ORGANIC CHEMISTRY

EXPERIMENT 4

SAPONIFICATION REACTION OF FAT: SOAP

PRODUCTION

GROUP MEMBERS :
1. IHSAN BIN IDRIS CHIN (55101212178)
2. AHMAD RIDHAUDDIN BIN RUSLAN (55101212104)
3. NIK MUHAMMAD KHALIS BIN NIK MOHD SAPAWI (55101212098)
4. IDZUAN BIN IDRIS CHIN (55101212177)

SECTION : 2 DIP C

LECTURER’S NAME : MADAM NORAINI BINTI BUROK

DATE OF EXPERIMENT : 15 March 2013

DATE DUE : 20 March 2013

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OBJECTIVES

 To synthesize a sample of hard soap

 To test the soap produced.

MATERIALS

Apparatus Chemicals

Conical Flasks NaOH

Beaker 95% ethanol
Filter funnel Fat
Hirsch / Buchner funnel 50% water/ethanol mixture NaCI
Watch glass Solution
Measuring cylinder 4 % calcium chloride solution
Dropper Trisodium phosphate
Filter paper Ice-water
Aluminium foil Distilled water
10 ml graduated cylinder
pH paper

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PROCEDURE

Part A
Preparation of Soap

A NaOH solution was prepared.

(0.25 g sodium hydroxide dissolved in a mixture of 1.0 ml of distilled water and

1.0 ml of 95% ethanol.)

0.25 g of fat was placed in a 50 ml conical flask and the prepared

sodium hydroxide solution was added into the flask.

The mixture was heated in a bath of 100 oC.

The flask was covered with some aluminium foil. The Erlenmeyer flask
was swirled for few minutes by using tong.

The soap will precipitate from the boiling mixture within 20

minutes.

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 0.4 ml of a 50 % water/alcohol mixture was added to replace the
solvent if observed that some alcohol and water had evaporated.

The mixture was heated for a maximum time of 25 minutes.

4 ml of NaCl solution was placed in a 15 ml beaker and the saponified

mixture was transferred from flask to beaker.

The mixture was stirred while the beaker was cooled in an ice-water
bath.

The prepared soap was collected on a Hirsch funnel of ice cold distilled
water to remove excess NaOH.

Air was continuously drawn through the filter for a few minutes to
partially dry the product.

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 Part B
Testing on prepared Soap

0.01 g of soap was removed from the filter paper and was placed in a
clean 10 ml graduated cylinder.

3 ml of distilled water was added, the cylinder was closed with a thumb
and the mixture was shaken vigorously for 15 seconds.

The level of the foam was noted down after 30 seconds standing.

The pH of the aqueous solution was checked.

5-10 drops of 4% calcium chloride solution was added to the soap mixture from a Pasteur
pipette. The mixture was shaken for 15 sec and was allowed to stand for 30 seconds. The
effects of the addition of calcium chloride were observed.

0.5 g of trisodium phosphate was added and the mixture was shaken
again for 15 seconds. The results were observed again after 30 seconds.

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 RESULTS

Conditions Observation

1. Soap + 3 mL distilled water 5 mL of foam was formed

1. Litmus paper turned from orange to

2. Test with litmus paper blue.

2. pH value of 8.

Mixture from No 1 + 5~10 1. Mixture turned cloudy.

3.
drops of 4% calcium chloride 2. Precipitate formed from solution

Mixture from No 2 + 0.5 g

4. 1. Remains cloudy.
trisodium phosphate
2. Foam was not formed

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 DISCUSSION

This experiment is about the production of soap. Saponification is a chemical reaction

between fats and a strong base (in this case NaOH) that results in the formation of a salt and
glycerol. The saponification process involves the heating of the fats with an alkaline solution.
The alkaline solution will then hydrolyse the fats to alcohol together with the salt of a long
chain carboxylic acid (Soap). Common salt was added and the soap precipitates. The
glycerine produced is a chemical compound with a variety of uses.

This experiment is divided into two parts; Part A and Part B. In part A, the experiment
began by firstly synthesize a sample of hard soap. After the synthesis of soap is
accomplished, the test for the synthesized soap was conducted (Part B).

