EXPERIMENT 6

SAPONIFICATION AND PROPERTIES OF SOAP

OBJECTIVES

Upon completion of the experiment, the student should be able to:

1. synthesize bath soap and liquid hand soap; and

2. compare the properties of the prepared soap with those of a commercial soap and
detergent.

LIST OF CHEMICALS

● NaOH pellets ● Citric acid

● Coconut oil ● Perfume

● Commercial bath soap* ● Glycerine

● Detergent* ● Benzalkonium chloride or triclosan

● Plastic cup* ● Water based dye or food color

● Sodium lauryl ether sulfate (SLES) ● pH paper

● Coco diethanolamide (CDEA) ● 3M HCl

● Distilled water ● Solid vegetable fat

● Sodium chloride

* To be assigned by the instructor a week before the performance of the experiment.

LIST OF APPARATUS

● beakers ● 2 watch glass

● 2 stirring rods ● test tubes

● spatula ● test tube rack

● top loading balance ● thermometer

● graduated cylinder ● water bath

● hot plate
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Experiment 6. Saponification and Properties of Soap

SAFETY PRECAUTIONS

1. NaOH is very caustic and can cause severe burns to the skin and is especially harmful
to the eyes. Handle it with great care. Wash your hands immediately and thoroughly if
you get it on your skin.
2. Be careful in using thermometer. Never use it to stir liquids. If the liquid is being
heated on a hot plate, do not rest the thermometer on the bottom of the container as it
will be overheated.
3. Perform the addition of water to NaOH under the hood.
4. Wear laboratory gown or apron during the entire laboratory period and safety goggles
when doing the experiment.
5. Be careful with hot objects; never use bare hands to touch them as this might cause
serious burns on your skin. Do not place hot objects on the table top.

WASTE DISPOSAL

All of the chemicals from this experiment can be disposed down the drain or in the trash.

DISCUSSION

Soap is a mixture of sodium salts of various naturally occurring fatty acids. Air bubbles
added to a molten soap will decrease the density of the soap and this it will float on water. If
the fatty acid salt has potassium rather than sodium, a softer lather is the result.
Soap is produced by hydrolyzing a fat under alkaline (basic) conditions. The reaction is
called saponification.
Fats and oils are esters of glycerol (CH 2OH-CHOH-CH2OH), a trihydroxyalcohol, and three
long chain fatty acids. Since there are three ester groups per molecule, fats and oils are often
called triglycerides. Treatment of fats and oils with strong base such as lye (NaOH) or potash
(KOH) causes them to undergo hydrolysis to form glycerol and soap. The general chemical
equation representing saponification where R is a long hydrocarbon chain of carbon atoms is:

3 NaOH

Triglyceride Glycerol Soaps

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Experiment 6. Saponification and Properties of Soap

The type of fatty acid and length of the carbon chain determines the unique properties
of various soaps. Tallow or animal fats give primarily sodium stearate (18 carbon atoms) a very

hard, insoluble soap. Coconut oil is a source of lauric acid (12 carbon atoms) which can be made
into sodium laurate. This soap is very soluble and will lather easily.
The cleansing action of soap is determined by its polar end, Na + or K+, and non-polar
end, the anion of the carboxylic acid, in conjunction with an application of solubility principles.
Since like dissolves like, the non-polar end (hydrophobic or water-fearing part) of the soap
molecule can dissolve the greasy dirt which is also non-polar. The polar or the ionic end
(hydrophilic or water-loving part) of the soap is attracted to water molecules. A spherical
structure with the polar portions of the molecule on the surface and the non-polar parts of the
molecule in the center is attracted to the water and carries the non-water-soluble material away
with it. This spherical shaped unit of soap and grime is a micelle.

Since the cleansing action of soaps depends upon the fact that they ionize readily in
water, you can imagine what would happen if the ionic end lost its charge. The soap would no
longer be attracted to water molecules and could no longer emulsify oil and dirt. This is just
what happens in hard or acidic water. Hard water contains metal cations, such as Ca 2+ and Mg2+,
that react with the charged ends of soaps to form insoluble salts. The insoluble salts that Ca 2+
and Mg2+ form with soap anions cause the gray precipitate commonly called bathtub ring.
Synthetic detergents were developed to overcome these limitations of soaps.
Detergents are similar to soaps in having an ionic end and a nonpolar end. They have different
structures which make them less susceptible to forming insoluble Ca 2+ and Mg2+ salts. Many
detergents and a few soaps contain phosphates, which serve as bases to neutralize acidic water
and also forms insoluble salts with Ca2+ and Mg2+ ions. This prevents the reaction with soap that
forms bathtub ring. However, soluble phosphate salts, like sodium phosphate, when released
into rivers and lakes can cause explosive growths of algae. This can cause decay or eventual
death of the aquatic ecosystem due to deoxygenation from the decomposition of dead algae.
Because of this, phosphates in detergents have been outlawed in many places.
There are two procedures in soap making, the “cold” and the “hot” process. The cold
process, suitable for homemade soaps, produces soap bars which retain the glycerin by-product.
If the amount of alkali employed in the saponification is limited, there is an excess of fat
(superfatted). The hot process, more suitable for laboratory or industrial preparation, yields a
more chemically pure powder; by-products and excess starting materials are separated.

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Experiment 6. Saponification and Properties of Soap

In this experiment you will make a bath soap via the cold process and liquid hand soap.
Then, you will compare the properties of the toilet soap you made with those of a commercial
soap and a commercial detergent.

