1.

ABSTRACT

This experiment was carried out to produce soap by alkali hydrolysis of saponification
process and compare its properties to the synthetic detergent dynamo. The soap prepared using
vegetable oil, ethanol and sodium hydroxide. The soap is compared with detergent in terms of
pH value, emulsification of oils, reaction in hard water, reaction in acidic water and their
cleaning ability. Through observation and test that had being carried out, we know that the soap
is alkali solution with pH value 11 and produce precipitate when react with hard water. Soap
also does not suitable use in acidic solution. The soap does not perform its process effectively
in acidic solution. As a result from the experiments, detergent is better in cleaning than the soap
prepare as detergent does not produce precipitate, and soluble in acidic solution and can clean
dirt from cloth more effective than soap. The synthetic detergent have undeniably replaced
soap for many cleaning job.

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2. INTRODUCTION
Soaps and detergents are essential to personal and public health. Through their ability
to loosen and remove soil from a surface, they contribute to good personal hygiene; reduce the
presence of germs that cause infectious diseases; extend the useful life of clothes, tableware,
linens, surfaces and furnishings; and make our homes and workplaces more pleasant.

Soaps are water-soluble sodium or potassium salts of fatty acids. Soaps are made from
fats and oils, or their fatty acids, by treating them chemically with a strong alkali. (Anonymous,
2010.pp 383) Soap safely remove germs, soils and other contaminants and help us to stay
healthy and make our surroundings more pleasant. Soaps are made from fats and oils or their
fatty acids.

Fatty acids are merely carboxylic acids consisting of a long hydrocarbon chain at one
end and a carboxyl group (-COOH) at the other end. They are generally represented as
RCOOH. They are an important component of plants, animals and other microorganisms. They
are found in various parts of the body, such as cell membranes, the nervous system and as lung
surfactant. There are two groups of fatty acids: saturated fatty acids and unsaturated fatty acids.
Saturated fatty acids is the fatty acids that contain carbon-carbon single bonds. As
examples are stearic acid (C17H35COOH) & palmitic acid (C15H31COOH). (Campbell et. al,
2015, pp. 300)

Figure 2.1: the molecule structure of stearic acid and palmatic acid.

Unsaturated fatty acids which fatty acids contain one or more double bonds between
carbon atoms. For example, Oleic acid (C17H33COOH)

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 Figure 2.2: the molecule structure of oleic acid.
If the fatty acid has a single carbon-carbon double bond in the molecule, it is known as
a mono-unsaturated fatty acid. Oleic acid is a mono-unsaturated fatty acid. If a fatty acid has
two or more carbon-carbon double bonds in the molecule, it is known as poly-unsaturated fatty
acid.

The process of saponification occurred when triglycerides in fat or oil react with
aqueous NaOH or KOH, they are converted into soap and glycerol. This is called alkaline
hydrolysis of esters. Triglycerides consist of a three-membered carbon chain (glycerol
backbone) with a fatty acid bonded to each of the three carbon atoms in the glycerol backbone.
The bond between the fatty acid and the glycerol backbone is referred to as an ester linkage. In
the saponification process the ester linkage is broken to form glycerol and soap.

Figure 2.3: the saponification of triglyceride

The soap molecule has two parts which are a polar group (-COO-Na+) and a non-polar
group (R-hydrocarbon part). The polar group is called the head and the non-polar group is
called the tail. Thus, the soap molecule has a polar head and a non-polar hydrocarbon tail. The
polar head is hydrophilic in nature (water loving) and the non-polar tail is hydrophobic (water
repelling) in nature.( Frederick,2012, pp.223)

Figure 2.4 general soap molecule.

The saponification reaction is exothermic in nature, because heat is liberated during the
process. The soap formed remains in suspension form in the mixture.

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3. AIMS
1. To prepare soap by alkaline hydrolysis of saponification process.
2. Determine the soap and detergent cleaning mechanisms.
3. Identify the comparison in properties between soap and synthetic detergent.
4. Able to understand the formation of scum in hard water when soap is being used.
5. Able to identify which one is the better cleaning product.
6. Determine the behaviour of the soap and detergent in acid acidic solution.

