SAPONIFICATION

Abiog M.L., Arcellana J.E., Pangilinan C.J.

INTRODUCTION

Soaps are carboxylate salts with very hydrocarbon chains. In this

experiment we prepare soap from animal fat (lard) or vegetable oil. Soap can be
made from the base hydrolysis of a fat or oil. Animal fats and Vegetable oils are
esters of carboxylic acids; they have a high molecular weight and contain the
alcohol, glycerol (Bartels et al. 2002). Chemically, these fats and oils are called
triglycerides. The process of making soap is saponification (Oxford, 1997).
Saponification or the hydrolysis of esters under alkaline conditions is a chemical
reaction that has been used for centuries as means of making soaps (Siekmann
et al. 2000). Saponification occurs by heating triglyceride fats or oils with
aqueous alkali like sodium hydroxide that results in the hydrolysis of triglyceride
esters forming soap (G.D Beal, 1926). You may also choose to add a scent to
your soap by adding an essential oil. You can purchase the scent you want to
add or isolate it from the natural source using a process of steam distillation
(Willcox et al. 2000). The most common fatty acids range in size from 10-20
carbons and most often have an even number of carbon atoms including the
carboxyl group carbon (Centeno, 2009). Since the fat or oil starting materials are
not soluble in water then saponification reaction occurs in a very slow manner
unless some provision is used for bringing the fatty ester and base into the same
phase. Example of this is to use an alcohol as a solvent to solubilize the fat and
base together and then the alcohol is removed at the end to isolate the soap
(Bartels et al. 2003).

The fats and oils that are most common in soap preparations are lard and
tallow from animal sources, and coconut, palm, and olive oils from vegetable
sources. The length of hydrocarbon chain and the number of double bonds in the
carboxylic acid portion of the fat or oil determine the properties of the resulting
soap. For example, a salt of a saturated long-chain acid makes a harder, more
insoluble soap. Chain length also affects solubility. Tallow is the principal fatty
material used in making soap. The solid fats of cattle are melted with steam, and
the tallow layer formed at the top is removed. Soap makers usually blend tallow
with coconut oil and saponify this mixture. The resulting soap contains mainly the
salts of palmitic, stearic, and oleic acids from the tallow, and the salts of lauric
and myristic acids from the coconut oil. The coconut oil is added to produce a
softer, more soluble soap. Lard (from hogs) differs from tallow (from cattle or
sheep) in that lard contains more oleic acid (Kevin M. 2010).

Pure coconut oil yields to a soap that is very soluble in water. This soap
contains essentially the salt of lauric acid with some myristic acid. It is so soft
that it will lather even in seawater. Palm oil contains mainly two acids, palmitic
acid and oleic acid, in about equal amounts. Saponification of this oil yields a
soap that is an important constituent of toilet soaps. Olive oil contains mainly
oleic acid. It is used to prepare Castile soap, named after the region in Spain in
which it was first made. Toilet soaps generally have been carefully washed free
of any alkali remaining from the saponification and as much glycerol as possible
is usually left in the soap, and perfumes and medicinal agents are sometimes
added. There is also floating soaps which can be produced by blowing air into
the soap as it solidifies. Soft soaps are made by using potassium hydroxide,
yielding potassium salts rather than the sodium salts of the acids. They are used
in shaving cream and liquid soaps. Scouring soaps have abrasives added, such
as fine sand or pumice (Tadiello, 2004).

In this experiment, the learners should be able to make soap from fat or oil
by heating it with sodium hydroxide or perform saponification. The learners also
are able to compare the different properties of the said soap that was prepared
and the commercial detergents.

MATERIALS AND METHODS

IA. Test for Unsaturation

5 drops of olive oil, oleic acid, stearic acid, peanut oil, corn oil,
linseed oil were placed in six separated test tubes. Bromine was added in CCl4,
and was shook until a reddish brown color persisted. The samples were took
care to prevent cross contamination.

