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Experiment 1

This document summarizes an organic chemistry experiment on extracting and drying an aqueous solution. The experiment involves: 1) Extracting toluene from a water-toluene mixture using diethyl ether in a separating funnel. 2) Drying the combined ether layers with anhydrous magnesium sulfate and filtering. 3) Distilling the dried ether to separate out the toluene. The percentages of toluene and diethyl ether recovered were calculated based on initial and final volumes. Observations during the extraction and distillation processes were also reported.

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Mhi Ismail
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256 views

Experiment 1

This document summarizes an organic chemistry experiment on extracting and drying an aqueous solution. The experiment involves: 1) Extracting toluene from a water-toluene mixture using diethyl ether in a separating funnel. 2) Drying the combined ether layers with anhydrous magnesium sulfate and filtering. 3) Distilling the dried ether to separate out the toluene. The percentages of toluene and diethyl ether recovered were calculated based on initial and final volumes. Observations during the extraction and distillation processes were also reported.

Uploaded by

Mhi Ismail
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as DOCX, PDF, TXT or read online on Scribd
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ORGANIC CHEMISTRY FOR TECHNOLOGY

CHM 412
EXPERIMENT 1
EXTRACTION AND DRYING OF AQUEOUS SOLUTION

NAME:

MARIAM HANANI ISMAIL

STUDENT ID:

2014827564

GROUP:

ED2604A

DATE OF EXPERIMENT:

3RD MAY 2016

DATE OF SUBMISSON:

10TH MAY 2016

INSTRUCTORS NAME:

MADAM FARIDAHANIM MOHD JAAFAR

Pre lab assignment:


1) Write a paragraph what do you understand about polar solvents and give at least. Three
examples of polar solvents.
Polar solvents is a liquid with a molecules that have a slight electrical charge due to its shape.
Example are water, alcohol and ketone.
2) What is the meaning for the term immiscible solution?
Immiscible solution means the liquids did not dissolve in each other.
3) Draw a diagram of separating funnel and a simple distillation apparatus set up.

Chemicals
30ml of a mixture 50:50 ratio of water and toluene solution
40 ml of ether
Adequate amount of anhydrous magnesium sulfate

Apparatus
1 separating funnel, 150ml
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
1 filter funnel
1 150ml/250ml conical flask

Procedure
1

30 ml mixture was added with 50:50 ratio of water and toluene solution into a separating funnel.
Note: in this experiment 15ml of toluene and 15ml of water mix.

20 ml of ether was added and shook vigorously. While shaking, the tap was opened occasionally
to reduce the pressure built within, this process was stopped when no more hissing. The funnel
was left to stand until the separation of the two layers stable or clearly seen.

A few drops of the bottom layer were tested by mixing with distilled water in a beaker, after
identify which is an organic and aqueous layer. The ether layer containing toluene (i.e. organic
layer) was drained into a clean and dry conical flask. The remaining solution (aqueous layer)
layer was used for a second extraction. Note: the aqueous layer will be returned back to the
separating funnel with a fresh batch of 20ml ether.

Steps 2 and 3 were repeated using another/fresh batch 20 ml ether.

The combined ether layers were dried with adequate amount of anhydrous magnesium sulfate (or
anhydrous calcium chloride), this can be indicated by no more of the anhydrous solid stuck at the
bottom of the flask and a clear solution will be obtained. The drying agent was filtered out with
gravitational filter funnel.

Toluene was separated from ether by distillation.

The volume of toluene and ether obtained was recorded. The percentages of recovery for both
solvents were calculated.

The apparatus needed for extraction and distillation was drawn.

Results

Sample

Initial

Final

Percentag

volum

volum

e of

e (ml)

recovery

(ml)
dietyl ether
40
26,9
67.25 %
toluene
15
11
73.33 %
Results of diethyl ether & toluene recovered
Calculations
Percentage recovery of diethyl ether = (26.9 / 40) x 100 = 67.25 %
Percentage recovery of toluene = (11/15) x 100 = 73.33 %
Observations
1. During separation process, both clear solutions separate. Toluene and ether is the organic
solvent (upper) and distilled water is aqueous layer (bottom). When distilled water is
added, the bottom solution increase.
2. During distillation process, the temperature is kept below 60 70 OC as ether has the
boiling point of 35 OC and toluene is 111 OC. Thus, the ether is distillated in that
temperature range. However, if it exceeds that temperature range, the toluene will also
distillate. The clear solution became pale yellow when the ether distillate. This may be
caused by the contamination from the conical used to collect the distillate.
3. The estimation of adequate amount of MgSO 4 anhydrous used during the experiment is 3
spatula of MgSO4 anhydrous when there is no more oily solution on top of the solution
and .
4. Organic solvent is ether and toluene and the aqueous solvent is distilled water.

Questions
a

Anhydrous magnesium sulfate and anhydrous calcium chloride are examples of drying
agents which remove water reversibly. Why is it necessary to filter off these drying
agents before distillation?
It is necessary to filter off the drying agents before distillation is because, the heat of the
distillation process could release some of the water, initiate a chemical reaction,
decompose the drying agent, or interfere in another manner. Basically, filtering out the
solids makes the distillation more efficient and less likely to create any complications.

Although most organic solvents are less dense than water, chloroform and
dichloromethane are not.

Explain briefly how you would separate chloroform or

dichloromethane extract from an aqueous solution using a separating funnel.


To separate chloroform and dichloromethane, a separating funnel is used to extract
mixtures of different densities. The separating funnel is cone shaped with a stopper at the
top and a tap at the bottom. The liquids are added to the funnel, mixed and then allowed
to settle so that the different densities settle out and are then slowly released separately
through the tap once total separation has occurred. Both chloroform and dichloromethane
are denser than water. You will see two layers in separating funnel. The lower layer will
be chloroform and upper layer would be aqueous layer.

Diagrams:
Distillation (5marks)
Marks distribution according to the labels in the diagram involved. Thermometer (1 mark),
water in ( mark) & out ( mark) at the condenser, receiver (1 mark), heat source (1 mark),
the reaction/round bottom flask (1 mark),
Extraction (only 2 marks)-this is because it is given in the manual.

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