbols are unit less.

10. PRECAUTION & MAINTENANCE INSTRUCTIONS:

10.1 Air pressure should be constant during the experiment.

10.2 Silica gel should be dry.

10.3 Don’t exceed the pressure above 1kg/cm2.

11. TROUBLESHOOTING:
11.1 Sometimes moisture will come with air so keep out the silica gel and dry it in sun
light 4-5 hours. Dry form of silica gel is blue color.

12. REFERENCES:
12.1 McCabe, Warren L. Smith, Julian C. Harriott, Peter (2005). Unit Operations of
Chemical Engineering. 7th Ed. NY: McGraw-Hill. pp 539, 551-552, 554-556.

K.C. Engineers Limited, Ambala SOLID IN AIR DIFFUSION APPARATUS

Page No. 5 of 7 (Rev. 1)
 12.2 Dutta K. Binay (2007). Principles of Mass Transfer and Separation Processes.
ND: Prentice Hall of India Pvt. Ltd. pp 14-16, 87, 117.

DATA BOOK

12.3 Kothandaraman, C. P. Subramanyan, S. (2007). Heat and Mass Transfer Data

Book. 6th Ed. ND: New Age International (P) Ltd. p 33.

K.C. Engineers Limited, Ambala SOLID IN AIR DIFFUSION APPARATUS

Page No. 6 of 7 (Rev. 1)
13. BLOCK DIAGRAM:

K.C. Engineers Limited, Ambala SOLID IN AIR DIFFUSION APPARATUS

Page No. 7 of 7 (Rev. 1)
 Experiment No.- 5(b)

DIFFUSION COEFFICIENT
Aim:
To find the diffusion coefficient of Acetone vapor in air using Stefan’s Tube
apparatus.

Introduction:
Diffusion of a species takes place from a region of higher concentration to a lower
concentration region.
According to Fick’s Law
dC A
j A = − DA
dz (1)
jA is Molecular Flux of species A with respect to an observer moving with average
molar velocity
DA is diffusivity of species A in a mixture
CA is the concentration of species A in a mixture.
Diffusion coefficient controls the rate of diffusion. Generally, there are two types of
diffusion-
● Diffusion of a species A through non-diffusing B
● Equimolar counter diffusion

Theory:
The molecular diffusion coefficient of a vapor in a gas is measured using the
Stefan’s tube arrangement. Here a vertical tube is partially filled with Acetone and
air is passed continuously over the top of the tube. The Acetone evaporates and
the vapors diffuse through a stagnant gas film, which is present above the liquid
surface inside the tube. The diffusion coefficient is determined by noting the liquid
level from the top of the tube for a known interval of time.

1
A tube is filled with Acetone (A) such that the liquid level is at a distance 𝑧 from the
top end of the tube. Air with a partial pressure of 𝑝𝐴2 of A is passed slowly over the
top of the tube. Vapors of Acetone diffuse through a stagnant gas film of thickness
𝑧. The partial Pressure 𝑝𝐴1 in the gas adjacent to the interface is equal to the vapor
pressure of A at the temperature of the experiment. The partial pressure at the top
end of the tube is 𝑝𝐴2 . Although this is a case of transient diffusion, it can be
analyzed as a quasi-steady state model. The steady-state flux for the diffusion of
‘A’ through stagnant ‘B’ at a given 𝑧 is
DAB P ( PA1 − PA2 )
NA =
RTz PBM (2)
where,
DAB is the molecular diffusion coefficient of A in B
P is the total pressure
R is the universal gas constant
T is the temperature on absolute scale
PBM the log mean of PB1= P-PA1 & PB2 = P-PA2
If ‘ρ’ is the density of liquid A then,
 dz
NA =
M A dt , (3)
where, MA is the molecular weight of A
Eliminating NA from equations (2) and (3) and rearranging
RTPBM  zdz
DAB dt =
P( PA1 − PA2 )M A (4)
If z = z1 at t = 0 and z = z2 at t = t then by integrating equation (4), we obtain

RTPBM ( z22 − z12 ) 

DAB =
2 P( PA1 − PA2 ) M At (5)

Experimental Setup:

2
The experimental set up consists of a diffusion cell and inside the diffusion cell
there is a central vertical glass tube (which is opened at the top and closed at the
bottom end), which is surrounded by another glass tube. The air, which is admitted
into the cell, flows up around the tube through the annular between the glass tube
and the surroundings and escapes from the topside of the tube.

Figure: Schematic Diagram

Requirements:
1. Acetone
2. Stefan Tube
3. Cathetometer
4. Compressed Air Supply

Experimental Procedure:
1. The vertical glass tube is filled with Acetone liquid up to the top of the tube
and fitted in a position in the cell.
2. By focusing the cathetometer at the top end of the tube and at the liquid
surface initially the length z1 is measured accurately.
3. The air (B) flow is started and kept steady at a very low rate. Simultaneously
a stopwatch is also started.

3
 4. Measure the height of Acetone in the tube at every 30 minutes interval and
tabulate.

Precautions:
1. Set the cathetometer at the lower meniscus of acetone level to take
readings.
2. Use an additional convex lens to take readings of Vernier scale, if
necessary.
3. Switch on the compressed air supply just before the start of operation.

Observations:
Temperature =
Universal Gas Constant =
Molecular weight of Acetone =

Time Level of Acetone

Initial Height of the liquid ‘z1’ =

Final Height of the liquid ‘z2’ =
Time taken =

Calculations:
RTPBM ( z22 − z12 ) 
DAB =
2 P( PA1 − PA2 ) M At

‘ρ’ of Acetone is = 0.7857 g/cc

P is ambient pressure

4
PA1 is partial pressure of Acetone at air-liquid contacting point
PA2 is partial pressure of Acetone in bulk air
t is the time of operation
PB 2 − PB1
PBM =
P
ln B 2
PB1

P = PA1 + PB1 = PA2 + PB 2

Result:
Diffusion coefficient of Acetone in air is …. .

Sources of errors:
Report the possible sources of error found in the experiment and the
observations. Discuss exactly how these affect the experimental data (i.e. will
the readings be larger or will they be smaller due to the presence of a particular
source).