4
4. THEORY
Ordinary water does not remove dirt from clothes or skin because the dirt present is
oily or greasy in nature. Soaps are one of the most commonly used cleansing agents and are
capable of reacting with water to remove dirt. They are either animal origin or plant in origin.
Chemically, they are water soluble sodium or potassium salts of higher fatty acids such as
stearic acid, palmitic acid or oleic acid. Fatty acids are found in fats and oils.

(Equation 4.1)

The soap molecule is generally represented as RCOONa. In solution, it ionizes to form

RCOO- and Na+. Each soap molecule has a polar head group (carboxylate ion, COO- group)
and a long non-polar hydrocarbon tail (R group from long chain fatty acid).(Frederick, 2012,
pp.223) The polar head attracts the polar water molecule and is called hydrophilic end and the
non-polar tail attracts the water insoluble oily or greasy dirt particles.

Figure 4.1: general molecular structure of soap

When a dirty cloth is placed in soap solution, the long non-polar hydrocarbon tail of
soap molecules points towards the oily dirt particles and the polar heads point towards the
water. This forms a spherical structure with polar parts of the molecule on the surface and non-
polar parts in the center. This spherical structure is called micelle. This micelle is attracted
towards water and carries the oily dirt particles along with it. This causes the dirt particles to
detach from the fibres of the cloth. In this manner, clothes become free from dirt or dust.

5
 Figure 4.2 the formation of micelle

Although soap is a good cleaning agent, its cleaning capacity is reduced when used in
hard water. Hardness of water is due to the presence of sulphates, chlorides or bicarbonate salts
of Ca2+ or Mg 2+ ions. Soaps are sodium or potassium salts of long chain fatty acids. When
soap is added to hard water, the Ca2+ and Mg 2+ ions present in hard water react with soap. The
sodium salts present in soaps are converted to their corresponding calcium and magnesium
salts which are precipitated as scum. The insoluble scum sticks on the clothes and so the
cleaning capacity of soap is reduced.( Norman H.,2002, pp.773)

(Equation 4.2)

(Equation 4.3)

Hard water can be softened using ion exchange technique or by adding sodium
carbonate or water softener or distilled. Water softener react with Ca2+ , Mg 2+ and Fe3+ ions
and removing them from the water at the same time preventing the reaction of these ions with
soap. Then the soap can act as surfactant and emulsifier as usual. Detergent work better in hard
water than soaps. Detergent lather in hard water when soaps do not. A molecule of detergent
made from palm oil, called sodium lauryl sulphate has two ends of the molecule which are non-
polar and polar. This detergent is anionic detergent.

Figure 4.3 the alkyl sulfonate molecule in detergent

Sulfonic acid is a a stronger acid than carboxylic acid, syndets do not precipitate in
acidic solution. Synthetic detergent such as alkyl sulfonate above do not form insoluble salts
in hard water. Their Ca2+ and Mg 2+ are soluble in water.

6
5. APPARATUS

Apparatus Materials
Magnetic stirrer Vegetable oil
Magnetic stirrer bar Ethanol
Beaker Sodium hydroxide
Dropper Synthetic detergent (Dynamo)
Cloth strip Distilled water
250 mL Erlenmeyer flask Ice bath
Glass rod Saturated sodium chloride
Measuring cylinder 1% CaCl2 solution
Ph papers 1% MgCl2 solution
Retort stand and clamp 1% FeCl2 solution
Petric dish Tomato sauce
Mass weight electronic Mineral oil
Test tube with racks 1M hydrochloric acid
Vacuum filtration apparatus
Filter paper

Table 5.1: list of apparatus and materials used in the experiment.

