Experiment 3 : Lab Scale Soap Production

OBJECTIVES

The objectives of this experiment were:

The weight of materials to be used in the formulation of soap were calculated.

The soap bar with an average quality was produced by using basic formulations from
palm oil.

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 Experiment 3 : Lab Scale Soap Production

SUMMARY & FLOWCHART

As a summary, this experiment was conducted for the production of soap in a lab scale.
The objectives for this experiment were the weight of materials to be used in the formulation
of soap were calculated and the soap bar with an average quality was produced by using basic
formulations from palm oil. In the lab, experimenters were briefly explained by the lab
technician, about the theory of making the soap and the preparation for the ingredients. The
formulation of making soap was briefed to the experimenters. Next, the experimenter
prepared the ingredients needed for making soap such as the oil, sodium hydroxide (NaOH),
salt or also known as sodium chloride (NaCl) and ethylene diamine tetra acetatic acid (EDTA)
0.1%. The experimenters first need to calculate the ingredients weight. Then, the experimental
procedure was carried out for the production of soap. Some of the samples were put into the
molds, and the balances were used for the analysis. The analysis was to carried out the
saponification values (SV), and the % moisture content. From the experimental result for SV,
the produced soaps show that a higher value compared to the theoretically. The SV calculated
shows that the produced soap is not suitable to use for skin. Generally, saponification value
shows the length of carbon chain of the acid present in particular oil and fat. Therefore, the
higher the saponification value, the shorter the chain acid present in oil and fats caused the
percentage of the soap production is lower. This can be concluded that the saponification
value is not valid to use for soap production. For the experimental result of % moisture
content, the average of moisture content value is 4.98%. Theoretically moisture content of
soap production must be in range of 9 to 15% to get the desired quality of soap. This shows
average of moisture content in experimentally is not achieving the desired quality.

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 Experiment 3 : Lab Scale Soap Production

Ingredients such as NaOH, salt and EDtA were prepared after the weight were calculated

Ensure the blended oil done heated to 70-80⁰C

The ingredients were poured half in volume every 3-5 minutes each into the blended oil

Poured the balanced ingredient with 3-5 minutes period each into the blended oil

The colour was poured

Mixed them well

Poured into the molds Analysis

Let cooled pH value

Stamping Saponification Value

Soap production % Moisture Content

Figure 1 shows the flowchart in lab scale soap production experiment.

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 Experiment 3 : Lab Scale Soap Production

INTRODUCTION/THEORY

Saponification is the reaction from mixing the oils with an alkaline base such as Sodium
Hydroxide (NaOH) or Potassium Hydroxide (KOH). Oils are most important component of
the soap making process, and without oil (or fatty acids of oils) the saponification reaction
cannot take place. In general, oils that are great for cleaning produce a harder bar but are not
that moisturizing, while moisturizing oils produce softer bars and do not clean as well. Each
oil requires a different amount of base to react completely and can be looked up in a
saponification table. Reaction below are the typical reaction of soap.

Figure 2 shows the typical reaction of soap

According to Bruice (2007) these fats and oils are called triglycerides. In fact, a single
triglyceride molecule in a fat may contain three different acid residues (R1COOH, R2COOH,
R3COOH), and not every triglyceride in the substance will be identical. Each fat or oil has a
characteristic statistical distribution of the various types of acids possible. These fatty acids
can be ‘Saturated’ or ‘Unsaturated’ and each fatty acid or oil has different properties and
benefits that contribute to the finished product. Saturated oils or fatty acids tend to be solid at
room temperature, such as Coconut Oil and Palm Oil. According to John & McMurry (1988)
these types of oils contain Lauric Acid, Myristic Acid, Palmitic Acid and Stearic Acid. They
are likely to make a harder and higher-lather cleansing soap bar. Unsaturated fatty acids or

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 Experiment 3 : Lab Scale Soap Production

oils tend to be liquid at room temperature and have a lower melting point than saturated fatty
acids. These oils include Olive Oil and Sunflower Oil.

Next, according to the David R. Klein (1995) the unsaturated fatty acids that are
present to a high degree in these oils are oleic and linoleic acid which contributes to a softer
finished product. In this experiment, the oils used are helianthus annuus (sunflower) seed oil
and elaeis guineensis (palm) oil. Palm oil is made up of palmitic acid, oleic acid and linoleic
acid, amongst other fatty acids at lower levels. The palmitic acid fraction of the oil provides
some hardness to the soaps when saponified, and the oleic and linoleic acid provide softness.
Once saponified, palm oil produces ‘sodium palmate’ when reacted with sodium hydroxide.
Liquid soaps are not often produced using palm oil. Other than that, sunflower oil is a widely
used liquid unsaturated vegetable-derived oil. This oil contains oleic and linoleic acid, which
makes it a very fluid ingredient, but is not often used as a single ingredient in soap as it does
not provide enough foam. For example, coconut oil and sunflower oil make up our organic
liquid Castile. The coconut oil provides the foaming properties when saponified, and the
unsaturated sunflower oil aids in producing a clear, liquid soap when reacted with potassium
hydroxide.

