CHM207 Lab Report Eks.3

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FACULTY OF APPLIED SCIENCES

UITM TERENGGANU, CAMPUS BUKIT BESI

CHM207
LAB REPORT

EKSPERIMENTS TITLE: EXSTRACTION AND DRYING OF AN AQUEOUS


SOLUTION.
GROUP: AS1242A

NO. NAME STUDENT ID


1. MUHAMMAD NAZHIF SYAHMI B. 2022892922
MUSSALMAN
2. NUR AINA FIRZANAH BT. MOHD ROFFI 2022470092
3. MUHAMMAD AKMAL HAKIM B. AZLAN 2022497804
4. MUHAMMAD ILHAMI FATHI BIN 2022846152
HEMIZUL

LECTURER NAME: WAN FARAHIYAH BINTI WAN KAMARUDIN


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

INTRODUCTION
The partial removal of a molecular solute from one liquid (usually water)
into another immiscible liquid is called solvent extraction in organic chemistry.
In the laboratory, the two immiscible liquids are shaken thoroughly in a
separating funnel fitted with a good stopper. The tap is open at times during the
shaking to release any pressure caused by solvent vapors. A solvent such as
ether is used because its boiling point is low, and it can be distilled from the
extracted solution and recycled. In other hands volatile organic liquids such as
ether is dangerously flammable.
Although water and ether are immiscible, water does in fact, dissolve to some
extent in ether. Due to this fact the ether extracted is always dried thoroughly
with a suitable drying agent (such as anhydrous magnesium sulphate) before the
ether is distilled off.
For a given volume of extracting solvent, it is more efficient to carry out
extraction by successive se of equal portions of the solvent rather than the use
of the whole volume in a single extraction.

CHEMICALS
15 ml of toluene solution
40 ml of diethyl ether
2 g of anhydrous magnesium sulphate
APPARATUS
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
1 pocket thermometer

PROCEDURE
1 . 15 ml of toluene and 15 ml of distilled water were mixed in a separating
funnel .
2 . 20 ml of diethyl ether was added and shaken vigorously . The tap was opened
occasionally while shaking to reduce the vapour pressure built up within . The
solution was kept shaken until no more pressure released from the solution . It
was left to stand for 2 minutes or until the solution form two stable layers .
3 . The tap was opened and then the diethyl ether layer containing toluene was
drained into a dry conical flask . The remaining aqueous layer was used for a
second extraction .
4 . The experiment was repeated by using another 20 ml diethyl ether .
5 . The combined diethyl ether layers containing toluene with one spatula of
anhydrous magnesium sulphate were dried until a clear solution is obtained .
The drying agent was filter out .
6 . The toluene was separated from ether by distillation .
DIAGRAM

DATA/RESULT
Volume of toluene used: 15ml.
Volume of diethyl ether used: 40ml.
Volume of toluene after distillation: 10ml.
Volume of diethyl ether after distillation: 0ml.
Boiling range of diethyl ether: 35°c to 109°c
Boiling point of toluene: 110°c
Percentage yield of toluene recovered:
10
×100 = 66.67%
15

Percentage yield of diethyl ether recovered: 0%


DISCUSSION
In this experiment, liquid-liquid extraction was used. Liquid-liquid extraction
involves the separation of the solutes of a liquid solution by contact with another
insoluble liquid. Solutes are separated based on their different solubilities in
different liquids. Drying is also involved in this experiment. Drying organic
solutions is the process of synthetizing and isolating an organic compound often
results in an organic compound or solution contaminated with water. In aqueous
extraction some water will be transferred into the organic phase because of
partial miscibility of the organic phase and water. This water must be removed
before the required compound can be properly characterized. Drying agent
used is anhydrous magnesium sulphate because it works well with solvent like
diethyl ether. For the result, organic solvent should be the top layer while water
will be at bottom layer. This is because organic solvent is less dense than water.
By adding a drop of water, we can know which one is aqueous layer where the
water droplet will dissolve. There are several errors that may occur during this
experiment. First is adding too much drying agent. This will cause water and
some of the products to be absorbed. Thus, less product will be gained. Second
is where the bottle cap is not closed when taking some drying agent. This will
cause the drying agent to absorb water in air and make the drying agent do not
work effectively. To overcome this error, do not put too much drying agent by
adding a little bit at a moment until the solution becomes translucent. Second,
always close the drying agent container to avoid any moisture of air will be
absorb by drying agent.
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.

Add a bit of water from squirt bottle to the separatory funnel . If the top
layer is aqueous , the water droplets should mix with the top layer and the
droplets will look like it disappears . If the bottom layers is aqueous , the
water droplets will fall through the top layer and mix with it .

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


experiment?

Anhydrous magnesium sulfate (MgSO4) is commonly used as a drying


agent. In this experiment, the MgSO4 is added into the combined diethyl
ether layers solution containing toluene to dry the remaining water found
on the layer of the organic compounds.

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?

Before the drying agent is added , the organic layer has to be separated
from the aqueous layer . Then add the drying agent if there is a second
layer on the bottom .

CONCLUSION
In conclusion, the upper layer is an organic solvent which is diethyl ether,
while the lower layer is an aqueous layer. The objective of this experiment has
been effectively attained. The methods for extracting toluene from water have
been learned. In addition, we learnt how to dry a dehydrated solution. As an
example, before ether toluene and ether is distilled we have use anhydrous
magnesium sulphate as a drying agent to dry it.
REFERENCES
https://en.wikipedia.org/wiki/Liquid%E2%80%93liquid_extraction
https://www.thermopedia.com/content/752/

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