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6. PROCEDURE
PART A: SOAP PREPARATION

1. 25 mL of vegetable oil is placed in a 250 mL Erlenmeyer flask. 20 mL of ethanol and

25 mL of 6 M sodium hydroxide solution are added to the flask. The mixture is stirrer
with a stirring rod to mix the contents of the flask.
2. 250 mL Erlenmeyer flask is heated in a boiling water bath inside a 600 mL beaker.
3. The mixture is continuously stirred during the heating process to prevent the mixture
from foaming. If the mixture should foam to the point of nearly overflowing, the flask
is remove from the boiling-water bath until the foaming subsides, then continued
heating. The mixture is heated for 20-30 minute or until the alcohol odour is no longer
detectable.
4. The paste-like mixture is removed from the boiling-water bath and the flask is cooled
in an ice bath for 10-15 minutes.
5. While the flask is cooled, the vacuum filtration apparatus shown in Figure 3-5 is
assembled. The vacuum flask to a ring stand with a utility clamp is secured to prevent
the apparatus from toppling over.

Figure 6.1: the vacuum filtration apparatus

6. A piece of filter paper is weighted to the nearest 0.001 g and the mass is recorded.
The filter paper is placed inside the Buchner funnel. The paper is moisten with water
so that it fits flush in the bottom of the funnel.
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 7. Once the flask has cooled, 150 mL of saturated sodium chloride (NaCl) solution is
added to the flask to "salt out" the soap.
8. The water is slowly turned onat the aspirator. The mixture is poured from the flask
into the Buchner funnel. Once all of the liquid has filtered through the funnel, the
soap is washed with 10 mL of ice-cold water. The suction filtration is continued until
a1l of the water is removed from the soap.
9. The soap is removed from the funnel and being pressed between two paper towels to
dry it. The filter paper and dried soap are weighted, and the mass is recorded to the
nearest 0.001 and the mass of the soap is determined by difference and record the
mass.

PART B: COMPARISON OF SOAP AND DETERGENT PROPERTIES-

PRECIPITATION AND EMULSIFICATION

1. A stock soap solution is prepared by dissolving 2g of your prepared soap in 100 mL

of boiling, distilled water. The mixture is stirrer until the soap has dissolved and the
solution is allowed to cool.
2. Step 1 is repeated using 2 g of synthetic detergent (Dynamo). When both solutions are
cooled, the pH of each solution is determined using pH paper.
3. Three test tubes are labelled as test tube 1, 2, and 3. 4 drops of mineral oil are added
to each test tube. 5 mL of distilled water is added to test tube 1. 5 mL of stock soap
solution is added to test tube 2. 5 mL of stock synthetic detergent is added to test tube
3.
4. Each of the solution are mixed by shaking and let stand for three to five minutes. Note
which of the solutions, if any, emulsifies the oil by forming a single layer.
5. The mixtures is poured into the Waste Container. The three test tubes is cleaned and
dried.
6. Three test tubes are labelled as test tube 1, 2, and 3. 2 mL of stock soap solution is
placed in each of the three test tubes. 2 mL of 1% CaCl2 solution is added to test tube
1. 2 mL of 1% MgCl2 solution is added to test tube 2. 2 mL of l% FeCl2 solutions
added to test tube 3. Each test tube are shake to mix the solutions. The observations
are recorded.
7. 4 drops of mineral oil is added to each of the test tubes in Step 6. Each test tube are
shake to mix the solutions and let the solutions stand for three five minutes. Note
which of the solutions, if any, emulsifies the oil by forming a single layer.

9
 8. Steps 6-7 are repeated using -2 mL of stock detergent solution. Which solutions form
a precipitate?
9. Note which of the solutions, if any, emulsifies the oil by forming a single layer.
10. The mixtures poured into the Waste Container.
11. 5 ml of stock soap solution is placed in cine clean test tube and 5 rnL of stock
detergent solution in a second test tube. 1 M HC1 is added one drop at a time to both
solutions until the pH in each test tube is equal to 3. (Use pH paper to measure). The
number of drops of acid added to each mixture counted. Does a precipitate form in
either mixture?
12. 1 drops of mineral oil is added to each test tube in Step 11. Each test tube is shake to
mix the solution. Is the oil emulsified in either mixture?

