CHE150L

Experiment No. 3: Saponification

Alaraz, Adrian; Barbastro, Shanlaine; Capanayan, Carlos Miguel;

Espiel, Jericho; Francisco, Kian James; Quicay, Cedric John

I. Introduction

During the process of saponification, a fat molecule is broken down by sodium hydroxide (lye) into
four smaller molecules. Out of these four molecules, three of them are soap and one is glycerol. To put it
simply, saponification refers to the chemical reaction that takes place when an acid and a base combine to
form a salt. In this reaction, a base is a substance that provides electrons or hydroxide ions (OH-) and/or
accepts protons, while an acid is any molecule or ion that donates protons or hydrogen ions (H+) and/or
accepts electrons. To create soap, one must mix an acid oil or fat with a basic substance, such as sodium
hydroxide or lye, resulting in the formation of a salt known as soap. Various types of acids can undergo
saponification when they come into contact with bases. Examples of acid include olive oil, coconut oil, and
vegetable oil. Triglycerides, defined as molecules comprising three fatty acids connected to a glycerol
molecule, possess distinct properties for each acid and interact in different ways with the base (sodium
hydroxide or lye) (Fakai et al., 2014).

The distinctive molecular structure of soap makes it capable of emulsifying fats and oils. With their
nonpolar tails embedded in the oil and their charged "head" groups towards the surrounding water, soap
molecules form micelles around oil droplets. Grease and filth can be more easily washed away thanks to
this technique, which enables tiny oil droplets to disperse in water. Using hot water, which can melt solid
fats, and agitation, which disperses fats and oils into smaller droplets, improves the efficacy of soap.
However, soap is less effective in hard water that contains magnesium and calcium ions because these ions
combine with soap molecules to produce precipitates that result in "soap scum." Since soap precipitates
when exposed to these ions, the solution no longer contains many soap molecules. As a result, soap won't
produce as many bubbles in hard water. Water that has extremely few or no ions that precipitate with
washing is referred to as "soft water". As a result, soap will work considerably better in soft water than in
hard water. While detergents and soaps both feature a charged head group and a lengthy, nonpolar tail
group, detergents are not made from organic fats or oils. Since detergents don't precipitate out with calcium
or magnesium ions, they can be used in both soft and hard water (Spitz, 2009).

After completing the experiment, students will have the abilities and information required to create two
different types of soap: bath soap and liquid hand soap. They will have a greater comprehension of the
saponification process as well as the capacity to produce useful and efficient cleaning agents thanks to this
practical experience. In addition, students will be able to compare the qualities of the soap they make to
those of a soap and detergent that is sold commercially. By comparing their handmade soap to regularly
used commercial items, students will be able to assess the effectiveness, lathering potential, aroma, and
other critical qualities of their homemade soap, deepening their understanding of the chemistry of soap and
product evaluation.

II. Methodology

Table 1. List of materials and chemicals used to make liquid soap.

Materials List of Chemicals

Test Tube (3 Pieces) Sodium Dodecyl Sulfate (SDS)
100 ml Graduated Cylinder Coco Diethanolamide (CDEA)
Stirring Rods (2 Pieces) Sodium Chloride
400 ml beaker Citric Acid
50 ml beaker (3 pieces) Perfume
140 ml beaker Glycerin
Test Tube Rack Triclosan
Yakult Cups (2 Pieces) Distilled Water
Povidone-Iodine
Colorant
 Table 1 shows the list of materials and chemicals needed to create liquid soap from scratch.

The first step of making liquid hand soap is to pour about 20 grams of Sodium Dodecyl Sulfate
(SDS) into a 400 ml beaker. 220 ml of distilled water was measured using a graduated cylinder. It was
poured and mixed with the SDS using a stirring rod until it dissipates completely (Figure 2).

Figure 1. Beaker with SDS and Distilled Water. Figure 2. Stirring the beaker to mix the solution.

Then, 5 ml of CDEA is added to the solution and mixed lightly to prevent any formation of bubbles
(Figure 3). Then the 2.5 ml of glycerin and 0.25 g of triclosan were mixed in a separate 15-ml beaker (Figure
4).

Figure 3. Stirring the beaker to mix the solution. Figure 4. Mixing of glycerin and triclosan
 Next step that had done was combining the glycerin and triclosan mixture into the SDS solution
and mixed thoroughly. Now that the preceding tasks have been successfully completed, the next phase
involves introducing color and fragrance. To add a personal touch and enhance the visual appeal of the
liquid soap, food coloring is employed to tint the solution. During this stage, the experimenters have the
creative freedom to choose any color or combination of colors for the process. Once the colorant has been
mixed in thoroughly, 1 mL of perfume is introduced to the solution and blended thoroughly as well. In this
case, the group decided to add some lemon perfume and orange colorant (Figure 5).

