Objective:The purpose of this experiment is to understand the concept of the cross current extraction and to

determine the efficiency of each stage in the multistage cross current extraction. This was done
by using mixture of toluene and acetic acid as a feed and distilled water as a solvent. Solute
acetic acid is extracted from toluene to the water.

Apparatus:Standard flash, conical flask, burette, pipette and funnel.

Components: Toluene as carrier (A), Acetic acid as solute (C), Distilled Water as (B), NaoH as titrating agent
and phenolphthalein as indicator.

Theory:Liquid-liquid extraction is a separation method and mass transfer operation in which liquid of
mixture (feed) is treated with an immiscible or nearly immiscible solvent to get the desirable
component which is soluble in solvent from the liquid of mixture. Separation of component can
be done by distillation which is most preferable method and gives higher purity components but
when relative volatility of component is very low and heating need to be avoided, distillation
method is not preferable, then liquid-liquid extraction method is used for separation. This method
separates compounds based on their relative solubility in two different immiscible liquids.
There are three ways of extraction method. These are co-current, counter-current and crosscurrent method.In this experiment cross current method was used. Cross current method is very
preferable in laboratory and for lab experiments because each stage is made up of an equilibrium
stage where the two liquid phases are mixed together for a period of time until equilibrium is
attained. Fresh solvent is added to each stage in this method while in co-current and cross-current

method solvent is added only once. This method is very rarely used in industry because of the
large volume of solvent required and low concentration of solute extracted by this method.

Efficiency of stage can be calculated by following formula:

% Efficiency =

moles of acetic acid extracted

moles of acetic acid feed

x100

Figure 1:- Schematic of cross current method

Procedure:Initially in first stage a solution mixture is prepared by mixing 60 ml of toluene and 40 ml of

acetic acid in a flask. Then 60 ml of distilled water is mixed. Mixture is shaken for 10 minutes
and then it is left unattended until 2 layers of immiscible phases are not formed clearly in the
flask. 95 ml of the settled down phase is taken out and it is diluted to 285 ml thus the normality
of liquid taken out would be N/3, where N is actual normality. Then 10 ml of this solution is
titrated with NaOH solution which has normality of 0.93 N. In second and third stage again 60

ml of water is added in mixture and same procedure is followed but 63 ml of the settled down
phase in second stage and 60 ml of the settled down phase in third stage is extracted and solution
will not be diluted as in 1st stage. After that same procedure is repeated.

Observations & Readings:-

Obs no.

1
2
3

Stage 1
Stage 2
Stage 3

Amount of

Amount of

Amount of

Amount of

Amount of

carrier

solute

solvent

extract

NaoH

added

added

added

removed

required

(ml)

(ml)

(ml)

(ml)

(ml)

60
-

40
-

60
60
60

95
63
60

21
8.5
0.5

Result:Mole of acetic acid extracted in stage 1 = 0.556

Mole of acetic acid extracted in stage 2 = 0.049
Mole of acetic acid extracted in stage 3 = 0.003

Efficiency of stage 1 = 79.58 %

Efficiency of stage 2 = 34.87 %
Efficiency of stage 3 = 2.99 %

Conclusion:It was observed that efficiency is decreasing stage by stage; this is because the amount of
extracted solute is decreasing stage by stage as solute is decreasing in carrier in each stage.
Amount of extracted solute was maximum in 1st stage and then decreases stage by stage due to
high driving force in 1st stage. Since no solute is added after 1st stage and volume of solvent is
added in each stage so concentration of solute decreases stage by stage thus driving force
decreases. Amount of extraction and efficiency depends on the amount of solvent added if
amount of solvent decreases, efficiency decreases. Selectivity, density, viscosity, relative
volatility and corrosivity are the major affecting factors. Selectivity factor determine the number
of stages required for extraction. Density difference should be high between the feed and the
solvent for better separation. High viscosity of solvent affects the mass transfer and separation
method.

Discussion:Initially in stage 1, reading of NaOH volume was not getting correctly measured in titration
procedure. Sometimes end point was coming very early and sometimes very late. It was may be
due to some human errors i.e. while making solution or putting indicator in solution.

Sample Calculation:
For stage3:
Volume of NaOH normalized = 21 ml
N1*V1= N2*V2
V1= Volume of NaOH
N1= Normality of NaOH
V2 = Volume of the extracted solution
N2= Normality of the extracted solution
N2= (N1*V1)/V2
= 0.93*8.5/10
= 0.7905
N = 0.7905 N
Moles extracted would be
N=n/V
n = N*V
= 0.7905*63/1000
= 0.04980 moles
Moles of acetic acid in total solution

Volume: 40 ml
Weight = 40*density
Density = 1.05
= 40*1.05
= 42 grams
Moles
= 42/60.05
= 0.7
Initial moles in raffinate of stage 1 = 0.7- 0.556=0.144 moles

Efficiency
= Moles extracted/moles in solution
= (0.049/0.144) *100
= 34.87 %

References:1. http://www.slideshare.net/GerardBHawkins/liquid-liquid-extraction-basic-principles?
next_slideshow=1
2. http://en.wikipedia.org/wiki/Liquid%E2%80%93liquid_extraction
3. http://www.powershow.com/view/3acbb3-ZmNkZ/Chapter_5_LiquidLiquid_Extraction_powerpoint_ppt_presentation