Discussions:

1. Calculate the expected diffusion coefficient using the Chapman-Enskog

equation and compare with the experimental diffusivity.
2. Write about the effect of air flow rate and temperature on diffusion
coefficient. What should be the optimum air flow rate?
3. Give any five differences between the mass transfer coefficient and the
diffusion coefficient.
4. Give any five inferences from the experiment.
5. List five industrial uses of the experiment.

References:
1. Treybal, R.E, “Mass-Transfer Operations”, 3rd ed., McGraw-Hill, NY, 1981,
page 21-38, 88-93.

5
2. Binay K. Dutta, “Principles of Mass Transfer and Separation Processes”,
Prentice Hall of India Pvt Ltd., ND, 2007, page 7-73.

6
 1

Experiment No.- 1

BLAINE APPARATUS

Aim:
To determine porosity and specific surface area for a given powder.

Introduction:
There are several operations in Chemical Engineering which deal with bed of non-
porous particles. Determination of specific surface of a non-porous powder is a
commonly accepted method for finding particle size of that powder. There are several
ways of doing this, an air permeability method (Blain’s method) is one those.

For example, the fineness of cement is measured as specific surface. Specific surface
is expressed as the total surface area in square meters of all the cement particles in one
kilogram of cement. The higher the specific surface is, the finer cement will be.

Theory:
Surface area per unit mass is an important parameter used to characterize particles and
this characterization is important in several areas of chemical engineering. In this
experiment, we will measure the surface area of particles using a simple Blaine’s
apparatus which uses the dependence of pressure drop across a packed bed on the
effective size of the particle.

For a single phase flowing through a packed bed, the pressure drop across the packed
bed is given by Ergun’s equation:

p 1.75U o 2 (1 −  ) 150 U o (1 −  ) 2
= +
L d P 3 d P 2 3

Where
∆p is the pressure drop across the bed,
 2

L is the length of the bed (not the column),

dP is the equivalent spherical diameter of the packing,
ρ is the density of fluid,
μ is the dynamic viscosity of the fluid,
Uo is the superficial velocity
Ԑ is the void fraction (porosity) of the bed.

Reynolds number for porous medium is given by

U o Dp
Re PM =
 (1 −  )
Kozeny-Carman equation describes the laminar flow. It is valid for low Reynold’s
number which is given by:

p 150U o (1 −  ) 2 L
=
 d P 2 3 
Using Ergun’s equation pressure drop across a packed bed is related to the effective
diameter of the particle and porosity of the bed. The effective diameter of the particle
can be related to the surface area per unit volume using the following relationship –

6
Sv =
dP

Substituting the above equation in Ergun’s equation at low Reynolds number we get,

p 4.17 Sv 2  (1 −  ) 2 U 0
=
L 3

 p 3 
Sv =  
 4.17 L (1 −  ) U 0 
2

The surface area per unit volume measured in the above relation is related to the
surface area of the particle per unit mass via the true density of the particle phase -
Sv
.
P
 3

In the experiment, we will make direct observations for the pressure drop across a
packed bed along with the velocity of the fluid in the Blaine’s apparatus. Porosity will be
related to the bulk density and true density of the particulate phase in the packed bed
which will be calculated separately. The other constants like length of the bed and
viscosity of the fluid are already known.

Experimental Setup:

The apparatus consists of a U-tube with an opening connected to a Vacuum Pump, a

Powder Holder attached to one end and a Plunger to be placed on top of the powder
holder as shown in figure below. The vacuum pump is used to create a pressure
differential between the two arms of the manometer, which then drives the air to flow
through the powder held in the powder holder. This in turn reduces the level in the
manometer arm corresponding to that end.

Fig 1. Blaine’s Apparatus

 4

The pressure difference across the powder holder is calculated by measuring the levels
in the manometer arms and the rate of air flow is calculated by measuring the rate of
change of the water level in the same. With these measurements, the specific surface
area of the powder can then be found by using the Ergun equation.

Requirements:
Specific gravity bottle, measuring cylinder (10 ml), CaCO3 powder, vernier caliper, filter
paper.

Experimental Procedure:
Estimation of True Density of powder
Measure the following
1. Weight of empty specific gravity bottle W0
2. Weight of bottle + powder W1
3. Add carefully liquid such that there is no air bubble
4. Weight of bottle+ Powder & liquid W2
5. Clean the bottle thoroughly
6. Weight of bottle + liquid W3
7. Calculate true density of the Powder by the given equation.
(𝑊 −𝑊 )
𝜌𝑡𝑠 = (𝑊 −𝑊 1)−(𝑊0 −𝑊 ) × 𝜌𝑙𝑖𝑞 ...… (1)
3 1 2 1

Estimation of Bulk density of powder

1. Find the empty weight of 10 ml measuring jar Wo
2. Fill the jar with some powder (half level) and tap the jar up to 7 times.
3. Note down the volume occupied by the powder V
4. Find the weight of the jar + powder Wp
5. The bulk density of the Powder is given by weight/volume of the powder-

bs =
(W p – Wo )
V
 5

Estimation of Porosity and Specific Surface Area

1. Measure diameter, (dh) and depth of the powder holder, (Lh).
2. Measure the plunger length, (Lp).
3. Cut a filter paper equivalent to plunger diameter.
4. Slowly put the punched disc and the filter paper into the powder holder and observe
that they are placed horizontally one above the other.
5. Weigh the powder holder along with the plunger, filter paper and punched disc, W0.
6. Calculate approximately the quantity of powder required, given the bulk density of the
powder from Eq. 2.