Figure 5. The lemon perfume and orange colorant added in the solution.

Afterwards, 0.125 grams of citric acid was added slowly along with 5 grams of sodium chloride
(Figure 6). This ensures that the liquid soap will have a pH of 7 to 8 and makes the liquid soap more viscous.
The solution was then stored into a bottle container.
 Figure 6. Adding the citric acid and sodium chloride into the solution.

To determine the properties of the liquid soap, a comparison was made between commercial liquid
detergent, commercial hard soap, and freshly made liquid soap in terms of their pH, cleansing ability, and
how they behaved in acidic and hard water.

Liquid Soap Properties Determination

First, three beakers were used, and each soap was labeled for each beaker. One gram of each soap
was added to each beaker, followed by the addition of 50 ml of distilled water (Figure 7).

Figure 7. Samples of each soap were commercial detergent (left), commercial soap (center), and freshly
made soap (right) in 50-ml distilled water.
 Second, the pH was determined. pH paper was used for each of the three soap solutions to
establish whether they were acidic or basic (Figure 8).

Figure 8. Using a pH paper for freshly made soap.

Third, each of the soap solutions was tested for its cleansing ability by employing Povidone-Iodine
(preferably a 10% solution) to determine its effectiveness in removing Iodine from the cheesecloths. The
process also involved counting the number of rubs required to determine which soap was more efficient at
cleaning the Iodine (Figure 9).

Figure 9. Putting Povidone-Iodine in three cheesecloths.

 Lastly, the behavior of each of the soap solutions when in contact with acidic water was
examined. Each soap solution was placed in a separate test tube at a volume of 10 ml (Figure 10).
Subsequently, five drops of 3M HCl were added to each test tube, and any changes in color, pH, etc.,
were observed. Afterward, the test tubes were drained, and the test was repeated to observe the separation
of the oil from the soap (Figure 11).

Figure 10. Addition of 5 drops of 3M HCl to each test tube.

Figure 11. Addition of oil to each test tube

III. Results and Discussion

 In the process of making soap, there are typically two distinct layers that become visible: the upper
layer, referred to as the "soap phase," and the lower layer, known as the "water phase." The upper layer
generally comprises a mixture of Sodium Dodecyl Sulfate (SDS), water, and other components. In contrast,
the lower layer primarily consists of water and other water-soluble ingredients like glycerin, fragrances,
and various additives. This separation into two layers occurs due to the varying solubility of each
component within the solution. Liquid hand soap formulations encompass a wide range of ingredients,
some of which can readily dissolve in water, while others cannot. The surfactant employed, namely Sodium
Dodecyl Sulfate (SDS), tends not to be soluble in water, resulting in its tendency to form a distinct phase.
Conversely, ingredients such as glycerin, fragrances, colorants, and other additives dissolve easily in the
water phase. The observed separation arises as a consequence of these ingredients grouping together based
on their respective solubility characteristics.

In a typical liquid hand soap solution, the primary surfactant and ingredients used does not have a
strong or distinct odor. The sodium dodecyl sulfate (SDS) and similar surfactants are typically odorless and
another main component of the solution, which is water, is also odorless. Any fragrance or scent in the soap
solution comes from the addition of fragrance or perfume compounds. Manufacturers often include specific
fragrances to make the soap more appealing and enjoyable for uses. In the experiment, the fragrance added
has a citrus-scent similar to the smell of lemon extracts. This is one of the common scents used or added to
soap solutions.

Both Cocodiethanolamine (CDEA) and Sodium Dodecyl Sulfate (SDS) are surfactants. During the
addition of CDEA to SDS, the appearance became cloudy and eventually gave a foamy white solution. This
foamy solution is caused by CDEA since it is a foaming agent. As the solution was stirred continuously,
the viscosity of the solution increases. This increase in viscosity is due to the reaction of CDEA to SDS,
which leads to the formation of amides. As it was further stirred, the solution turned from a white cloudy
solution to a slightly cloudy solution but remained foamy at the top.