PART C: COMPARISON OF THE CLEANING ABILITIES OF A SOAP AND

DETERGENT.

1. Three beakers are cleaned, dried and labelled. 20 mL of stock soap solution (from
Step 1 in section 3.4.3) is placed in the 1st beaker. 20 mL of stock detergent solution
(from Step 2 in section 6.4.4) is placed in the 2nd beaker. 20 mL of a commercial
liquid Dynamo is placed.
2. Three cloth test strips that have been soaked in tomato sauce is obtained place one
strip is placed in each of the beakers. One cloth strip placed in beaker 1 (from above),
one cloth strip in beaker 2, and one cloth strip in beaker 3. Stir each solution
repeatedly with a stirring rod for 5 minutes.
3. The cloth strips are removed from the soap and detergent solution and the excess
water is squeezed out. Each cloth strip are visually compared to determine their
relative cleanliness. The observations are recorded.

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7. RESULT AND CALCULATIONS
Part A: Soap preparation

Mass of filter paper (g) 0.544 g

Mass of filter paper + soap (g) 46.421 g
Mass of soap recovered (g) 45.877 g
Table 7.1: mass of soap prepared
The mass of soap prepared is 45.877 g

Part B: Comparison of Soap and detergent properties

The pH value of soap and detergent

Brand name of synthetics detergent Dynamo

pH of soap solution 11
pH of synthetics detergent solution 8
Table 7.2; the pH of soap and detergent

Based on the result above, the pH of soap is 11 while the pH of detergent is 8. Thus, the soap
is more basic compared to synthetic detergent dynamo as it has higher pH value.

The emulsification of soap and detergent

Emulsification
System Observation
occurred
Distilled water + 4 2 layer formed. The upper layer is oil
No
drops of mineral oil since oil is less dense than water
2 layer formed. The upper layer is oil
Soap + 4 drops of
since oil is less dense than soap No
mineral oil
solution.
Detergent + 4 drops of The solution became white solution.
Yes
mineral oil Single layers form.
Table 7.3; emulsification of oil in different system.

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Emulsification referred to when the oil droplets are dispersed throughout the water which
form only single layer. From the table 7.3, the oil can only being emulsified by detergent.
While, distilled water and soap do not form any emulsification.

Properties of Soap and Detergent in Hard and Acidic Solution.

2 2 2

Figure 7.1 soap and detergent in hard solution.

Precipitate Oil emulsified

System Detergents Detergents
Soap Soap
dynamo dynamo
Yes, Precipitate
Yes, Oil
2 mL CaCl2 + 4 Yes, White partially
No, pale colour emulsified.
drops of mineral precipitate coagulate. Oil
solution formed Single layer is
oil formed partially
formed
emulsified
No, Precipitate Yes, Oil
2 mL MgCl2 + 4 Yes, Milk white No, pale blue
coagulate. emulsified.
drops of mineral precipitate colour solution
Double layer Single layer is
oil formed formed
formed formed
Yes, Orange Yes, Oil
2 mL FeCl2 + 4 No, yellow
solution with No, Oil layer is emulsified.
drops of mineral colour solution
orange formed. Single layer is
oil formed
precipitate formed
Table 7.4; observations of different system in hard solution.

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From the table 7.4, the soap prepared produces precipitates when reach in hard solution while
detergent does not produces any precipitate. Detergent also good in emulsified oil compared
to the soap prepared. Detergent is better in cleaning than soap as it does not produce any salts
and can breaks down oil molecules.

Detergent Soap

Figure 7.2 soap and detergent in acidic solution.

Sample Soap Detergents

Initial pH 11 8
Final pH 3 3
Number of 1M HCl drops 8 drops 4 drops
Observation The solution turn milky The solution turn colourless

Addition of 1 drop mineral Oil does not emulsified with Oil does emulsified with
oil soap, double layer formed dynamo, single layer formed.