Through this experiment, results were able to be obtained smoothly. When 3 mL of

distilled water was added to the soap, it was observed that 5 mL of foam/ bubbles was
formed. Next, when the mixture was tested with a piece of litmus paper, it was observed that
the litmus paper turn from orange to blue with a pH value of 8. The mixture was then added
with 5 to 10 drops of 4 % Calcium Chloride, and from what has been observed, the mixture
turned cloudy and precipitate was formed from the solution. After that, 0.5 g of Trisodium
Phosphate was added and the results were observed yet again. It can be observed that the
mixture remains cloudy and no foam was formed.

Fat + 3NaOH ----> 3 moles of Na-fatty acid complex (this is for hard soap) + glycerol

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 In the preparation of soap, ethanol was used in order to hasten the saponification
process. Otherwise, the process will take a significant longer period of time. Theoretically,
the addition of soap to distilled water will form foam/ white mass of bubbles. The reason for
this is, so that the mixture will not produce any more foam in the following tests. The litmus
paper test resulted to the change of colour from red to blue which indicates an alkaline
solution (pH 8 ~ pH 14). The addition of Calcium Chloride will supposedly form an insoluble
salt (soap scum). This occur because calcium replaces sodium in the mixture, thus precipitate
was formed/ cloudy mixture. Not just that, the addition of Trisodium Phosphate will lead to
the formation of a builder which prevents the formation of soap scum. Based on the
comparison of the theory and results obtained, the results obtained are similar to that of the
described theory. Hence, the objectives of this experiment were achieved.

There are many errors that might occur during the experimentation process which will
drastically influence the results obtained. One of the errors might be caused by physical
errors (caused by experimenters). The lack of efficiency and focus of the experimenters in
conducting the experiment would strongly affect the results especially in recording down
observations. Furthermore, during the experiment, the measurement of the chemical needed
may have not followed the actual measurement needed or the chemical may have not been
covered tightly with aluminium foil that led to evaporation of the chemical. From that, the
results obtained may not be as expected. Moreover, parallax error and misreading of the
analytical balance might contribute to the errors during the process of experimentation. For
instance, the fats need for the experiment is only 0.25 g, but more than the needed amount
was used. Hence, the mass weighed ended with a different amount in which affects the end
result.

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 CONCLUSION

In conclusion, it was proven through theory, equations and experimentations that the
Saponification method can be used to produce soap by mixing Sodium Hydroxide (NaOH)
with fats which produces Sodium Salt of a specific acid used (soap) with Glycerol; whereby
the soap produced were in solid state ‘hard soap’ as the soap’s characteristic is dependent on
the alkali used. In this case, the alkali used was Sodium Hydroxide (NaOH), it produces ‘hard
soap’ as proven by theory. It was observed that the results obtained supported the theory of
Saponification.

The prepared soap was tested with a litmus paper for observation. It was observed that the
litmus paper turns from orange to blue in which refers to an alkaline sample that has a pH
value of 8. Monitored results were supported much by theory as the presence of soap was in
the range of pH values 8 to 12. Hence, based on both the results acquired and the theory
stated, the objectives were achieved as hard soap was synthesised using Sodium Hydroxide
(NaOH) and the prepared soap was tested.

In obtaining best results, the possible errors that might occur during the experiment have
been controlled. The process of weighing the filtered soap was carried out with extreme
caution to prevent any unwanted errors in the experiment in which will affect the results
achieved. Furthermore, parallax and physical errors (caused by experimenters) have also been
controlled by confirming the measured samples with team members. Confirmations were
repeated several times to achieve maximum precision in readings. By the end of this
experiment, we will be able to carry out one of the basic soap making methods which is
Saponification, to be used in the future, as a future engineering technologist.

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 TUTORIAL
Post Laboratory Questions

1. Give a definition of saponification.

A process by which triglycerides are reacted with sodium or potassium hydroxide to

produce glycerol and a fatty acids salt called ‘soap’. Lipids that contain fatty acid ester

linkages can undergo hydrolysis. This reaction is catalysed by a strong acid or base.

