LIQUID – LIQUID EXTRACTION

AIM

To determine the % recovery of Acetic acid from a solution of Water – Acetic acid mixture
using Ethyl acetate as solvent by
1. Single stage
2. Three stage cross current extraction and to determine the stage efficiencies.

INTRODUCTION

Liquid extraction, sometimes called solvent extraction, is the separation of the constituents of
a liquid solution by contact with another insoluble liquid. When a solution of water-acetic
acid is agitated with ethyl acetate some of acetic acid will dissolve in the ester and only little
ester mixes with the aqueous phase. Since at equilibrium the densities of the aqueous and
organic layers are different, they form two layers on settling and can be decanted from each
other.
The solution which is to be extracted is called feed, and the liquid with which the feed is
contacted is the solvent. The solvent rich product is called the extract, and residual liquid
from which solute has been removed is the raffinate. Here acetic acid is the solute(C), water
is the carrier solvent(A) and ethyl acetate is the extracting solvent (B)

PROCEDURE

Single Stage

1. Prepare a feed solution by mixing 50 mL of water and 5mL of acetic acid. Add 75 mL
of ethyl acetate as the extracting solvent to it.
2. Stopper the flask, keep it in a flask shaker and shake for about 1 hr.
3. Separate the contents of flask using separating funnel.
4. Take about 25 mL of the organic layer and determine its refractive index or determine
the density of the layer using specific gravity bottle.
5. Obtain the mass fraction of acetic acid in the organic layer using a calibration chart or
by applying any basic stoichiometric concepts.
6. Similarly determine the mass fraction of acetic acid in the aqueous layer by titrating
against NaOH.

Multistage (Three stage) Cross current Operation

1. Prepare a feed solution by mixing 50 mL of water and 5mL of acetic acid.

2. Add 25 mL of ethyl acetate as the extracting solvent to it.
3. Stopper the flask and agitate the contents using a shaker for about 20 minutes.
4. After 20 min. separate the two layers using separating funnel and add 25 mL of Ethyl
acetate to the aqueous layer.
5. Agitate the contents for another 20 minutes.
6. Again separate the two layers and add another add 25 mL of Ethyl acetate to the
aqueous layer and agitate for 20 minutes.
7. After third agitation, separate the layers and determine the mass fraction of acetic acid
in extract and raffinate.
 8. Both single and multistage can be carried out at a time by adding required quantities
into 4 flasks, shaking one flask for 60 minutes continuously while removing the other
3 flasks after 20 min.

OBSERVATION

Sp. Gravity of water =

Sp. Gravity of acetic acid =

Sp. Gravity of ethyl acetate =

STANDARDISATION OF HCl

Weight of Na2CO3 taken in 100 cc volumetric flask =

Volume of Na2CO3 Titre value of HCl , ml

solution
Tit 1 Tit 2 Tit 3
ml

STANDARDISATION OF NaOH

Weight of oxalic acid taken in 100 cc volumetric flask =

Volume of oxalic Titre value of NaOH, ml

acid solution
Tit 1 Tit 2 Tit 3
ml

Single Stage

Volume of Extract =

Wt of sp.gravity bottle alone =

Wt of sp.gravity bottle with extract =

Sp. Gravity of Extract =

Volume of NaOH used for titration =

Multistage

Stage 1

Volume of Extract =

Wt of sp.gravity bottle alone =

Wt of sp.gravity bottle with extract =

Sp. Gravity of Extract =

Stage 2

Volume of Extract =

Wt of sp.gravity bottle alone =

Wt of sp.gravity bottle with extract =

Sp. Gravity of Extract =

Stage 3

Volume of Extract =

Wt of sp.gravity bottle alone =

Wt of sp.gravity bottle with extract =

Sp. Gravity of Extract =

Volume of NaOH used for titration =