Ws = (d h )2 [ Lh − Lp ]bs (2)
4
7. Weigh Ws gm of solid in the balance and slowly fill up the powder holder. It is filled
slowly by pushing the plunger each time a small quantity is added into the powder
holder.
8. Check if the plunger goes completely. Then add little powder so that the plunger is a
little above approximately less than 1mm.
9. Use the gap gauge to measure the gap Lg made by the plunger.
10. Find the weight of the holder along with plunger after filling powder to it, Wt.
11. Keep the holder over the Permeameter tube having rubber cork.
12. Observe that there is no air leakage between the solid holder and the cork.
13. Switch on the Vacuum Pump and operate the glass cork to pull up the liquid.
14. Ensure that the liquid does not cross the top marking.
15. Close the glass cork and remove the plunger from the powder holder. The liquid will
start falling.
16. Note the time taken, t for the liquid level to move from X1 to X2 marking from the top.
17. Remove the solid and clean the Permeameter.
(Wt − W0 )
18. Calculate porosity given by equation  = 1− (3)
( ) ts d h 2 ( Lh − Lp + Lg )
4
19. From calculated ‘  ’ & time measured ‘t’, calculate specific surface area.
 6

0.5
 t 3 
S=K 2 
 ts ( Lh − Lp + Lg ) (1 −  ) 
2 (4)

System parameter, K = 3.4906x105 cm-1/2 sec-1/2

Precautions:
1) Don’t push the plunger into the powder holder very hard otherwise it can tear the
filter paper and powder will start to pass through the holder.

2) Do not let the liquid rise above the permissible height.

3) Make sure that the rubber cork is fitted tightly on the glass tube.

Observations:
Sample- CaCO3 powder
Liquid – Water (density= 1 gm/cc)
1 ) Determination of true density:
Wt. of empty Wt. of bottle Wt. of bottle + Wt. of bottle True density
Sp.Gravity +powder powder+liquid +liquid
(W1 − W0 )
bottle (W gm) (W 2 gm) (W3 gm) ts =  liq
1
(W3 − W0 ) − (W2 − W0 )
(W0 gm)

2 ) Determination of bulk density:

Wt. of 10 ml Wt. of 10 ml measuring jar Volume occupied by Bulk density

(W – Wo )
measuring jar + powder powder after tapping (V)
bs =
p

(Wo gm) (Wp gm) V

 7

Blaine’s Apparatus
Diameter of the powder holder, (dh) = mm = cm
Depth of the powder holder, (Lh) = cm
Length of the plunger, (Lp) = cm
Weight the powder holder + plunger + filter paper + punched disc, W0 = gm


Quantity of powder needed ( approx.) , Ws = (d h )2 [ Lh − Lp ]bs = gm
4
Gap made by the plunger, Lg = mm = cm
Weight of the holder along with plunger after filling powder to it, Wt = gm

Observation Table:
Time taken, t for the liquid level to move from X1 to X2:
Obs. Time (s) Avg. time (s) (X1 –X2) cm
1
2
3

Results:
Report the bulk density, true density, porosity and the specific surface area for the given
powder. Report the specific surface area in m2/gm (1 m2/gm= 104 cm2/gm).

Sources of errors:

Report the possible sources of error found in the experiment and the observations. Discuss
exactly how these affect the experimental data (i.e. will the readings be larger or will be they be
smaller due to the presence of a particular source).
 8

Discussion:
The following topics need to be discussed in detail in the report.
1. What is the conclusion of the experiment? Is the objective fulfilled?
2. Give a physical interpretation of your results.
3. Provide any additional suitable inference.

References:
1. V.N.P. le, E.Robins, M.P. Flament, Air Permeability of Powder: A potential tool
for dry powder inhaler formulation development, European Journal of
Pharmaceutics and Biopharmaceutics 76 (2010) 464-469
2. 2. B. Kaye, Permeability technique for characterizing fine powders, Powder
Technology 1 (1) (1967) 11-22
 Experiment No. 2 (a)

FLOW THROUGH PACKED BED

Aim:
1) To calculate the pressure drop per unit length of bed.
2) To plot modified friction factor vs. modified Reynolds No. on a log-log plot.
3) To verify Ergun equation, Kozney-Karman equation and Burke-Plummer equations.

Introduction:
Chemical Engineering operations commonly involve the use of packed beds. These are
devices in which a large surface area of contact between a liquid and a gas or a solid and a
gas or liquid is obtained for achieving rapid mass and heat transfer and for chemical reactions.
Packed bed column is a cylindrical column packed with certain packing material. The packing
can be randomly filled with small objects like Raschig rings or else it can be a specifically
designed structured packing. These packings enhance the surface area available for transfer
operation. There are many engineering applications that utilize a packed bed. The forms more
commonly implemented today are incorporated with systems involving adsorption of a solute,
distillation, filtration and separation (e.g., water purification via waste removal). In an ion
exchange or catalytic reactor, a single fluid (liquid or gas) flows through a bed of densely
compacted granules used.

Theory:
Flow through a packed bed can be regarded as fluid flow past some number of submerged
objects. When there is no flow through the packed bed, the net gravitational force (including
buoyancy) acts downward. When flow begins upward, friction forces act upward and
counterbalance the net gravitational force.
The frictional force can be expressed in terms of a friction factor. This leads to equations
describing the flow of a fluid past a collection of particles. There are several approaches to
treating fluid flow through packed beds. The most successful of these is the Ergun Equation,
which describes flow in both the laminar and turbulent regimes.
The Ergun equation is given by

p 1.75Vs 2 (1 −  ) 150 Vs (1 −  ) 2 ………….. (1)

= +
L DP 3 DP 2 3
Where
∆p is the pressure drop across the bed,
L is the length of the bed (not the column),
Dp is the equivalent spherical diameter of the packing,
ρ is the density of fluid,
μ is the dynamic viscosity of the fluid,
Vs is the superficial velocity
Ԑ is the void fraction (porosity) of the bed.

Reynolds number for porous medium is given by

Vs D p
Re PM =
 (1 −  )

Kozeny-Carman equation (2) describes the laminar flow. It is valid for RePM less than about 10.

p 150Vs (1 −  ) 2 L ……………… (2)

=
 DP 2 3 

Burke-Plummer equation (3) describes the turbulent flow. It is valid for Re PM greater than 1000.

p 1.75Vs 2 (1 −  ) L ………………… (3)

=
 DP 3

Modified Reynold’s number is defined as:  wVDP

Re m =
 (1 −  )

Modified friction factor is defined as: PL D p 3

fm =
 wV 2 (1 −  )

Where Dp is the equivalent diameter, ΔPL, ε, ρw, μ and V are pressure drop per unit length, bed
porosity, density of water, viscosity and velocity of water in bed respectively.
Experimental Setup:
The apparatus consists of a glass column packed with rasching rings. Sump tank with pump is
provided for water circulation. Control valve, by pass valve and rotameter provided in pipeline
for flow control. Three pressure tapings are provided in the packed column. Pressure difference
between taping 1 & 2 or 1 & 3 can be measured by manometer after opening corresponding
valves. Flow rate can be measured by the rotameter provided.

