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INTRODUCTION
Liquid-liquid extraction can be defined as transferring one or more
solute(s) contained in a feed solution to another immiscible liquid (solvent).
The solvent that is enriched in solute(s) is called extract. The feed solution
that is depleted in solute(s) is called raffinate. This experiment is about to
extract substance from liquid phase into another liquid phase performed
using a separator funnel.
In order to separate a substance from a mixture, we dissolve the
substance in a suitable solvent. By dissolving the substance, we can
separate the soluble compound from an insoluble compound.
As we know, the title of this experiment is liquid liquid extraction, thus
the main process involved is extraction. Extraction involves the contacting of
a solution with another solvent that is immiscible with the original. Due to
different densities, two phases are formed after the addition of the solvent.
Mass transfer will occur when the solute in the solution has more affinity
towards the added solvent.
OBJECTIVES
acid-water
and
show
its
dependence
on
concentration.
Demonstrate how a mass balance is performed on the extraction
column and to measure the mass transfer coefficient with the aqueous
phase as the continuous medium.
THEORY
Liquid-liquid extraction is a useful method to separate components or
compounds of a mixture. The extraction is based on the transfer of a solute
substance from a liquid phase into another liquid phase according to the
solubility.
At an equilibrium, in a dilute solution, the concentration of the solute in the
two phases are called the distribution coefficient or distribution constant, K
and describes in the following formula:
K = Y/X
Y: is the concentration of the solute in the extract phase
X: is the concentration of the solute in raffinate phase
Let
V w:
Vo:
X:
Y:
Subscripts :
1: Top column
2: Bottom column
X1 :
X 1 X 2
ln ( X 1 X 2)
(X 20)
X 2:
X1
( X 1 X 1 )
with concentration
Y1
APPARATUS
PROCEDURE
Experiment A:
1 A mixture of 50 ml organic solvent and 50 ml of demineralised are
made up in a conical flask.
2 5 ml of propionic acid is added. 5ml can be pipette into the flask using
a pipette with a rubber bulb.
3 A stopper is placed into a flask and it is shaken for a minimum of 5
minutes.
4 It is then poured into a separating funnel and it is left for 5 minutes.
Later, the lower aqueous later is removed.
5 A 10 ml of sample of the layer is taken and titrated against 0.1M
sodium hydroxide solution using phenolphthalein as indicator.
6 The experiment is repeated for two further concentration of propionic
acid. For example, for initial additions of 3 ml and 1 ml of propionic
acid.
Experiment B:
1 100 ml of propionic acid is added to 10 litres of organic phase. The
mixture is mixed well to ensure an even concentration then the organic
phase feed tank (bottom tank) is filled with the mixture.
2 The level control is switched to the bottom of the column (electrode
switch S2)
3 The water feed tank is filled with 15 litres of clean demineralised water,
the water feed pump is started and the column is filled with water at a
high flow rate.
4 As soon as the water is above the top of the packing, the flow rate is
reduced to 0.21 litre per minute.
5 The metering pump is started and a flow rate is set to 0.2 litre per
minute.
6 The unit is ran for 15 to 20 minutes until steady conditions are
achieved, the flow rates are monitored during this period to ensure
that they remain constant.
7 15ml of sample from the feed, raffinate and extract streams are taken.
It is ensured to not use the calibration valve V8 for taking feed
samples.
8 10 ml of
each
sample
is
titrated
against
0.1M
NaOH
using
EXPERIMENT A
DETERMINATION OF DISTRIBUTION COEFFICIENT OF SOLUTION WITH WATER
AND ITS DEPENDENCE ON CONCENTRATION
PROPANOIC
ACID
ADDED (Ml)
AQUEOUS LAYER
ORGANIC LAYER
TITRE OF
M/10 NaOH
(mL)
50
PROPIIONIC
CONCENTRA
TION
(Y)
1.00
TITRE OF
M/10
NaOH
(mL)
71
PROPIIONIC
CONCENTRA
TION
(X)
1.43
0.70
15
0.50
36.8
1.23
0.41
13
1.30
17.5
1.75
0.74
10
K=Y/X
EXPERIMENT B :
DEMONSTRATING A MASS BALANCE IN THE EXTRACTION COLUMN AND
MEASURING THE MASS COEFFICIENT, K, WITH AUQEOUS PHASE AS THE
CONTINOUS MEDIUM
FLOW RATE OF
AQUEOUS
PHASE
(L/ min)
FLOW RATE OF
ORGANIC PHASE
(L/ min)
SODIUM
HYDROXIDE
CONCENTRATIO
N (M)
FEED (mL)
