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Extraction of Benzoic Acid Lab Report

Extraction of Benzoic Acid Lab Report

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Lab Report
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Published by: JohnConor on Mar 27, 2011
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06/03/2013

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Extraction of Benzoic Acid
1. Abstract
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 ableto find the values of the time taken for 10 droplets to travel from the top to the bottom, theconcentration of 50 droplets and the volume of NaOH needed to neutralize kerosene ± acidsolution 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 thedroplet, average size of the droplet, concentration of benzoic acid in aqueous, concentrationof benzoic acid in kerosene, mole of benzoic acid transferred, molar flux and mass transfer coefficient.
2. Introduction
The experiment is designed to determine the mass transfer coefficient. Consider a case whena drop of water moving through kerosene saturated with benzoic acid. Due to theconcentration difference between the benzoic in the kerosene and a water droplet, benzoicacid is transferred across the droplet interface into the water. The molar flux of benzoic acidthrough the interface,
B
(mol/m
2
.s) is given by: N
B
=
C
(C*
B
± C
B
) where C*
B
is theconcentration of benzoic acid in kerosene at saturation, C
B
is the concentration of benzoicacid in the aqueous phase and K 
C
is the mass transfer coefficient. In order to determine K 
C
 the values of N
B
, C*
B
and C
B
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-wallcolumn, etc.) and then use the results to design a full scale separation column. When this isn'tfeasible, more approximate arrangements must be made. In this experiment, kerosenesaturated with benzoic acid was purified by a simple solvent extraction process. Water wasused 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 thebottom. As the droplets travelled down the burette, they removed some of the benzoic acidfrom kerosene. By this experiment the rate at which benzoic acid was being transferred fromthe 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 dropletswere used. This information will be useful to design industrial scale extraction units operatingunder similar conditions.
3
. Experiment Methods and Materials
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)
 
The 100ml burette was filled with kerosene saturated with benzoic acid to around 5cmbelow the top.2)
 
A Pasteur pipette was filled with distilled water.3)
 
The pipette was positioned within 1cm of the kerosene surface.4)
 
The pipette was carefully squeezed to produce single droplets at a steady streamtrying to maintain an equal size of the droplets and making the droplets travelling atthe centre of the burette.5)
 
Steps 2-4 were repeated until the kerosene surface is near to the top of the burette.
 
6
)
 
The aqueous layer at the bottom of the burette was drained into a beaker. The amountof kerosene drained with the water was made sure to be minimized.7)
 
The level of the kerosene-water interface on the burette volume scale was noted downand recorded.8)
 
50 droplets were produced as described in steps 3-4 and the level of the interface wasread off again.9)
 
Steps 7-8 were repeated until the volume change is consistent and at least 3 readingswere obtained.10)
 
The time for a droplet to travel from the air-kerosene interface to the bottom of thecolumn was measured. This measurement was repeated for 10 times.11)
 
Steps 5-
6
were kept repeated until 50 ml of water is collected.12)
 
20ml 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 todetermine the benzoic acid concentration in the aqueous solution (C
B
).13)
 
10 ml of the kerosene saturated with benzoic acid together with 25ml of water waspipette 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 inthe aqueous solution (C*
B
). The solution was slowly titrated to allow sufficient timefor benzoic acid to be extracted into the aqueous phase.
4. Data Analysis
The specific results from the experiment allow us to determine time taken for 10 droplets totravel from the top to the bottom, the concentration of 50 droplets and the volume of NaOHneeded to neutralize kerosene ± acid solution with water.
4.1Experiment Results
Time taken for 10 droplets to travel from the top to the bottom
Droplet Time, t (s)1 4.
6
22 4.843 4.5
6
 4 4.505 4.5
6
 
6
4.597 4.388 4.449 4.
66
 10 4.44
Concentration of 50 droplets
50DropletsInitial burette bottomreading (ml)Final burette bottomreading (ml)Difference inreading (ml)
I 99.
6
97.2 2.4II 99.
6
97.4 2.2III 99.
6
97.
6
2.0Titration 1 -
Volume of NaOH needed to neutralize the collected water solutionfrom the burette
Collected Solution (ml) Sodium Hydroxide, NaOH (ml)
 
20.0 11.3
Titration 2 - Volume of NaOH needed to neutralize kerosene ± acid solutionwith water 
erosene ± Benzoic Acid Solution (ml) Water (ml) Sodium Hydroxide, NaOH (ml)
10 25 43
4.2 Calculations
a)
Average time travelled for each droplet
s
5
6
.41044.4
66
.444.438.459.45
6
.450.45
6
.484.4
6
2.4
! !
 b)
Average volume for 50 droplets
=
30.22.24.2
 = 2.2 ml
Average volume of a droplet
=
502.2
ml 
 = 0.044ml=
¹¹º¸©©ª¨¹¹º¸©©ª¨v
mml ml 
100011101044.0
33
 
38
104.4
m
v
!
 
Average Surface Area of the Droplet (Mass Transfer Area)
Assuming the droplet is spherical
 
mm
33 8833383
1019.2 1005.1 43104.4 34104.4 34
v
!
v
!
v
!!
v
!
 
The surface area of the droplet
25232
1003.
6
1019.24 4
m
v!v!!
 c)
Concentration of benzoic acid in aqueous

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