Fig1. Block diagram of packed bed

Requirements:
1. Fluid - water
2. Stopwatch
3. Measuring Cylinder
Procedure:
1) Close all the valves V1 to V9.
2) Fill the sump tank 3/4th of its capacity with water.
3) Fill mercury in the manometer by opening air vent valves V6-V7 and then close both the
valves.
4) Open bypass valve V2.
5) Connect electric supply to the set-up.
6) Switch ON the pump.
7) Open control valve V1 and set the flow rate to maximum value, by observing rotameter.
8) Close air vent valves V6-V7.
9) Set the flow of water by control valve V1, bypass valve V2 and rotameter.
10) Note down the flow rate of water.
11) Record the manometer reading for taping 1 & 2 by opening corresponding pressure
taping valves V3-V4.
12) Record the manometer reading for taping 1 & 3 by opening corresponding pressure
taping valves V3-V5.
13) Repeat the experiment for different flow rate of water.

Precautions:
1) Never close completely the control valve V1 and bypass valve V2 simultaneously.
2) To prevent clogging of moving parts, run pump at least once in a fortnight.

Observations:
Data:
Acceleration due to gravity g = 9.81 m/s2
Viscosity of fluid μ = 8.29 x 10-4 N-s/m²
Bed porosity ∈ = 0.66
Density of manometer fluid ρm = 13600 kg/m3
Density of water ρw = 1000 kg/m3
Distance between pressure taping L = 0.36 m (For taping 1 & 2)
Distance between pressure taping L = 0.72 m (For taping 1 & 3)
Diameter of column D = 0.048 m
Equivalent Diameter of packing DP = 0.00847 m
 Observation Table:

Flow rate Select the pressure tapping (1&2)/(1&3)

S.No.
Fw (LPH) h1 (cm) h2 (cm)

Calculations:
Modified Reynold’s number  wVDP
Re m =
 (1 −  )
Fw 10−3 (m /s)  D 2 (m )
3 2
Where, Q (m/s)
V= Q= A=
A 3600 4

Modified friction factor PL D p 3

fm =
 wV 2 (1 −  )

Where, P P = (  m −  w ) g  h (N/m3) h2 − h1 (m)

PL = h =
L 100

Calculation Table:

S.No. ΔPL Rem fm

Result:
1) Plot the modified friction factor ( f m ) Vs modified Reynolds number (Rem) on log-log plot.

2) Determine the coefficient from the above plot and compare with Kozney Karman
Equation, Burke- Plummer Equation and Ergun Equations.
Sources of errors:
Report the possible sources of error found in the experiment and the observations. Discuss
exactly how these affect the experimental data (i.e. will the readings be larger or will they be
smaller due to the presence of a particular source).

Discussion:
1) Any additional inferences from experimental data
2) Give examples of five industrial uses of Packed Bed reactors.

References:
1) McCabe, Smith (2005). Unit Operations of Chemical Engineering. 7th Ed. NY: McGraw-
Hill. pp 163-166.
2) Foust, Alan S. Wenzel, Leonard A. Clump, Curtis W. Maus, Louis Andersen, L. Bryce
(1980). Principles of Unit Operations. 2nd Ed. NY: John Wiley & Sons. pp 637-6
 Experiment No. 2(b)

FLUIDIZATION

Aim:
1) To study the fluidization characteristics of Liquid- Solid fluidized bed
2) To determine the velocity of fluid.
3) To calculate the pressure drop per unit length of bed.

Introduction:
The terms “fluidization” and “fluidized bed” are used to describe the condition of fully
suspended particles, since the suspension behaves like a dense fluid. If the bed is tilted, the
top surface remains horizontal and large objects will either float or sink in the bed depending on
their density relative to the suspension. The fluidized solids can be drained from the bed
through pipes and valves just like a liquid and this fluidity is one of the main advantages in the
use of fluidization for handling solids. Fluidized beds are used successfully in a multitude of
processes both catalytic and non-catalytic.

Theory:
Fluidization converts a bed of solid particles into an expanded, suspended mass that has many
properties of a liquid. This is one of the methods available for contacting granular solids with
fluids. A fluidized bed provides a higher interfacial surface area of contact and high transfer
rates. When a fluid passes upward through a bed of solids, there will be a certain pressure drop
across the bed required to maintain the fluid flow.
At low fluid velocities, there is a pressure drop across the bed but the solid bed is static (curve
AB) as the fluid velocity is gradually increased; a certain velocity is reached when the bed
starts expanding. At this point, the pressure drop across the bed equals the mass per unit area
of the bed. This point is known as point of incipient fluidization (Point B). The pressure drop is
maximum at B.
Once the particles are separated, pressure required to maintain fluidization is less as indicated
by Point C. As the velocity is further increased the pressure drop remains constant until the bed
assumes a loosest stable form of packing (Point D).
 Fixed Bed
B Fluidized Bed

Log A
(Pressure Drop)
C D

Log (fluid velocity)

V2
The nature of fluidization can be predicted by the Froude’s Number Fr 2 =
gDP

If Fr<1 Particulate fluidization, Fr>1 Aggregative fluidization.