Table 7.5: soap and detergent in acidic solution.

From the table 7.5, we can observe that soap produces white precipitate when reach with
HCI. The soap also cannot emulsify oil even in acidic condition. Detergent does not produce
any precipitate when reach with HCl and it can emulsified oil even in acidic condition.

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Part C: Cleaning Comparison of a soap and detergents

Figure 7.3: cleaning by Figure 7.4: cleaning by Figure 7.5 cleaning by

soap detergents dynamo

Sample Soap Detergents Dynamo Liquid

Cleanliness Slightly clean Very clean Not very clean
Table 7.6 relative cleanliness of soap, detergent and dynamo liquid.

Based on result in table 7.6, detergent show to have the highest relative cleanliness compared
to soap and detergents. Thus, the relative cleanliness as follow:

Detergent (dynamo + water) > Soaps > Dynamo liquid

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8. DISCUSSION
In the saponification process, for preparation of soap in Part A, the fatty acid
carboxylate ions are formed in the presence of the strong base which is used sodium hydroxide,
NaOH for this experiment. Then, these carboxylate ions are the conjugate bases of the fatty
acids therefore, it is able to accept a proton to form the stable compound. When it placed into
water, these conjugate bases are able to accept the proton from any sources including the water.
When triglycerides are reacted with sodium hydroxide, the bond between the oxygen atom of
the carboxylic acid group and the carbon atom of the glycerol is broken. The oxygen atom
picks up the sodium atom from the sodium hydroxide and thus makes this end of the fatty acid
chain soluble in water. The sodium salt of a fatty acid is called soap. The hydroxide group (OH)
from sodium hydroxide then attaches to the glycerol molecule. When all three fatty acids are
removed, the reaction is complete. The presence of ethanol during this process allows the
reaction to take place at medium heat.

In part B, there are several testes had being carried out to determine the properties of
soap and detergent. First, the pH of soap and detergent is measure using pH papers. The soap
has pH value of 11 while pH value of detergent is 8. Soap is the salts of a weak acid.
Consequently, hydrolysis occurs to some extent when soap dissolve in water, which make the
soap solution to be slightly alkaline (basic) and give pH 11 due to partial hydrolysis of the acid.

Next, the ability of soap and detergent to emulsified oil is tested. For the test of
comparison of emulsification of soap and detergent, emulsification occurred only for test in s
detergent, but not in soap and distilled water. Emulsification can be described as the solution
that form is in a single layer. Soaps and detergent have molecular structures which are both
capable of emulsifying or dispersing oils and similar water-insoluble substances. The unique
properties of soap and detergent lie in the fact that one end of the chain is water soluble
(hydrophilic) and the other end is not (hydrophobic). In the process of washing with soap, a
particle of grease is surrounded by soap molecules. The hydrophobic ends attach to the grease
particle, thus leaving the hydrophilic end exposed to the water. This allows the oil particle to
freely move around in the water and emulsified, therefore, be washed away. The oil does not
emulsified in soap for the experiment that had being carried out maybe because the test tube
does not shaken well.

In test 3, the reaction of soap and detergent in hard water in studied. The soap form
precipitate in all of the solutions added which are CaCl2 , MgCl2 and FeCl2 as well emulsifies

15
the oil. So that, this may not appear as a good characteristics for the soap as the cleaning agent
if there formed precipitate and emulsifies oil on the cloth. Furthermore, compare to the
detergent, it is a better cleaning agent because it not formed any precipitate while react with
the mineral that may be contains in the hard water. The sodium and potassium salts of most
carboxylic acids are water soluble. However, the calcium, magnesium, and iron salts are not.
Thus, when soaps are placed in hard water that contains such ions, an insoluble, curdy solid
forms. Most of us have seen these results in the form of a bathtub ring or soap scum floating in
bath or wash water. This process removes soap ions from solution, and decreases the cleaning
effectiveness of soaps. The calcium, magnesium, and iron forms of most detergents are more
soluble in water than the corresponding soap compounds. Consequently, detergents function
almost as well in hard water as they do in soft water.