Last but not least, the pH of each soap must be check before the soap are sale as
commercial product This is to make sure that the soap are safe to each users and to avoid any
serious sickness to occur. There are many ways to test the pH value of the soap such as by
using phenolphthalein and pH metre. The test range for phenolphthalein is pH 8 until pH10,
changing from colourless to a deep pink. Colourless to light pink is fine. The more intense the
pink, the more basic it is. A soap that gives a deep pink colour may be an indication of an
erroneous measurement or non-uniform mixture. A soap giving a deep pink colour could be
dangerous. Verify the pH using a pH meter. Soaps with a pH more than 10 can be irritating to
the skin depending on skin type. Soaps with a pH more than 11 should not be used on the
skin. They can be grated and used as laundry soap which generally has a pH of 10 until pH
12.

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 Experiment 3 : Lab Scale Soap Production

RESULT, ANALYSIS AND DISCUSSION

This experiment has been carrying out with several objectives. First objective is to
calculate weights of materials to be used in the formulation of soap and another one is to
produce average quality of soap bar using basic formulations from palm oil.

Table 1: Formulation of Soap

Materials Weight (g)

RBDPO 700
Sunflower oil 300
NaOH 120 (mL)
NaCl 24
EDTA 2.4

From table 1 above, five materials such as Refined Bleached Deodorized Palm Oil
(RBDPO), sunflower oil, sodium hydroxide (NaOH), sodium chloride (NaCl), and 0.1% of
Ethylene diamine tetra acetatic acid (EDTA) has been added by different formulation to
produce soap. RBDPO is function as soap thickener. Therefore, weight of RBDPO is higher
than other materials. Sunflower oil is used in soap recipes gives stable lather, conditioning and
silky feel of soap. Only 300 grams of sunflower oil are used in making soap because if more
sunflower oil is utilized, it will create a very soft soap. 120 mL of NaOH solution is used in
making soap to create lye solution. When NaOH is added, the solution turns cloudy. Lye
solution will mixed with fats and oils and undergo saponification process to produce soap.
Other ingredient is NaCl which function to higher the solidity of soap. Another ingredient is
EDTA. 2.4 mL of EDTA is used in making soap to reduce moisture of soap. Less content of
EDTA may cause brittle soap. From the objective above, it is important to weight every type
of the material using basic formulations of palm oil to produce a good quality of soap.

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 Experiment 3 : Lab Scale Soap Production

Table 2: Result of Analysis

Analysis Sample 1 Sample 2 Sample 3 Average

pH value 11 10 11 11
Saponification value 152.75 164.09 157.08 157.97
Moisture content 5.29 4.96 4.69 4.98
(%)

Another objective in this experiment is to study the process of lab scale soap
production by determining pH value, saponification value and moisture content of soap.
Basically, this experiment undergoes cold process. Based on the theory, pH for cold process
soap is 9 to 10 and naturally alkali. (Google.com, 2017) Between this pH, the soap can gently
help to clean the skin. From the result that has been carried out, the average of pH value of
soap is 11. Therefore, in terms of pH value, this experiment is not successfully carried out
because of the pH value of soap is not suitable for skin. It is because, due to the procedure, the
correct time to test the pH value is after two weeks. It is to ensure that the soap is cured first
before taking the pH value. Another reason why pH value higher is because too much lye is
used and effect less of oil used to turns it into soap. Increasing pH level will irritate and burn
the skin. The production of soap is not suitable to use for skin.

In this experiment, saponification value has been determined. Saponification value is

defined as a measure of the total of acid which expressed as the number of weight of sodium
hydroxide required completing the saponification process in a one gram of fat. Theoretically,
saponification value for palm oil is 142 which are the characteristics of soap is hard, great
cleansing, no fluffy lather, stable lather, and great skin care. (Inquiry et al., 2017) Compared
to the experimental result, there are three sample of saponification value that has been taken
and the average for saponification value is 157.97. This experimental result give a higher
value compared to the theoretically and this proved that based on the experimental data, the
saponification value shows that soap is not suitable to use for skin. Generally, saponification
value shows the length of carbon chain of the acid present in particular oil and fat. Therefore,
the higher the saponification value, the shorter the chain acid present in oil and fats caused the
percentage of the soap production is lower. This can be concluded that the saponification
value is not valid to use for soap production.