Pressure drop across a fixed bed is given by Ergun’s equation:

p 1.75Vs 2 (1 −  ) 150Vs (1 −  ) 2
= +
L DP 3 DP 2 3
Where
∆p is the pressure drop across the bed,
L is the length of the bed (not the column),
Dp is the equivalent spherical diameter of the packing,
ρ is the density of fluid,
μ is the dynamic viscosity of the fluid,
Vs is the superficial velocity

Minimum Fluidization Velocity (Vmf):

This is the minimum superficial fluid velocity required for the fluidization to occur. It can be
obtained by setting the pressure drop across the bed equal to the weight of the bed per unit
area of cross section, allowing for the buoyant force of the displaced fluid.
p
= g (  P −  )(1 −  )
L

At the condition of incipient fluidization (Vs=Vmf, Ԑ=Ԑmf=Minimum void fraction)

150Vmf  (1 −  mf ) 1.75Vmf2  (1 −  mf )
2

+ = (1 −  mf ) (  P −  ) g
s2 Dp2 mf 3 s Dp mf 3
Experimental setup:
The apparatus consists of a glass column packed with spherical glass beads and the water
flows through the rotameter, fitted in pipeline. Sump tank with pump is provided for water
circulation Pressure tapings are taken out from inlet and outlet pressure, are connected to a
differential manometer. Discharge is measured with the help of rotameter.

Fig1. Block diagram of fluidized bed

Requirements:
1. Measuring cylinder
2. Stopwatch
3. Meter Scale
4. Liquid- water
Procedure:
1) Close all the valves V1-V8.

2) Fill sump tank 3/4th of its capacity with water.

3) Fill CCl4 in the manometer by opening air vent valves V5-V6 & then close both the
valves.

4) Open by-pass valve V2.

5) Connect electric supply to the set-up.

6) Switch ON the pump.

7) Open valve V1 and set the flow rate to maximum value.

8) Release the air by opening pressure tapping valve V3-V4 corresponding air vent valve
V5-V6.

9) Close air vent valves V5-V6.

10) Set the flow of water by control valve V1 and bypass valve V2 and rotameter.

11) Note down the initial height of bed in column.

12) Record the flow rate of water.

13) Note down the manometer reading by opening pressure tapping valve V3 and V4.

14) Repeat the experiment for different flow rate of water.’

Precautions:

1) Never close completely the delivery line and by-pass line valves simultaneously.
2) Always use clean water.
3) If pump gets heat up, switch OFF the main power for 15 minutes and avoid closing the
flow control valve and bypass valve simultaneously during operation.

Observations:
Data:
Inside column diameter D = 0.048 m
Gravitational acceleration g = 9.81 m/s2
Density of manometric fluid ρm = 13600 kg/m3
Density of water ρw = 1000 kg/m3
 Observation Table:

S.No Z (m) Q (LPH) R1 (cm) R2 (cm)

Where Z is bed height, Q is volumetric flow rate and R1, R2 height in manometer limbs

Calculations:

Cross sectional area of column A= D 2 (m2)
4

Q  10−3
Velocity of fluid V= (m/s)
3600  A

R2 − R1
Height difference in manometer R= (m)
100

Pressure drop p = ( m −  w ) gR (N/m3)

p
Pressure drop per unit length pL = (N/m2)
L

Result:
1. Plot ΔP vs V. Note down minimum fluidization velocity from the graph.

2. Plot ΔP vs H and note point of bed expansion condition.

3. Calculate theoretical values of minimum fluidization velocity using equations and

compare it with experimental values.

Sources of errors:
Report the possible sources of error found in the experiment and the observations. Discuss
exactly how these affect the experimental data (i.e. will the readings be larger or will they be
smaller due to the presence of a particular source).
Discussion:
1. Show derivation of Vmf from Kozney – Carman equation.

2. Any additional inferences from experimental data.

3. Any suggestion for improvement of the apparatus.

4. Give five examples of important reactions in fluidized bed reactors.

References:

1) McCabe, Warren L. Smith, Julian C. Harriott, Peter (2005). Unit Operations of Chemical
Engineering. 7th Ed. NY: McGraw-Hill. pp 177-182.
2) Foust, Alan S. Wenzel, Leonard A. Clump, Curtis W. Maus, Louis Andersen, L. Bryce
(1980). Principles of Unit Operations. 2nd Ed. NY: John Wiley & Sons. pp 642-64
 Experiment No.- 3

SEDIMENTATION
Aim:
1) To study the settling behavior of slurry.
2) To plot the curve between height Vs time and velocity Vs concentration.

Introduction:
Sedimentation is the separation of a suspension or a slurry into a clear liquid, lying
above a solid residue, i.e., liquid is essentially free from particles. It consists of a
thick sludge containing a high concentration of solids. Therefore, it is a process of
phase separation.
Sedimentation is effectively used in water treatment process where suspended
solids from water is removed using gravity. Solid particles entrained by the
turbulence of moving water may be removed naturally by sedimentation in the still
water of lakes and oceans.

Theory:
Sedimentation is the process in which particles heavier than liquid medium settle
to the bottom of a liquid and form sediment (or concentrated slurry). In the gravity
settling, two main forces acting on particles: the apparent mass such as gravity
and a drag force that is due to particle motion in fluid. As many particles are
settling, the motion of the particles can be considered as hindered settling. The
hindering effects are strongly dependent on the volumetric concentration of solids,
Cv, and the relative motion of particles can be determined by Richardson and Zaki
relation given in 1954, provided the terminal velocity of the settling particles is
known,

Where,
vth is the hindered settling velocity of the solid particle
vt is the terminal velocity of the solid particle
Cv is the volumetric concentration of the solids

1
 m is the empirical exponent related to the particle Reynolds number Rep,
and Wallis (1969) proposed the following correlation to find m,

Where, Rep is the Particle Reynolds number (v is the kinematic viscosity) as

defined below,

At the beginning of a batch sedimentation process, the solid is uniformly distributed

in the liquid with a total suspension depth of H0 (Fig.1). After a short while, the
solids have settled to give a zone of clear liquid, zone A and a zone D of settled
solids. Above zone D is a thin transition layer, zone C, in which the solids content
varies from that in the original pulp to that in zone D. Above zone C is zone B
where the concentration is uniform and equal to the original concentration. The
boundaries between zones D and C and between C and B are not clear, but the
boundary between zones A and B is usually sharp. The depth of zones D and A
increase as settling continues. The depth of zone C remains nearly constant, and
that of zone B decreases. Eventually zone B disappears and solids are all in zones
C and D. Finally, the sedimentation process stop when there are only two distinct
zones, A and D.