Saponification is the alkaline hydrolysis of the fatty acids ester. An example of the

reaction is :

2. Explain how soap can function as “dirt remover”.

Soap is an excellent cleanser because of its ability to act as an emulsifying agent. An emulsifier is
capable of dispersing one liquid into another immiscible liquid. This means that while oil (which
attracts dirt) doesn't naturally mix with water, soap can suspend oil/dirt in such a way that it can
be removed.

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3. Synthetic detergent functions in the same way as soaps. Give the advantages of synthetic
detergent over soaps
DETERGENT
Detergents can produce better performance in
hard water.
Detergents are made of synthetic petrochemicals.
detergent doesn’t produce any scum or residue
during washing of clothes and so it is better to
wash clothes with detergents earlier.
Detergents can perform well even in acidic water.
Detergents are sodium salt of long chain benzene
sulphonic acid or the sodium salt of a long chain
alkyl hydrogen sulphate
Detergents don't need expensive vegetable oil for
their preparation
SOAP
the soaps cannot suitable for use in hard water.
soap is made of vegetable oils and fatty acids, so
that consumption of natural resources is high in
soaps whereas in detergents only chemicals is
needed, so no consumption of natural resources
highly.
soap will produce scum or residue during
washing of clothes and this requires repeated
washing of clothes with water until the scum is
removed from the clothes completely.
the soaps cannot fit for use in acidic water
because the fatty acids settled down in the form
of precipitate in acidic water.
Soaps are sodium salts of higher fatty acids
Soaps cannot be used (free fatty acids are
precipitated).
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4. Reaction of fat with NaOH will produced long chain carboxylic acid (soap) in form of bar.
What would be happen if sodium hydroxide (NaOH) is replaced by Potassium hydroxide
(KOH)?

The best soaps are sodium fatty acids. They have an ionic side, which helps them be soluble in
water and a long organic chain to create a hydrophobic region to make it easier to form micelles
in water to pick up great. In addition, Soaps have distinct properties. Sodium hydroxide (NaOH)
gives "hard soap",if sodium hydroxide (NaOH) is replaced by Potassium hydroxide (KOH), a soft
soap is formed.

5. Name the all types of chemical reaction in this experiment.

a) Hydrolysis
b) Neutralization
c) Purification

6. Explain the reason of your findings for the followings:

a) Soap + 3 ml distilled wáter.

So that the soap will not lather (Production of a mass of white bubbles/ foam)

b) Soap mixture + 5-10 drops of 4% calcium chloride.

An insoluble salt is formed called soap scum. Calcium takes the place of the sodium (Na),
and a calcium salt is formed. This will result to the formation of a whitish precipitate.
2[CH3-(CH2)n-COONa] + CaCl2 ----> [CH3-(CH2)n-COO]2Ca + 2NaCl

c) Soap mixture + 0.5 g trisodium phosphate.

What is known as a builder is formed. A builder prevents the formation of insoluble

compounds in hard water. Basically, prevents the formation of soap scum.

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 REFERENCES

1. [RapidGuide, 2012],
http://www.ask.com/answers/57271161/why-is-ethanol-used-in-saponification
[19th March 2013]

2. [Brothers Handmade, 2013],

http://www.brothers-handmade.com/saponification.html
[19th March 2013]

3. [medtekph, 2009],
http://answers.yahoo.com/question/index?qid=20081210091801AAUK3Uh
[19th March 2013]

4. [wiseGEEK, 2013],
http://www.wisegeek.org/what-is-saponification.htm
[19th March 2013]

5. [Anonymous, 2013],
http://wiki.answers.com/Q/What_happens_when_trisodium_phosphate_is_added_to_soap
[19th March 2013]

6. [Anonymous, 2013],
http://wiki.answers.com/Q/What_happen_when_distilled_water_added_to_soap,
[19th March 2013]

7. [Anonymous, 2013],
http://wiki.answers.com/Q/What_is_formed_when_soap_is_added_to_water_with_dissol
ved_calcium_chloride
[19th March 2013]

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