RAFFINATE (mL)
EXTRACT (mL)
PROPIONIC ACID
EXTRACTED
FROM THE
ORGANIC PHASE
(mol/min)
PROPIONIC ACID
EXTRACTED
FROM THE
AQUEOUS
PHASE (mol/min)
MASS TRANSFER
COEFFICIENT
(kg/min )
0.2
0.2
0.1 M
0.025 M
17.0
10.0
6.0
0.04
54.1
15.0
23.2
0.03
CONCENTRATION OF
PROPIONIC ACID (M)
0.1 M
0.025 M
0.17
0.10
0.06
0.14
0.04
0.06
PACKING DIMENSIONS :
LENGTH: 1.2 m
DIAMETER : 50 mm
0.012
0.0025
0.3556
0.044
11
SAMPLE CALCULATIONS:
Experiment A
1 Calculation of concentration (Aqueous)
( 5 m l P r o p i o n i c Ac i d )
Fo rm u l a : M 1 V 1 = M 2 V 2
M1 =
V1 =
Vo l u m e o f N a O H ( m l )
M2 =
C o n c e n t r a t i o n o f P ro p i o n i c a c i d ( m o l e s )
V2
Vo l u m e o f P ro p i o n i c a c i d ( m l )
( 1 m l P ro p i o n i c Ac i d )
(0.1)(13 ml) = M2(1ml)
M2 = 1.3 M
C a l c u l a t i o n o f c o n c e n t r a t i o n ( 0 rg a n i c )
( 5 m l P ro p i o n i c Ac i d )
(0.1)(71 ml) = M2(5ml)
12
M1 = 1.42 M
( 3 m l P ro p i o n i c Ac i d )
(0.1)(36.8 ml) = M2(3ml)
M2 = 1.23 M
( 1 m l P ro p i o n i c Ac i d )
(0.1)(17.5 ml) = M2(1ml)
M1 = 1.75 M
2 C a l c u l a t i o n o f D i s t r i b u t i o n C o e ffi c i e n t , K :
D i s t r i b u t i o n c o e ffi c i e n t ( 5 m l P ro p i o n i c Ac i d )
Fo r m u l a :
phase, Y
C o n c e n t r a t i o n o f t h e s o l u t e i n t h e r a ffi n a t e
phase, X
K = 1.00 M
1.43M
K
= 0.70
D i s t r i b u t i o n c o e ffi c i e n t ( 3 m l P ro p i o n i c Ac i d )
K = 0.50 M
1.23 M
K
= 0.41
13
D i s t r i b u t i o n c o e ffi c i e n t ( 1 m l P ro p i o n i c Ac i d )
K = 1.30 M
1.75 M
K
= 0.74
Experiment B
1 C o n c e n t r a t i o n o f P r o p i o n i c Ac i d a t f e e d :
Fo rm u l a : M 1 V 1 = M 2 V 2
(0.1)(17.0 ml) = M2(10ml)
M2
= 0.17M
C o n c e n t r a t i o n o f P ro p i o n i c Ac i d a t Ra ffi n a t e ( X 1 )
(0.1)(10.0 ml) = M2(10ml)
M2 = 0.1M
Concentration of Propionic Acid at Extract (Y1)
(0.1)(6.0 ml) = M2(10ml)
M2 = 0.06 M
2 T h e fl o w r a t e o f a q u e o u s a n d o r g a n i c p h a s e = 0 . 2 L / m i n
3 Ra t e o f a c i d t r a n s f e r = V w ( Y 1 - 0 )
= 0.2 (0.06 - 0)
= 0.012 mol/min
0 . 0 1 2 k g / s = Vo ( X 1 - X 2 )
= 0.2 (0.1 X2)
14
To
L o g m e a n d r i v i n g f o rc e =
calculate
the
X1*,
X1 - X 2
X1
ln
X 2
calculate
the
average
c o e ffi c i e n t f r o m e x p e r i m e n t A
K
=0.70 +0.41+0.74
3
K = 0.62
Y1 = 0.06 M
K = Y1
X1*
X1* = 0.097M
X1= ( X2-0)= 0.04 M
X 2 = ( X 1 -X 1 * ) = 0 . 1 - 0 . 0 9 7 = 0 . 0 0 3
Lo g m e a n d r i v i n g f o rc e =
=
(0.04)-(0.003)
ln
0.04
(0.003
)
= 0.0143
15
X 1 - X 2
X 1
ln
X 2
distribution
5 M a s s t r a n s f e r c o e ffi c i e n t ( b a s e d o n t h e r a ffi n a t e p h a s e )
0.012
2.36 x0.0143
= 0.3556 kg/min
16
DISCUSSION
18
CONCLUSION
19
RECOMMENDATION
From the experiment that we have conducted, there are several recommendations that can
be taken to obtain more accurate results which do not differ much from the theoretical values and
observations. Before starting the experiment, we need to make sure that we have our safety attire
such as lab coat, safety helmet, and fully covered shoes to handle the experiment. We also need
to make sure the unit is checked properly where it is in a good conditions and follow the
procedures properly. If needed, use the medical gloves to avoid any solution in contact with our
hands. During titration, it needs to be made in the fume chamber to avoid us inhaling any toxic
gases and so the gaseous produced is sucked immediately when there is a gas released in a
chemical reaction. Also during titration, make sure the titration is stopped until a light pink
solution is formed to get the accurate result. When taking the reading of the volume of sodium
hydroxide titrated, avoid parallax error by making sure that eyes level is perpendicular with the
scale of the burette.
20
REFERENCES
http://www.thermopedia.com/content/752/
M. Lovric. (2000). Liquid-liquid extraction. Retrieved 7 November 2014, from
http://en.wikipedia.org/wiki/Liquid%E2%80%93liquid_extraction
Chemwiki (2001). Liquid liquid extraction. Retrieved 7 November 2014, from
http://chemwiki.ucdavis.edu/Reference/Lab_Techniques/Liquid-Liquid_Extraction
Organic Chemistry. (2014). Extraction. Retrieved 7 November 2014, from
http://orgchem.colorado.edu/Technique/Procedures/Extraction/Extraction.html
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APPENDIX
22