Fig .1: Batch Sedimentation

Experimentally one can easily determine the height of the interface of clear liquid
and slurry from the bottom of the flask at different time. The settling rate can be
shown on a plot of this interface height (between zone A and B) vs. time. In the

2
beginning, the settling rate is almost constant. When zone B disappears, the
settling rate decreases and steadily drops until the ultimate height is reached. In
some cases, the interface height keep decreasing for long hours, and the ultimate
height can only be estimated.

Experimental Setup:
The experimental setup consist of three measuring cylinders of 500 ml. Light
sources are mounted on the board to see the height of layers clearly. Weighing
machine is provided to measure the weight of CaCO3 powder. Beakers and glass
rods are provided to mix the CaCO3 on water. A Stopwatch is provided to take the
readings of time corresponding to height.

Procedure:
1. Calculate the true density of CaCO3 by the following method:
Weight of empty specific gravity bottle = W0
Weight of bottle + powder = W1
Add carefully liquid such that there is no air bubble
Weight of bottle+ Powder & liquid = W2
Clean the bottle thoroughly
Weight of bottle + liquid = W3

2. Prepare suspension of three different concentration (vol%) in water: one in the

range 1-2 vol%, 2nd in the range 2-3 vol% and third 3-4 vol%.
3. Calculate accurate amount of material and water required to prepare the slurry.
4. Shake the 3 cylinders upside down closing the top with hand to obtain a uniform
concentration of the slurry.
5. Let the solids settle undisturbed. Note down the time required for the interface
of slurry – clear water (you need good adjustment of your eye) to move down
the cylinder until no further level fall is noticed.
6. Take data until liquid–solid interface remains steady.

3
 7. Plot height(H) Vs time(t) graph.
8. Calculate velocity (Ups) and concentration(C).
9. Convert the above height vs time curve to velocity vs concentration.

Precautions:
1) All the weight taken in measuring cylinders should be accurate.
2) CaCO3 powder should be well mixed into water.
3) Take the reading of height of interface (slurry-clear water) from top to
bottom.
4) Add little amount of KMnO4 if interface is not visible.

Observations:
True Density of CaCO3 = …..

Observation Table-1: Sample preparation

Vol. fraction C Vol. of CaCO3 Weight of CaCO3 Water taken

Sample 1
Sample 2
Sample 3

4
 Observation Table-2: Height vs time data
Sample- Time Height Sample- Time Height Sample- Time Height
1 2 3

Calculations:
Velocity of particle Ups = ΔH/Δt
Concentration at any height C = CoHo/H
Here Co is initial concentration of sample and Ho is initial height

Results:
Plot the curve between height(H) Vs time(t) and velocity(U) Vs concentration(C).

Sources of errors:
Report the possible sources of error found in the experiment and the observations.
Discuss exactly how these affect the experimental data (i.e. will the readings be
larger or will they be smaller due to the presence of a particular source).

Discussions:
1) Discuss the role of terminal velocity and Reynolds number.
2) What is the difference between terminal velocity and hindered velocity?
3) Discuss the settling behavior of particles.

5
 Experiment No.- 4
SIEVE ANALYSIS

Aim:
To determine the particle size distribution and the distribution parameters by sieve analysis
and also to determine optimum sieving time.

Introduction:
For the characterization of bulk goods of different forms and sizes, the knowledge of their
particle size distributions is essential. The particle size distribution, i.e. the number of
particles of different sizes, is responsible for important physical and chemical properties such
as solubility, flow ability and surface reaction. In many industries such as food,
pharmaceutics and chemistry traditional sieve analysis is the standard for production and
quality control of powders and granules. Advantages of the sieve analysis include easy
handling, low investment costs, precise and reproducible results in a comparably short time
and the possibility to separate the particle size fractions. Therefore, this method is an
accepted alternative to analysis methods using laser light or image processing. Sieve shaker
can replace manual hand sieving to conduct sample size reduction, material separation and
assist particle analysis.

Theory:
Sieve analysis is a technique used to determine the particle size distribution of a powder.
This method is performed by sifting a powder sample through a stack of wire mesh sieves,
separating it into discrete size ranges.

The sand is sieved through a set of sieves. The material retained on different sieves is
determined.
The weight fraction of material retained on any sieve is given by

Wn
= …………. (1)
W

Wn = weight of sand retained on sieve ‘n’ = (weight of sand+weight of sieve) - weight of sieve

W= total weight of the sample.

Sieving Time Estimation-

The optimum time for sieving is given by

 0.001 min-1 ..…… (2)
dt
 = weight fraction of the solid sample.
The time corresponding to this slope gives the optimum sieving time.

Rosin-Rammler distribution is given by

Q( x) = exp  −( x ) n  ………… (3)

 xd 

Q3 ( x) = 1 − exp  −( x ) n  ……….. (4)

 xd 
Where,
Q(x) is the oversize percentage
Q3(x) is the undersize percentage
xd is the size parameter
x is the particle size
n is the Rosin-Rammler distribution parameters.
Experimental Setup:
The rotap sieve shaker consists of a series of six sieves of different openings. It is run by a
FHP motor. The running parts operate in oil. No special foundation is required for the
installation of machine. A time switch from 0-60 minutes is provided.

Fig 1. Block diagram of rotap sieve shaker

Requirements:
1. Sieves
2. Electronic weighing balance
3. Raw material for feed (sand)
4. Wire Brush
Precautions:
1. Before sieving, the sand should be air dried in order to avoid lumps of fine particles
and also to prevent clogging of the finer sieves.

2. Sieves should also be cleaned before use.

3. Sieves should be arranged in descending sieve number.

4. Apparatus bolts should be well tight before start experiment.

Procedure:

1. Clean the sieves top and bottom by brush.

2. Note down the weight of each empty sieve and respective sieve number and also the
bottom pan.

3. Weigh 50 - 100 gms of the solid sample.

4. Arrange all the sieves over the pan in descending sieve number (ascending opening
size).

5. Place the weighed sample onto the top sieve and close with the lid.

6. Keep the entire set of sieves on sieve shaker and tighten the bolts so that the sieve set is
in position and does not come out during operation.

