CHM207

TITTLE : Experiment 1C: Extraction and Drying of an Aqueous Solution

NAME: IYLIA ZAFIRAH BINTI AMRAN

CLASS: AS116 3A

MATRIX NUMBER: 2019409608

LECTURER : SHARIFAH NADZIRAH BT WAN HAMID

Introduction

Reduction of molecular solute from a substance widely used in liquid suspension using immiscible
medium is recognized as solvent or liquid-liquid extraction. This method is widely used in organic
labs, where the combination of two immiscible liquids in a separating funnel is shook thoroughly
after both the tap and also the stopper are closed. Any pressure produced through solvent vapor
should be extracted from time to time by lifting the tap.

Throughout this experiment, the solvent is diethyl ether, and the ether group is well known to have
a very low boiling point that the solvent was quickly purified and recycled. As being one of the
reactive organic solvents, the ether family is extremely flammable.

By observation all water/aqueous layers are immiscible, but in some situations water
dissolved/migrate to the ether medium (as air of water vapor/moist) would be seen by naked eyes.
Because of this, after extraction, that the very first phase of the drying process that includes the use
of anhydrous substances such as magnesium sulfate or calcium chloride or other appropriate drying
agent followed by distillation for further purification.

In solvent extraction procedure; to obtained higher percentage of recovery of product or extraction

it can be obtained through successive/multiple extractions, where equal of amount of the solvent
required will be used in multiple extractions.Throughout the method of solvent extraction; to
achieve a higher percentage of product recovery or extraction, it can be achieved by subsequent
extractions at which necessary volume of solvent has been used in multiple extractions.

Objectives

To learn the techniques of separating toluene from water (and other inorganic compounds) by
extraction and to learn the techniques of drying a dehydrated solution.

Chemicals and Apparatus

15 ml of toluene solution,40 ml of diethyl ether,2 g of anhydrous magnesium sulphate,1 separating

funnel,1 retort stand,1 100 ml round bottom flask,1 condenser,1 still head,1 thermometer,1 filter
paper,1 heating mantle,1 150 ml measuring cylinder,2 rubber hoses,1 adapter and 1 pocket
thermometer.
Procedure

1.In a separating funnel , 15ml of toluene and 15ml of distilled water was mixed.

2.Shake vigorously after adding 20ml of ether. Open the tap occasionally while shaking to reduce the
vapour pressure built up within, keep shaking until no more pressure released from the
solution.Wait until the solution formed two stable layers or leaved to stand for 2 minutes.

3.Into a dry conical flak , drain the diethyl ether layer containing toluene after the tap was opened
.The remaining aqueous layer was used for a second extraction.

4.Using another 20ml diethyl ether , the experiment was repeated.

5.Until a clear solution was obtained , the combined diethyl ether layers containing toluene was
dried with about one spatula of anhydrous magnesium sulphate (or anhydrous calcium chloride).The
drying agent was filtered out.

6.By distillation method, toluene was separated from ether.

RESULTS

Volume of toluene used: _______4.0ml__________________

Volume of diethyl ether used: ___13.1ml_________________________

Volume of toluene after distillation : ___11ml________________________

Volume of diethyl ether after distillation : ___26.9ml________________________

Boiling range of diethyl ether: ___34.6oc________

Boiling point of toluene : ____110.6oc_______________

Percentage yield of toluene recovered:

(Include your calculations)

(26.9/40) x 100 = 67.25%

Percentage yield of diethyl ether recovered:

(Include your calculations)

(11/15) x 100 = 73.33%

QUESTION

1. When you are extracting an aqueous solution with an organic solvent, you are uncertain

of which layer in the separatory funnel is aqueous, how would you quickly sort out the

issue.

If the top layer is aqueous, the water droplets should mix with the top layer, and they will look as if
they disappear. If the bottom layer is aqueous, the water droplets will fall through the top layer to
mix with the bottom layer .If it is difficult to track where the water droplets go, also keep track of the
volume of the layers: whichever layer increases with the addition of water is the aqueous layer.

2. What is the purpose of using anhydrous magnesium sulphate in the experiment?

Anhydrous magnesium sulfate is used as a drying agent. The anhydrous form is hygroscopic (readily
absorbs water from the air) and is therefore difficult to weigh accurately; the hydrate is often
preferred when preparing solutions.

3. Draw the apparatus needed for extraction.

4. How do you estimate the anhydrous magnesium sulphate added is enough for the

solvent in the experiment?

Put a small amount of anhydrous magnesium sulphate into the solvent and swirled the mixture.If the
solution is translucent and there is still drying agent flowing around the mixture and not clump , the
solution is reasonably dry.
DISCUSSION

In this experiment, liquid-liquid extraction (LLE) is used, also known as solvent extraction and
partitioning, as a tool for distinguishing compounds or metal complexes based on their relative
solubility in two separate immiscible liquids, typically water (polar) and organic solvent (non-polar).
There is a net migration of one or more organisms from one liquid to another liquid form, usually
from aqueous to organic. Anhydrous magnesium sulfate is used as a drying agent. The anhydrous
form is hygroscopic (readily absorbs water from the air).For the product,organic solvent should be
the top layer while water will be at the bottom. In the separating funnel, the aqueous layer is on the
bottom, meaning the organic layer must be less dense than water meanwhile the aqueous layer is
on the top, meaning the organic layer must be more dense than water.

There are few mistakes that can arise during this experiment. First the stopcock is not secure
enough to cause the solution to be poured out To solve this be sure that the stopcock is slightly tight
so that it can still be quickly twisted over, but is not so loose that the solvent may seep around the
joint. Second, the errors existed by applying too much of the drying agent that would allow the
absorption of some of the substance and even of water. Do not use too much from the drying agent
in one time to avoid such errors. Add a little at one time until the solution is transparent and not
clumpy.

CONLUSION

To conclude , at the end of this experiment , we get to determine what is the top layer and what is
the bottom layer . We got to observed that the top layer is the organic solvent which is diethyl ether
and the bottom layer is the aqueous layer .Besides , we also achieved the objectives of this
experiment which is separating toluene from water (and other inorganic compounds) by extraction
and to learn the techniques of drying a dehydrated solution.