OBJECTIVES

The objectives of this experiment are:

• To calculate weights of the materials to be used in the formulation of soap

• To produce average quality of soap bar using basic formulation from palm oil

SUMMARY

The objective of this experiment is to calculate weights of the materials to be used in the
formulation of soap and to produce average quality of soap bar using basic formulation from
palm oil. In this experiment, the procedure is divided in three part where the first part is the
preparation of ingredients. The second part is the experimental analysis where the sample were
tested on the pH value and saponification value. The last part for the procedure was measuring
the moisture content of the sample. From the result of the experiment, the pH value of the soap
is 11.8 which means it is an alkaline, therefore it is not an acceptable pH value for a soap as
the general pH value for soap production is between 7 until 10. Next, the saponification value
of the soap is 0.142. Then, the average moisture content of the soap is 16.8%. The standard
moisture range of the unit is 0.0 to 17.0. The moisture content obtained from the experiment
are in the range. In a conclusion, the objective of the experiment was achieved but there is a
room of improvement in the pH value as it is unacceptable for its high value of alkalinity. Few
steps can be improved in this experiment in order to achieve the best result.
METHODOLOGY

Preparation of ingredients

The ingredients that have been used in this experiment are listed as below:

• Refined Bleached Deodorized Palm Oil (RBDPO)

• Sunflower oil
• Sodium Hydroxide (NaOH)
• Sodium Chloride (NaCl)
• 0.1% Ethylene Diamine Tetra Acetatic Acid (EDTA)
• Water
Experimental Procedures

The blended oil was melted in the water bath at 70-80°C

The reactor was turned on and pre-heat for about 5 minutes

Next, the blended oil is added into the mixer and mixed for 10 minutes

Then, addhalf
Then, the of
remaining
the NaOHof solution
NaOH, NaCl and EDTA
is slowly addedinto
andthe mixer
half and
of the let is
NaCl it added
for 20 minutes
into the for
the reaction to take place.
solution after 10 minutes of adding NaOH solution.

Next, half of EDTA is added into the mixer.

After the solution seems homogenous, the solution is placed in the flat plate and let the
solution solidify become semi solid

The semi-solid soap is then cut into piece and stamped (covered with tissue) by using a
stamper to form the shape including the name of company on it.
Experimental Analysis

1. pH Value
The pH value of the soap bar is decided by using the pH paper while the value is
recorded in the results table.

2. Saponification Value

Apparatus
• Conical flask
• Reflux condenser
• Hot plate
• Burette, 50 mL capacity
• Pipette, 25 mL capacity

Solutions

• Hydrochloric acid, 0.5 M

• Potassium Hydroxide (KOH), 0.5 M solution
• Phenolphthalein indicator solution
• Boiling aid, fat free
 Analysis Procedure

2 g of the test sample is weighed to the nearest 5 mg into a conical flask

About 25 ml of ethanolic potassium hydroxide is added. The reflux condenser that joint to
the flask was placed in the heating device for it to be boiled slowly and shaken for 60
minutes or 2 hours might be possible because of high melting point.

2 to 3 drops of phenolphthalein indicator are added into the hot solution before being
titrated with the standard volumetric hydrochloric acid solution. The titration is made until
the pink colour of the indicator just disappeared.

The titration for the blank test also been carried out by using 25 mL of ethanolic potassium
hydroxide solution, omitting the test portion.

All data are recorded in the results table.

Results Calculations Formula

Saponification Value (SV) =

Where;

M = Molarity of standardized HCl solution

V0 = Volume of titrant of blank (mL)

Vt = Volume of titrant of test sample (mL)

M = mass of test portion (g)

Moisture Content

Apparatus

• Air oven
• Analytical balance
• Petri dishes
• Desicator

Analysis Procedures

Dry clean petri dishes are heated inside an oven at 103 ⁰C for 15 minutes and are
cooled inside desiccators. The dishes are weighed, to the nearest 0.001 g.

The sample is weighed to approximately 10 g into the dish and is returned to the
desiccators until the oil has thoroughly cooled. The dish plus oil are weighed and
placed in the middle shelf of the oven at 103°C for 2.5 hr.

The dish is removed and let to be cooled at room temperature in the desiccators (30 to
45 mins) before being reweighed to the nearest 0.001 g.

If the moisture content exceeds 0.3%, the dishes are being reheated inside the oven for an
interval of 30 minutes until their moisture content is below 0.3%.

All data are recorded in the results table.