7. Switch on the sieve shaker and allow the material to be sieved for 5 min.

8. After the sieving operation, take out the set from sieve shaker.

9. Take out each sieve carefully to avoid loss of sieved material and weigh them on a
balance.

10. Note down the weight of each sieve tray with sample against respective sieve size.
11. Repeat steps 8-10 times till there is negligible change in the weights of the sieves with the
samples as compared to the previous reading.

Observations:

Time Weight of Sieves + Material (gm)

(Min)
Sieve 1 Sieve 2 Sieve 3 Sieve 4 Sieve 5 Pan

Calculation:
Time Weight % ()
(Min) Sieve 1 Sieve 2 Sieve 3 Sieve 4 Sieve 5 Pan

Calculate the optimum sieving time = ……. Min

Plot the final distribution data on Rosin-Rammler distribution graph and determine the Rosin-
Rammler parameters xd and n.

( )
ln ln( 1 ) = n ln x − n ln xd
Q

Results:
1. Plot weight fraction of the samples on each sieve vs particle size as a function of time.

2. Estimate time required for completion of sieving.

3. Estimate the constants of rosin Rammler distribution equation.

4. Plot the cumulative undersize distribution on Rosin Rammler distribution graph paper.

5. Plot Size distribution as a function of time ( vs t).

6. Tabulate and plot differential, cumulative undersize weight percent distribution vs

particle size.

Sources of errors:
Report the possible sources of error found in the experiment and the observations. Discuss
exactly how these affect the experimental data (i.e. will the readings be larger or will be they
be smaller due to the presence of a particular source).

Discussion:

1) Discuss the particle size distribution using sieve analysis results.

2) Give five industrial applications of sieving.

References:

1. Brown, George Granger(1995). Unit Operations, first Ed. ND: CBS Publishers &
Distributers. Pp 10-13, 15, 18-19

2. McCabe, Warren L. Smith, Julian C. Harriott, Peter(2005). Unit Operations of

Chemical Engineering. Seventh Ed. NY: McGraw-Hill, pp 971-972, 1000-1005
 Experiment No.- 4B

CYCLONE SEPARATOR

Aim:

● To calculate the collection efficiency of a given cyclone separator.

● To study the effect of inlet gas velocity on collection efficiency.

Introduction:

Cyclones are the principle type of gas-solids separator employing centrifugal force,
and are widely used. They are basically simple constructions; can be made from a
wide range of materials and designed for high temperature and pressure operation.
Cyclones are also extensively used for separating solids from liquids, especially for
purpose of classification.

Theory:

Cyclone is the most widely used centrifugal separation equipment for separating dust
or mist from gases. It consists of a vertical cylinder with a conical bottom, a tangential
inlet near the top, and an outlet for dust at the bottom of the cone. The incoming dust
laden air travels in a spiral path around and down the cylindrical body of the cyclone.
The centrifugal force developed in the vortex tends to move the particles radially
toward the wall, and the particles that reach the wall slide down into the cone and are
collected. The cyclone is basically a settling device in which a strong centrifugal
force, acting radially, is used in place of a relatively weak gravitational force acting
vertically.

Experimental setup:

The setup consists of I.D. blower connected to discharge side of cyclone separator. A
flow meter with manometer is provided to measure flow of air. Collector is provided to
collect solid particles. Flow control valve and by pass valve are provided for control
the flow.
CGFGFGFGFGF

Requirements:

Electricity Supply: Single phase, 220 V AC, 50 Hz, 5-15 Amp combined socket with earth
connection. Earth voltage should be less than 5 volts, Floor Area Required: 2 m x 1.0 m,
Electronics Weighing Balance: Capacity 2 kg (least count 1 gm), Raw material for feed
(Cement dust, fine dust, fly ash – 0.5 kg)

Experimental procedure:

Starting procedure:

● Prepare feedstock of cement dust or fine sand or fly ash with constant average particle
size.

● Note down the weight and size of particle of the feed.

● Switch ON the power supply.

● Start the cyclone separator.

● Fix the flow rate of air by adjusting the flow control valve V1 and by pass valve V2.

● Note down the manometer reading.

● Feed the dust particles by opening the valve.

CGFGFGFGFGF

● Collect the particles from bottom.

● Measure the weight of particles collected from the bottom of cyclone.

● Repeat the experiment for different particle size.

● Repeat the experiment for different flow rate of air.

Closing procedure:

● When the experiment is over switch OFF the power supply.

Precautions:

● Never run the apparatus if power supply is less than 180 volts and more than 230 volts

● Always use the dry particles.

● If the motor shaft is not moving but electric power is showing ON then switch OFF the
power supply and move the motor shaft manually. When it moves freely, then start it
again.

Observations:

Data:
Acceleration due to gravity g = 9.81 m/s2
Diameter of pipe for pitot tube d = 0.042 m
Density of manometric fluid ρm = 1000 kg/m3
Density of air ρa = 1.21 kg/m3
Coefficient of pitot tube Cv = 0.98

Observation table:

Sno. S h1 (cm) h2 (cm) W (kg) Wc (kg) R1 (cm) R2 (cm)

(mm)

Calculations:
CGFGFGFGFGF

∆𝐻 = ( )(
ℎ1−ℎ2
100
ρ𝑚
ρ𝑎 )( )
− 1 𝑚 𝑜𝑓 𝐻2𝑂 𝐴 =
π
4
2
( 2) 𝑉 = 𝐶𝑉
𝑑 𝑚 ( 3
)
2𝑔∆𝐻(𝑚/𝑠) 𝑄 = 𝑉𝐴 𝑚 /𝑠 η =
𝑊𝑐
𝑊
×100(%)

Where,
A-cross sectional area of pipe
Cv-coefficient of pitot tube
d- Diameter of pipe of pitot tube
g- Acceleration due to gravity
Q-flowrate of air
V-inlet velocity of air
⧍H-head loss
Wc-weight of particles collected at bottom of cyclone
W-weight of particles fed to the cyclone
h1,h2-reading of manometer for flowrate
R1,R2-reading of manometer for pressure drop

Results:

Report the collection efficiency of given cyclone separator.

Discussion:

● Discuss the various forces which should be taken into account in cyclone.

● Study the effect of inlet gas velocity on collection efficiency.

● What is the separation factor of cyclone and how it can be increased?

