c




 
 


The purpose this experiment was carried out was to determine the overall mass transfer
coefficient of benzoic acid between kerosene and water. Through the experiment, we are able
to find the values of the time taken for 10 droplets to travel from the top to the bottom, the
concentration of 50 droplets and the volume of NaOH needed to neutralize kerosene ± acid
solution with water. Calculation are done on the average time travelled for each droplet,
average volume for 50 droplets, average volume for 1 droplet, average surface area of the
droplet, average size of the droplet, concentration of benzoic acid in aqueous, concentration
of benzoic acid in kerosene, mole of benzoic acid transferred, molar flux and mass transfer
coefficient.



The experiment is designed to determine the mass transfer coefficient. Consider a case when
a drop of water moving through kerosene saturated with benzoic acid. Due to the
concentration difference between the benzoic in the kerosene and a water droplet, benzoic
acid is transferred across the droplet interface into the water. The molar flux of benzoic acid
through the interface, NB (mol/m2.s) is given by: NB = KC (C*B ± CB) where C*B is the
concentration of benzoic acid in kerosene at saturation, CB is the concentration of benzoic
acid in the aqueous phase and KC is the mass transfer coefficient. In order to determine KC
the values of NB, C*B and CB must first be known.

Mass transfer coefficients are not readily available for any and all systems. The "best"
solution is to experimentally measure coefficients on a bench scale (using a wetted-wall
column, etc.) and then use the results to design a full scale separation column. When this isn't
feasible, more approximate arrangements must be made. In this experiment, kerosene
saturated with benzoic acid was purified by a simple solvent extraction process. Water was
used as the extracting agent. The burette was filled with kerosene saturated with benzoic acid.
Water droplets were introduced at the top of the burette and collected by the beaker at the
bottom. As the droplets travelled down the burette, they removed some of the benzoic acid
from kerosene. By this experiment the rate at which benzoic acid was being transferred from
the kerosene to the aqueous phase was calculated. For this purpose, the concentration of
benzoic acid in the extract leaving the burette, the time of travel and the size of the droplets
were used. This information will be useful to design industrial scale extraction units operating
under similar conditions.

-c 




The apparatus used in the experiment include conical flask, 4 decimal place balance, Pasteur
pipette, burette, stirrer, dropper, beaker, stand and clamp, filter funnel, filter paper, spatula,
kerosene, water and benzoic acid.

The experiment procedures include:

1)V The 100ml burette was filled with kerosene saturated with benzoic acid to around 5cm
below the top.
2)V A Pasteur pipette was filled with distilled water.
3)V The pipette was positioned within 1cm of the kerosene surface.
4)V The pipette was carefully squeezed to produce single droplets at a steady stream
trying to maintain an equal size of the droplets and making the droplets travelling at
the centre of the burette.
5)V Steps 2-4 were repeated until the kerosene surface is near to the top of the burette.
  )V The aqueous layer at the bottom of the burette was drained into a beaker. The amount
of kerosene drained with the water was made sure to be minimized.
7)V The level of the kerosene-water interface on the burette volume scale was noted down
and recorded.
8)V 50 droplets were produced as described in steps 3-4 and the level of the interface was
read off again.
9)V Steps 7-8 were repeated until the volume change is consistent and at least 3 readings
were obtained.
10)VThe time for a droplet to travel from the air-kerosene interface to the bottom of the
column was measured. This measurement was repeated for 10 times.
11)VSteps 5-  were kept repeated until 50 ml of water is collected.
12)V20ml of the aqueous solution was pipette into a conical flask, 2 to 3 drops of
phenolphthalein were added as indicator and it was titrated with 0.03M NaOH to
determine the benzoic acid concentration in the aqueous solution (CB).
13)V10 ml of the kerosene saturated with benzoic acid together with 25ml of water was
pipette into a conical flask. 2 to 3 drops of phenolphthalein were added as indicator
and it was titrated with 0.03M NaOH to determine the benzoic acid concentration in
the aqueous solution (C*B). The solution was slowly titrated to allow sufficient time
for benzoic acid to be extracted into the aqueous phase.