According to Statzak et al. (2015), shampoos and conditioners containing sodium lauryl sulfate use
sodium chloride as a thickening agent. The soap that forms during saponification stays in suspension in the
mixture. By incorporating common salt into the suspension, it precipitates as a solid. It is known as salting
out of soap. This salting out technique helps to isolate the soap portion of the mixture and remove impurities.
Goel et al (2017), also stated the sodium chloride is also used as an antimicrobial agent. This could mean
that Sodium chloride could contribute to the increase of the shelf life of the soap since it makes it less
conductive of microbial growth. Triclosan is used as a biocide to eliminate antimicrobial growth within the
liquid soap (Giuliano & Rybak, 2015)

Table 2. pH of the soaps

SOLUTION pH BASIC/ACIDIC
Your soap 8 Basic
Commercial soap 5 Acid
Commercial detergent 10 Basic

Table 3. Cleansing Ability of each soap

Times it took to wash off the

SOLUTION OBSERVATIONS
Iodine
Lathering ability, silky or slimy 30
Your soap
feeling, moisturizing
Slimy feeling, but not lather 54
Commercial soap
well
High lathering-ability, drying on 27
Commercial detergent
the skin

Distilled water Neutral, does not deeply cleanse

Testing the pH level is crucial to determine if soap is suitable for skin use. Typically, handmade
soaps fall within the alkaline range, with a safe pH range of 10 to 8 for skin application. A pH exceeding
11 is excessively harsh and can lead to skin irritation, while anything below pH 8 isn't feasible for handmade
soaps as it compromises cleansing efficacy. In the table provided above, the soap created in the experiment
registers a pH of 8, indicating its skin safety and moisturizing properties. Conversely, the commercial soap
(dishwashing liquid soap) has a pH of 5, making it acidic, resulting in suboptimal lathering and rinse-off.
The commercial detergent, boasting a pH of 10, falls on the basic side, ensuring skin safety, robust cleansing
capabilities, and abundant lather, but it can have a drying effect on the skin.
 The cleansing efficacy of soaps is compromised in acidic solutions since they undergo a change
where long chain fatty acids are formed. In acidic conditions, soap salts do not readily break down into their
constituent ions, rendering them inefficient as cleaning agents.

Soap and detergents possess an amphiphilic or amphipathic character, which greatly enhances their
cleaning efficacy. The hydrophilic segment of these molecules exhibits an affinity for water. In soap, this
hydrophilic head predominantly consists of the carboxylate group (-COO-), while in synthetic detergents,
it can exhibit variability but often incorporates sulfonate or sulfate groups (-SO3- or -OSO3-). This
hydrophilic head facilitates the dissolution and interaction of soap and detergents with water.

Conversely, the hydrophobic segment of these molecules is water-repellent but has an attraction to
oils and grease. Typically, in both soaps and detergents, this is represented by an elongated hydrocarbon
chain, which may be derived from fatty acids in the case of soap or be synthetically formulated in the
context of detergents. The hydrophobic tail plays a pivotal role in binding to and dissolving oily or greasy
substances.

The combination of these two structural features empowers soap and detergents to function as
potent cleaning agents. In aqueous environments, they give rise to micelles—collections of soap or
detergent molecules. The hydrophilic heads extend outward, establishing interactions with water, while the
hydrophobic tails face inward, encapsulating and dissolving oily or greasy materials. This micellar
arrangement enables soap and detergents to emulsify oils and greases, breaking them down into smaller
droplets that can be suspended in the water and subsequently removed. This inherent property underlies
why soap and detergents are highly effective at eliminating impurities, oils, and various contaminants from
diverse surfaces, including skin and clothing.

Table 4. Reactions in acidic water

OBSERVATIONS AFTER 5
SOLUTION INITIAL OBSERVATIONS
MINUTES
Clear at the bottom, cloudy at
Clear solution, minimal
the center with high lathering at
Your soap lathering at the top
the top
 Clear solution with high
Clear solution with moderate
Commercial soap lathering at the top
lathering at the top

Cloudy all thought out with high

Cloudy with moderate lathering
Commercial detergent lathering at the top
at the top

Table 5. Reactions in hard water

SOLUTION HARD / TAP WATER

Clear at the bottom, cloudy at the center with high
Initial lathering at the top
Your soap

After 5 min
Clear solution, moderate lathering at the top
Clear solution with moderate lathering at the top
Initial
Commercial soap
After 5 min Clear solution with less lathering at the top
Cloudy all thought out with high lathering at the
Initial top
Commercial detergent

After 5 min Cloudy with moderate lathering at the top

Hand washing with soap and water is regarded as a personal hygiene practice whereas, a detergent
is a synthetic surfactant, a chemical substance that cleans. A detergent contains one or more surfactants,
making it an efficient cleaning agent. The surfactants used in detergents can be designed to function well
in a range of situations due to their chemical makeup (Bhat et al. 2011). A combination of sodium/potassium
salts of long-chain fatty acids, produced by the hydrolysis of animal fat and alkali, compose the chemical
makeup of soap. In the experiment, lye or sodium chloride was used and vegetable oil for the saponification
process of liquid hand soap. Soap is generally biodegradable & environmentally friendly, breaking down
into harmless substances in the environment. Detergents on the other hand, vary depending on the specific
surfactant used. Some detergents are biodegradable, while others are less so. Biodegradability is an
important consideration for environmentally friendly detergents. Soap is found to be milder on the skin,
making it suitable for personal care products like hand soaps and body washes. Detergents are complete,
causing harsh effects on skin hence it is not suitable for frequent hand washing. As a result, both soaps and
detergents are different when it comes to commercial use. While soap is used in personal care products and
certain cleaning applications, its use is limited in detergents for laundry and dishwashing. Detergents are
versatile and widely used in various cleaning applications, including laundry detergents, dishwashing
detergents, surface cleaners, and industrial cleaning products.