● Differentiate between the terms classification and clarification.

References:
McCabe, Warren L. Smith, Julian C. Harriott, Peter (2005). Unit Operations of Chemical
Engineering. 7th Ed. NY: McGraw-Hill. pp 1066-1069.
 Experiment No.- 5

DRAG COEFFICIENT EXPERIMENT

Aim:
1) To determine the drag coefficient CD and plot the graph between drag coefficient Vs
particle Reynolds number.

2) To determine the diameter of irregular particle.

Introduction:
In fluid flow there is a transfer of momentum which gives rise to tangential stress or drag
on a smooth surface that is oriented parallel to the flow direction. This is called skin
drag. In addition to this, additional friction losses occur because of acceleration and
deceleration of fluid. The accelerative effects occur when the fluid changes its path to
pass around a solid body set in the flow path. This phenomenon is known as form drag.

Theory:
Under gravitational field, the motion of particle through a fluid is due to the density
difference between the particle and the fluid. Consider the motion of a spherical particle
of diameter Dp, density ρP through a fluid of viscosity µ and density ρF.

Three forces act on a particle which is moving through a fluid.

1. The body force due to external force field, gravitational or centrifugal force (Fe).

2. The buoyancy force, due to the displaced fluid acts parallel but in direction
opposite to the body force due to external field (Fb).

3. The drag force, which appears whenever there is relative motion between
particle and the fluid. The drag force acts to oppose the motion and acts parallel
with the direction of movement but in opposite direction (FD).
 Fig 1. Particle motion in fluid

Equation for motion of particle through fluid

du
m. = Fe − Fb − FD …………….. (1)
dt

Body force (gravity) Fe = mg

 
Buoyancy force Fb = m  F g
 P 

(CD u 2  P AP )
Drag force FD =
2

m = mass of spherical particle, u = particle velocity

CD = dimensionless drag coefficient

AP = projected area of particle measured in plane perpendicular to

direction of motion of particle.

From equation (1)

du g (  P −  F ) (CDu 2  F AP )
=
dt P − 2m
Terminal velocity (ut):
As the drag increases with velocity, acceleration decreases with time and approaches
zero. The particle quickly reaches a constant, maximum velocity, called terminal
du
velocity. The equation for terminal velocity can be found by taking =0
dt

g ( P − F ) (CDut 2  F AP )
P − 2m
=0

2 (  P −  F ) mg
ut =
CD  F  P AP
………….. (2)

 P ut DP
Re P =

Particle Reynolds number is given by

Experimental Setup:
The apparatus consists of three cylindrical glass tubes, each containing a different
liquid. The density and viscosity of each liquid are known. Fluorescent tube light
mounted on the backboard. A valve system is provided at the bottom of each tube for
removal of particle. There are spheres of known diameter and specific weight. There are
also irregular shaped particles of calcite and stone.
 Fig 2. Block diagram of drag coefficient apparatus

Requirements:

1. Liquids of different viscosities

2. Regular Particles of known diameter (glass or steel), Irregular shaped particles
3. Stop Watch
4. Balance
5. Screw gauge
Procedure:

1. Close all the valves V1-V6.

2. Fill the three tubes with three different liquid.
3. Measure the diameter of glass balls using a screw gauge.
4. Measure the distance between 2 strips marked along the flow path of the particle
on the glass column.
5. Drop the particles into the tube from above and record the time taken to cover
the distance between the strips. Ensure that the particle doesn’t come into
contact with the inner walls of the tube.
6. Repeat steps 3 and 4 for 6 other glass balls and 2 steel balls and 2 Rasching ring
particles.
7. For the Raschig ring, measure the Inner dia, Outer dia and length.
8. Repeat the experiment for 2 irregular shaped particles.
9. Remove the particles from glass tube by open the valve V1-V3.

Precautions:

1) During the experiment upper valve should be open and bottom valve should be
close.
2) Collect the balls by close the upper valve and open the bottom valve for reuse.
3) Ensure that particle doesn’t come in contact with the inner walls of tube.
4) There should not be bubble formation while dropping the particle in the column.

Observations:

Density Data:

Material Density (g/cm3) ρP

Glass

Steel

Calcite
Column Number:

Fluid properties:

Fluid: Temperature:

Density: Viscosity:

Table 1: For regular particles

S. Material Particle Length Time Ut ReP CD Ut CD

No Dia. of fall (sec)
(Spherical (m/s) (from graph) (m/s) Theoretic
objects) (DP) (m) al
experi experimental Theoretical
mental

1 Glass

2 Glass

3 Glass

4 Glass

5 Steel

6 Steel
 Table 2: For irregular particles

S. Irregular Inner Outer Length Equivalent Length Time Ut ReP

No. objects diameter diameter diameter, of fall
(mm) (s) (m/s)
Deq(mm)
(mm) (mm) (m)
experimental

1 Rasching
rings

2 Rasching
rings

Irregular Weight Density Volume Equivalent Length Time Ut ReP

objects (g) diameter of fall
(g/cm3) (cm3) (sec) (m/s)
(cm) (m)
experimental

1 Calcite

2 Calcite

Calculations:

 DP 3  P  DP 2  P ut D p
For spherical particles: m = , AP = , ReP =
6 4 µ

4 g (  P −  F ) DP
CD = …………… (3)
3u 2t  F

24
At Stokes law regime (ReP << 1): CD =
ReP

gD p 2 (  P −  F )
So, Ut =
18µ

Similarly calculate the drag coefficient and terminal velocity for irregular particles.
Results:

Plot the curve between drag coefficient (CD) and particle Reynold number (Rep).

Discussion:
1) What is the significance of Reynolds number.
2) Discuss the various regions of flow on the basis of Reynolds number.
3) Discuss the role of terminal velocity and drag coefficient.

References:
1. McCabe, Warren L. Smith, Julian C. Harriott, Peter(2005). Unit Operations of
Chemical Engineering. Seventh Ed. NY: McGraw-Hill. Pp 155-159, 167-172.

2. Dr Bansal, R. K.(2008). Fluid Mechanics & Hydraulic Machines. Ninth Ed. ND:
Laxmi Publications (P) Ltd. Pp 652-654.