 
The specific results from the experiment allow us to determine time taken for 10 droplets to
travel from the top to the bottom, the concentration of 50 droplets and the volume of NaOH
needed to neutralize kerosene ± acid solution with water.

c 



Time taken for 10 droplets to travel from the top to t he bottom
Droplet Time, t (s)
1 4. 2
2 4.84
3 4.5 
4 4.50
5 4.5 
  4.59
7 4.38
8 4.44
9 4.  
10 4.44

Concentration of 50 droplets
  




 $



  

 !"# !"# !"#
I 99.  97.2 2.4
II 99.  97.4 2.2
III 99.  97.  2.0

Titration 1 - Volume of NaOH needed to neutralize the collected water solution

from the burette
%
&
"# &' ()*'"#
 20.0 11.3

Titration 2 - Volume of NaOH needed to neutralize kerosene ± acid solution

with water
u+
 &
"# ,
"# &' ()*'"#
10 25 43

%

a)
-!

- 

4. 2 4.84 4.5  4.50 4.5  4.59 4.38 4.44 4.   4.44
A
10
A 4.5  u

b)
-!-  

2.4 2.2 2.0
=
3
= 2.2 ml
-!- 

2 .2 R
=
50
= 0.044ml
 1  10 3  1R 3 
= o0.044 R 




 1R  1000 
A 4.4  10 8 R 3

-!&   

".  #

Assuming the droplet is spherical
4
 A

3
3
4
4.4  10 8 R 3 A

3
3

3 A
o4.4 10 o3
8

4


A 3 1.05  10 8

A 2.19  10 3 R

.  



4
2
o

4 2.19 10 '3
2

 .03 10 '5 R 2

c)
%

 / 
NaOH + C H5COOH @ C H5COONa + H2 O
C H5COOH = A NaOH = B
 0.03R
 1 R 
3
B



 R 3  0.001R 3

= 30mol/m3
MAVA = MBVB
 
 A


A
o30 o1.13 10 5 R 3
2 10 5 R 3


R

 A 1  .95
R3
UThe concentration of benzoic acid in aqueous, CB= 1 .95 mol m-3





%

 0 




A
B B



o30 o4.3 10 '5

R3
110 '5 R 3


129 3
R

R
 The concentration of benzoic acid in kerosene, C*B= 129 mol m-3

 
 

R
 R

o

1 .95 '3
4.4 10 '8 R 3
 R 

7.458 10 '7 R

  
ƒ
  

 
NB =
ƒ

 

ƒ 


7.458 10 '7 R

NB

o .03 10 '5 R 2 o4.5 u
N B
2.712 10 '3 R
/ R 2 u


   


  = [CB (final) + CB (initial)] / 2 where CB (initial) = 0 mol/m3
 NB


 B ' B
2.712 10 '3 R
/ R 2 u


 1 .95R
/ R 3 
129R
/ R 3 '


 2 
 
2.25 10 '5 R / u


Based on the formula of mass flux, mass flux is inversely proportional to mass transfer area.
When the diameter of the droplet decreases, the mass transfer area between benzoic acid and
water droplet will decreases but the mass flux and mass transfer coefficient will increase.

1%
As a conclusion, the mass transfer coefficient of benzoic acid between kerosene and water is
2.25 x 10-5 m/s. Uncertainty about the accuracy of the values was related to the human error
in measuring droplets, error in recording the time, consistency of the sizes of each droplet
squeezed, the position of pipette when squeezing the droplet, the level of the kerosene-water
interface on the burette may not noted down correctly, the amount of kerosene drained with
the water may be too much and the possible error in finding the end point in titration. The
equipment deficiency could be another cause of deviation. This experiment is applicable in
industry for the extraction of solution.