B. Liebermman-Burchard Test
NOTE: This test have done by extreme caution
1. A few grains of cholesterol was placed in 3ml anhydrous chloroform by
used of clean dry test tube.
2. 10-20 drops of acetic acid anhydride were added and 2 drops of
concentrated H2SO4 were also added carefully. (Caution: The reaction was
highly exothermic. )
3. The formation of lilac color that was developed gradually were gently
mixed and observed, turned blue, and then to an emerald green color.

II. Preparation of soap

1. 10.0 grams of coconut oil was weighed in a beaker.
2. 20ml of 10% NaOH solution were mixed, covered with a watch glass,
was heated in boiling water bath, and stirred continuously in one direction until
saponification was complete. Test for saponification: one or two drops of the
mixture were shook with 5ml of warm water. Saponification was completed when
the mixture produced plenty of suds, and no oily globules separated on standing.
3. The mixture was poured into a mold and allowed it to set.
4. With 50ml of distilled water, the remaining soap from the container was
rinsed and set aside for part III.
III. Comparison of the properties of soap and detergents
1. A solution of 1g of a powdered detergent was prepared in 50ml of
distilled water.
2. In soap solution and detergent, the pH was tested by adding
phenolphthalein. The results were recorded. (Note: Phenolphthalein is colorless
in acid, purple in basic medium)
3. In two labeled test tubes, 10ml of soap solution were poured. In test
tube #1, 2ml of 0.5% CaCl2 were added; and also in test tube #2, 2ml OF 0.5%
MgCl2 were added. The procedure #3 was repeated but this time instead of soap
solution, the detergent solution was used.
4. 10ml of warm water were filled in a test tube. 1ml of cottonseed was
added, stoppered and shook. After observed, 1ml of soap solution was added to
the tube, was stoppered and shook again. Also was observed again. Procedure 4
was repeated by used of detergent instead of soap.

RESULTS AND DISCUSSION

Tests performed Soap Detergent

pH (specify acidic Soap is a base consisting of Detergents are made
or basic) metallic salts, usually in the from sodium hydroxide
form of sodium, from fatty and alcohols that made it
acids. basic.
Calcium Chloride The soap settles The
(CaCL2) solution at the bottom detergent
and didnt mix to was mixed
the CaCl2 throughout
solution. Soap the
forms a detergent
precipitate known as scum, a that made it cloudy.
hard water that consist of
CaCl2.
Emulsification Cotton seed oil Detergent
acts as the mixed
barrier to the with the
water at the oil and
bottom and water.
soap at the top.

Questions
1. Note the different fats tested for unsaturation. List them from the most
unsaturated to the least unsaturated.
Coconut Oil
Olive oil
Oleic acid
Peanut oil
Corn oil

2. Equation for

The preparation of soap from stearic acid and NaoH

C18H36O2+ KOH---> H2O+ C18H35O2K + H2O

The reaction of magnesium ions with sodium striate

Mg2+(aq) + 2C17H35COONa (aq) --> (C17H35COO)2Mg(s) +
2Na+(aq)

The magnesium stearate (octadecanoate) appears as a precipitate

- it makes up the 'scum' when soap is used with hard water.

3. From your observations, which is better emulsifying agent, soap or detergent?

Detergents are the best emulsifier for oils in water. Detergents are
molecules that have a water soluble head, and an oil soluble tail. The molecules
cluster around oils with their 'tails' in the oil and heads looking out at water,
forming a 'surface' that looks like it is water soluble.

CONCLUSION

Soaps are carboxylate salts with many hydrocarbon chains. We therefore

conclude that when preparing soap, it is very significant to finish saponification
completely in order to have no oily globules when it was tested into warm water.
In saponification, in the boiling solution of an oil substance and base, there will
be plenty of suds that will form.
We also discovered that the fats and oils that are most common in soap
preparations are lard and tallow from animal sources, and coconut, palm, and
olive oils from vegetable sources. We also knew that pure coconut oil yields to a
soap that is very soluble in water. This soap contains essentially the salt of lauric
acid with some myristic acid. It is so soft that it will lather even in seawater.
Lastly, we therefore conclude that through the use of phenolphthalein,
soap and detergent were both basic. When we place soap in hard water with the
elements Ca and Mg that are insoluble in water, precipitate will form. In this
process, the effectiveness of soap is decreased due to the soap ion removal in
the solution.

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