Detergents have significant environmental consequences, most notably water pollution from
surfactants, eutrophication from phosphates, and the potential for non-biodegradable detergents to persist
in ecosystems. The detergent components can enter the soil and water bodies from different sources.
Eutrophication, foaming, and altering parameters such as temperature, salinity, turbidity, and pH are more
important, and their effects need to be managed and controlled. The presence of microplastics in some
formulations further compounds the problem, with potential harm to aquatic life. The production and
packaging of detergents consume energy and contribute to plastic waste. Additionally, the use of harmful
chemicals in some detergents poses risks to the environment. Production of environment-friendly detergent
is an important issue around the world (Mousavi & Khodadoost, 2019).

IV. Conclusion

In conclusion, this lab experiment allowed the group to gain a deeper understanding of the
saponification process and the chemistry of soap. Through hands-on experience, they created a liquid hand
soap, and compared it with commercial soap and detergent soap. The results and observations from the
experiment revealed several important aspects of soap and detergent chemistry. The pH measurements
indicated that the produced liquid hand soap which has a pH of 8 and is close to neutral, falls within the
safe range for skin application, emphasizing its skin-friendly and moisturizing properties. On the other
hand, commercial soap and detergent exhibited varying pH levels 5 (acidic) and 10 (basic) respectively,
with implications for their effectiveness and potential drying effects on the skin. The experiment also
demonstrated the significance of water characteristics. In both acidic and hard water conditions, the
reactions in the soap and detergent solutions resulted in changes in appearance and lathering ability,
underlining the importance of water quality in cleaning effectiveness. Comparing the cleansing abilities of
the liquid hand soap, commercial soap, and commercial detergent highlighted the unique qualities of each
product. The produced liquid soap displayed lathering ability, a silky or slimy feeling, and moisturizing
properties, emphasizing its suitability for personal care. In contrast, the commercial soap and detergent had
their distinct characteristics, including slimy texture, lathering, and dry skin effects.
Moreover, the discussion shed light on the fundamental structural features of soap and detergents,
such as their amphiphilic nature, which allows them to effectively emulsify oils and grease, a crucial
property for cleaning agents. The report also underscored the differences between soap and detergents,
including their compositions, biodegradability, skin-friendliness, and applications. While soap is milder,
biodegradable, and suitable for personal care, detergents are versatile but can have environmental
consequences.
Overall, this lab experiment deepened the groups' understanding of the chemistry of the
saponification process. It provided valuable insights into the creation, characteristics, and applications of
soap and detergent, offering a practical application of chemical principles in everyday products.

V. References

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Bhat R; Prajna; Menezez V and,;Pavithra S. (2011) Antimicrobial Activities of Soap and

Detergents. Society of Education, INDIA. Retrieved from: [Link]

Fakai, I. M., [Link], [Link]-Yauri, & Musa. (2014). Production of Soap Using Locally
Available Alkaline Extract from Millet Stalk: A Study on Physical and Chemical Properties of Soap.
International Journal of Advanced Research in Chemical Science, 1(7), 1–7.
[Link]

Goel G.; Bhattacharya. S; Chandy M (2017). Soaps and infection control: From chemistry to
microbiology. Journal of the Academy of Clinical Microbiologists. doi: 10.4103/jacm.jacm_1_17

Giuliano, C. A., & Rybak, M. J. (2015). Efficacy of Triclosan as an Antimicrobial Hand Soap
and Its Potential Impact on Antimicrobial Resistance: A Focused Review. Pharmacotherapy: The
Journal of Human Pharmacology and Drug Therapy, 35(3), 328–336. doi:10.1002/phar.1553

Mousavi, S. A., & Khodadoost, F. (2019). Effects of detergents on natural ecosystems and
wastewater treatment processes: a review. Environmental Science and Pollution Research, 26(26), 26439–
26448. [Link]

Spitz, L. (2009). Soap Manufacturing Technology. [Link]

 Staszak, Katarzyna; Wieczorek, Daria; Michocka, Katarzyna (2015). Effect of Sodium Chloride
on the Surface and Wetting Properties of Aqueous Solutions of Cocamidopropyl Betaine. Journal of
Surfactants and Detergents, 18(2), 321–328. doi:10.1007/s11743-014-1644-8