For part C, the soap and detergent are tested in acidic solution. The precipitate formed
when HCl is added in soap while there no any precipitate in detergent as HCl is added. One of
these is caused by the weak acidity (pKa ca. 4.9) of the fatty acids. Solutions of alkali metal
soaps are slightly alkaline (pH 8 to 11) due to hydrolysis. If the pH of a soap solution is lowered
by acidic contaminants, insoluble fatty acids precipitate and form a scum. The acidic medium
change soaps into carboxylic acid and the action of soap becomes ineffective. Since detergents
are the salts of strong acids they do not decompose in acidic medium. Thus detergents can
effectively clean fabric even if the water is acidic.

Lastly, the relative cleanliness of the soap and detergent is determine as follows:
Detergent (dynamo + water) > Soaps > Dynamo liquid
Detergent is better in cleaning than soap because it can clean in hard water and acidic solution.
While soap have a higher relative cleanliness compared to dynamo liquid because the dynamo
liquid need water which can improve its ability as wetting agents.

16
9. CONCLUSION

By conducting the experiment, we known that we can produce soap using

saponification process. The experiment was successful as its purpose was achieved showing
that a specific brand- Dynamo detergent is a better emulsifying agent, wetting agent and better
cleaning than the soap tested.

From all the test had being tested on soaps and detergent, we can conclude that soap is
alkali that has a higher pH value 11 compared to detergent with pH value of 8. Both soaps and
detergent are soluble in water due to the present of hydrophilic polar end of atomic structure
and hydrophobic tail. This is the factor the emulsification of oil occurred in the test. Detergent
is better cleaning product than soap because it does not produced scum or precipitate when
react in hard water. Soap does not suitable to be used in hard water because the present of
calcium ion, magnesium ion and ferum ions making the soap become insoluble in water.

Other than that, by using soap in hard water, micelles will still occurred due to the
hydrocarbon of the soap structure. Detergent can handle acidic solution because they are salt
of strong acid. But, soap does not suitable to be used in acidic solution because acidic medium
can change soap into carboxylic acid and became ineffective.

For a dynamo liquid to clean effectively, there must be a present of water as an optimum
medium for detergent to do the cleaning process. The relative cleanliness as follow:
Detergent (dynamo + water) > Soaps > Dynamo liquid

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10. RECOMMENDATIONS

Instead of using vegetable oil, why do not we almond oil. Almond oil act as lather
increasing additive which help producing and support a formation of small bunch a tiny bubbles
that can help in removing dirt from cloth. In addition, the sodium hydroxide solution can be
replaced to potassium hydroxide that can produce a different soap.

Then, using pH meter electronic instead of pH paper because pH meter can give a better
and more accurate readings. So the number of HCl solution drops to make the soap and
detergent to became acidic at pH 3 can be more accurate.

Other than that, we can test the cleaning effectiveness of soap by adding some enzymes.
Soap can be as good as detergent but there are limiting as soap can be used in hard water and
acidic solution. But it an enzymes is added to the soap the relative cleanliness can be higher
than soap.

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11. REFERENCE AND APPENDIX

1. Anonymous, The chemical trade journal and Oil, Plant and colour review, Volume 2.
(2010), pp. 383.
2. Frederick A. Bettelheim, William H. Brown , Mary K. Campbell, Introduction to
General Organic and Biochemistry. 10 (2015), pp.300
3. Frederick A. Bettelheim, William H. Brown , Mary K. Campbell, Introduction to
Organic and Biochemistry. (2012), pp.223
4. David W. Oxtoby, H. P. Gillis, Norman H. Nachtrieb. Principle of Modern Chemistry
(2002), pp.773
6. American Cleaning Institute
http://www.cleaninginstitute.org/clean_living/soaps__detergents_chemistry.aspx

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