Moisture content value in soap production was determined to measure the quantity of
water contained in soap. High moisture content in soap can lead of excess water and
hydrolysis of soap between fatty acid and soap is occurred. Theoretically moisture content of

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 Experiment 3 : Lab Scale Soap Production

soap production must be in range of 9 to 15% to get the desired quality of soap. (Soap-
Making-Essentials.com, 2017) But in experimentally, the average of moisture content value is
4.98%. This shows average of moisture content in experimentally is not enough to achieve the
desired quality of soap because water is used to dissolve lye crystal. Low of moisture content
means soap has higher alkali. If less water is used in making soap, lye will fall out the water
solution of the solution and lye will not dissolve properly which exposed to hard white flakes
of moisture.

CONCLUSION

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 Experiment 3 : Lab Scale Soap Production

As a conclusion, for the SV result calculated shows that, the soap is not suitable to
apply on the skin due to the average of pH value of soap is 11 and the average for
saponification value soap is 157.97 which is more than the exact value of saponification of
palm oil which is 142. This experimental result give a higher value compared to the
theoretically and this proved that based on the experimental data, the saponification value
shows that soap is not suitable to use for skin. Generally, saponification value shows the
length of carbon chain of the acid present in particular oil and fat. Therefore, the higher the
saponification value, the shorter the chain acid present in oil and fats caused the percentage of
the soap production is lower. This can be concluded that the saponification value is not valid
to use for soap production. While for % moiture content, the average of moisture content
value is 4.98%. Theoretically moisture content of soap production must be in range of 9 to
15% to get the desired quality of soap. (Soap-Making-Essentials.com, 2017). This shows
average of moisture content in experimentally is not enough to achieve the desired quality.

RECOMMENDATION

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 Experiment 3 : Lab Scale Soap Production

In this experiment, there were several errors occur and there are future recommendation
for these problems. Firstly, problem occurring while running the moisture content analysis,
the petri dishes were held by hand without gloves or in other say was handle appropriately by
the experimenter. To avoid the moisture contents get contaminated from the hands effect, the
gloves must be wore while holding the petri dishes. Secondly, do not use aluminum foil
because it will react with your base and release hydrogen gas. When NaOH is dissolved in
water, a lot of heat is given off. This solution may become very hot and to prevent from skin
burning the gloves must be wore while handling the sodium hydroxide solution. Last but not
least, experimenter should use appropriate PPE while handling the chemical and apparatus in
laboratory. This can also ensure the safety towards the experimenter and the result taken can
be obtained precisely without being interrupted by the contamination.

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 Experiment 3 : Lab Scale Soap Production

APPENDIXES

Blended Melted Oil The Ingredients EDTA, Salt, NaOH

Blended Oil after mixed with ingredients Stamping

Cooled and cut into pieces before stamping Successful soap stamping

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 Experiment 3 : Lab Scale Soap Production

Samples mixed with water to test pH pH test

Titration for SV analysis Moisture content analysis

Moisture content samples analysis Team members with successful soap produced

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 Experiment 3 : Lab Scale Soap Production

Sample Formula for calculation

56.10 × M (V 0−V t)
SV =
m
mb−md
% Moisture and volatile matter = ×100%
mb−m

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 Experiment 3 : Lab Scale Soap Production

REFERENCES

1. Bruice,Paula Y.,1998,Organic Chemistry, 2nd Edition, journal of Chemical

Education, vol.75 (11), page 1390,DOI: 10.1021/ed075p1390.

2. J.,McMurr,1988, Fundamental of Organic Chemistry,Third Edition, 65 (8), page 720.

3. David R. Klein,1995,Organic Chemistry,vol.56, page 552.

4. Google.com. (2017). Cite a Website - Cite This For Me. [online] Available at:
https://www.google.com/url?
sa=t&rct=j&q=&esrc=s&source=web&cd=1&cad=rja&uact=8&ved=0ahUKEwjF4sj80szXA
hWCH5QKHR_tA3oQFggqMAA&url=http%3A%2F%2Fwww.soap-making-resource.com
%2Fsaponification-table.html&usg=AOvVaw2ZLEw6g3h5bNDHLJo_p509 [Accessed 20
Nov. 2017].

5. Inquiry, P., plus, g., Fizzies, B., Soap, C., Crafts, H., Products, L., Soap, M., Scrubs, S.,
Tricks, T., Cuisine, S., TV, S., News, B., Musings, B., Ramblings, P., Ramirez, Y., Masciarelli,
J., Ramirez, Y. and Bradford, S. (2017). How to Test pH with Red Cabbage - Soap Queen.
[online] Soap Queen. Available at: https://www.soapqueen.com/bath-and-body-tutorials/tips-
and-tricks/test-ph-red-cabbage/ [Accessed 20 Nov. 2017].

6. Soap-Making-Essentials.com. (2017). Determining water content of a soap recipe. [online]

Available at: http://www.soap-making-essentials.com/determining-water-content-of-a-soap-
recipe.html [Accessed 20 Nov. 2017].

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