PROCEDURE

I. SYNTHESIS OF BATH SOAP

1. Prepare 12.5 mL of 8M NaOH. (Read safety precaution No. 1)

a. Weigh a 150mL beaker on a top loading balance and add 4g of NaOH pellets to
it. Be careful not to sputter even a small amount of NaOH.
b. In the hood, add 12.5 mL of distilled water . To avoid splashes, use glass rod in
transferring water. Do not hold the beaker. Refer to Figure 6.1.
c. Stir the mixture of NaOH pellets and water until a clear solution is formed.
Caution: the beaker will become hot as the NaOH dissolves.
d. This solution is called lye and is very corrosive, so avoid contact with it.
2. Transfer 30 mL of coconut oil to a
beaker. Warm the beaker with the oil in Figure 6.1. Proper mixing of solutions for the
a hot plate or a hot water bath to synthesis of bath soap.
between 40 – 50 °C.
3. emove the oil from the hot water bath.
Trickle a small amount of lye down the
glass rod into the coconut oil very
slowly and then stop to stir (Refer to
Figure 6.1). Then, trickle a little more lye
in, etc. Do this continuously until all of
the lye is mixed. These steps takes time,
usually between ten to fifteen minutes.
Do not pour the lye into the oil too
quickly. Pouring the lye too quickly will
cause the oil to separate from the lye,
and your final product will be a failure.
4. Stir the mixture until it thickens. Avoid getting a mixture with 2 distinct layers – the lye
on the bottom and the oil on the top. If you see 2 distinct layers forming, stir vigorously
until the liquids are well-mixed.
5. If you want to add dyes or perfumes to your soap, do so now. Three to four drops are
sufficient. Do not add too much or you will ruin your soap.
6. Before it completely solidifies, transfer the soap to your plastic cup.
7. Label your plastic cup of soap and submit to your instructor.
8. The soap will be stored until it has solidified. This process takes one to two weeks.
II. LIQUID HAND SOAP
1. Weigh 20 grams of SLES in a beaker.
2. Dissolve the SLES in 220 mL distilled water until complete dispersion is achieved.
3. Add 5 mL of CDEA to the SLES solution and mix lightly to avoid formation of bubbles.
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Experiment 6. Saponification and Properties of Soap

4. Mix 2.5 ml of glycerine and 0.25 gram of triclosan in a separate container and add to #3
mixture.
5. Mix thoroughly and then add 1mL of perfume. Mix until complete dissolution is
achieved.
6. Add a pinch of colorant and mix thoroughly.
7. Add 0.125 gram of citric acid slowly. This will produce a pH of 7.0 - 8.0.
8. Slowly add 5 grams of sodium chloride until the desired viscosity is obtained.
9. Transfer the liquid hand soap made to a hand soap dispenser. Now it is ready to be
used.

III. DETERMINATION OF THE PROPERTIES OF SOAP AND DETERGENTS

Make separate test solutions of your prepared soap, a commercial soap and a
commercial detergent by dissolving about 1 gram of each in 50 mL distilled water.

1. pH: Test the pH of each test solutions using pH paper.

2. Cleansing ability: Test the ability of the detergent solutions to clean grease off. Put a
piece the same amount of grease on each watch glasses and test the ability of your
soaps to wash this off. Compare your soap results with the commercial soap,
commercial detergent and distilled water. Record your results.
3. Behavior in acidic water: Hydronium ions attach to one end of soap molecules,
destroying their cleaning ability by reducing their attraction to water molecules. To test
this, place 10 mL of each of your test solutions in separate clean test tubes, add 5 drops
of 3M HCl to each test tube, shake well and record your observations. Next, add 10
drops of oil to each test tube and shake well. Note your observations immediately. Set
aside the solutions for 5 minutes and observe again.
4. Behavior in hard water: Place 10 mL of each of test solutions into separate clean and
labeled test tubes. Add 2 mL of tap water to each test tube. After the addition, shake
well and immediately observe the nature of the contents, look for cloudiness,
precipitates, films, etc. Record your observations. Allow the test tubes to stand
undisturbed for 5 minutes, observe their conditions and record these observations.

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Experiment 6. Saponification and Properties of Soap

Name: Date Performed:

Course/Section: Date Submitted:
Group No: Instructor:

REPORT SHEET
Experiment 6
SAPONIFICATION AND PROPERTIES OF SOAP

RESULTS AND INTERPRETATIONS

I. PREPARATION OF SOAP

Q1: How many layers were observed? Why?

Q2: Were there any odors coming from the soap solution as you were preparing it? What
is a likely identity of this odor?

II. PREPARATION OF LIQUID HAND SOAP

Q1: Write your observations as CDEA is added to the SLES solution.

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Experiment 6. Saponification and Properties of Soap

Q2: What is the role of sodium chloride?

III. DETERMINATION OF THE PROPERTIES OF SOAPS and DETERGENTS

Table 6.1. pH of soap and detergent solutions.

SOLUTION pH BASIC / ACIDIC
Your soap
Commercial soap
Commercial detergent

Table 6.2. Cleansing abilities of soaps and detergents.

SOLUTION OBSERVATIONS
Your soap

Commercial soap

Commercial detergent

Distilled water

Table 6.3. Reactions in acidic water.

SOLUTION INITIAL OBSERVATIONS OBSERVATIONS AFTER 5 MINUTES
Your soap

Commercial soap

Commercial detergent

Distilled water

Table 6.4. Behavior in hard water.

SOLUTION HARD / TAP WATER DISTILLED WATER

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Experiment 6. Saponification and Properties of Soap

Your soap Initial

After 5 min

Commercial soap Initial

After 5 min

Commercial detergent Initial

After 5 min

POSTLAB QUESTIONS

Q1: What is the structural feature that makes both the soap and detergent effective as
cleansing agents?

Q2: Compare and contrast the action of soap and detergent.

Q3: Explain how an acidic solution affects the cleaning ability of the soap.

Q4: Discuss the environmental impact of detergents.

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Experiment 6. Saponification and Properties of Soap

REFERENCES

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