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 + n B 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
kr DA DB [ Bo ]
φ 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 ]
φb = 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:
 π  
( )
Aav = πDav Lav + 2   Dav2 − d r2 
Average surface area =  4  

Ap = πDav 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
φexp =
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”, 3rd ed., John Willey & Sons,
NY, 1999, Page 376-390