Results Calculations Formula

% Moisture and volatile matter = x 100%

Where;

m = mass of the dish (g)

mb = mass of the dish and test sample (g)

md = mass of the dish and test sample after drying (g)

INTRODUCTION

The soap is basically known for cleansing and lubricating products. Generally, it is
known of carboxylate salts consists with very long hydrocarbon chains. Basically, it can be
made from the base hydrolysis of fat or oil. The soap was made as surfactants purposely for
washing, bathing and cleaning. Back in ancient Roman, the tradition called the ‘Saponification’
process as mixing rainwater, potash and animal tallow (rendered form of beef or mutton fat).
Back then, the process of making soap was known as a long and tiring process. The process
begun by melting and filtering the fat. Then, the potash solution was added. As we know that
the water and oil do not mix, the mixture must be continuously stirred and heated sufficiently
for making the fat melted. This chemical reaction called as ‘Saponification’ will take place in
between the fat and hydroxide which resulted in a liquid soap. Once the fat and water are no
longer separated, the mixture will be cooled down. During this stage, the salt which is the
sodium chloride will be added and act as the separator of excess water with the soap. The soap
will be at the top and it will be skimmed off. It will be placed in wooden molds for curing
process. This process basically took a few months which is to allow the reaction to be fully
completed.

The production of nowadays is much more effective less time consuming. The
manufacturing of soap is basically retained like it was back then where the fats and oil are
technically heated by adding the strong base which commonly used is sodium hydroxide or
potassium hydroxide which will produce fatty acid salts and glycerol that undergoes the
saponification process. The salt of fatty acid is known as soap which have the ability for
cleaning purposes as it has soft and waxy material. Next, the soap processing involved with the
positive ion such as Na+ or K+ and negative ion. The hydrolysis of animals or vegetable fats is
produced by anions of long-chained carboxylic acids.

The ester process which is naturally occurred in animal fats and vegetable oils results as soap
which is a generic term for sodium or potassium salts of long-chain organic acids (fatty acids).
RCO2H is the functional group which contain in all organic acids. The alkyl groups can be
listed as the R shorthand notation consists of methyl, CH 3-, ethyl CH3CH2-, propyl,
CH3CH2CH2-, or more complex hydrocarbon chains. The R shorthand notation been used by
the chemists because of these groups can be very large and the hydrocarbon chain has little
effect on the compound’s chemical reactivity. Generally, the RCO 2R functional group
contained in all esters. The R groups in soaps are the hydrocarbon chains that generally contain
up to 12-18 carbon atoms. While sodium fatty acids such as lauric (vegetable oil), palmitic
(palm oil), and stearic (animal fat) acids are just a few examples of soaps.

The hydrocarbon chain contains in soap may consists of saturated (no double bonds) or
unsaturated (contain double bond chains). The sodium salts are usually contained in bars of
soap as it is solid. While potassium salts always be the basis of liquid soaps, greases and
shaving cream. Triglycerides are known as esters which derived from three fatty acids. It is
usually found in fats and vegetable oils.

Figure 1: Triglyceride Molecule composed from Lauric Acid and Glycerol

The hydrolysis of an ester which produced a carboxylic acid salt and an alcohol is called
as saponification. The process of saponification can be explained as a lone pair of electrons on
the Hydroxide (OH-) is attracted to the partially positively charged Carbon (C) atom in the C=O
bond in the ester. The C-OR’ bond breaks generating a carboxylic acid (RCO2H) and an alcohol
(R’COH). The sodium salts (RCO2-Na+) had been converted by NaOH carboxylic acids. Once
the triglyceride is saponified, the soap and glycerol are produced. Therefore, the R groups in
the triglyceride may or may not have the same chain of length. Therefore, saponification results
to different types of soaps.
RESULT

Table 1: Formulation of soap bar

Material Weight (g)

RBDPO 500
Sunflower oil 500
NaOH 62.5
NaCl 62.5
EDTA 20
Water 375
Fragrance 5

Table 2: Result of analysis

Analysis Sample 1 Sample 2 Sample 3 Average

pH value 12.2 11.4 11.8 11.8
Saponification 0.142 0.136 0.148 0.142
value
Moisture 17.2 17.6 15.6 16.8
content (%)
ANALYSIS & DISCUSSION

The objectives of this experiment are to calculate weights of materials to be used in

the formulation of soap and to produce average quality of soap bar using basic formulations
from palm oil. The first objective is obtained and shown in Table 1

Soap is a substance that has the ability to remove dirt from a surface such as human
skin, textile or any other solids when being dissolved in water (Davidsohn, 2019). The
molecular structure of soap contains two part which are the hydrophobic (water-insoluble) such
as fatty acid or other long chain carbon group and hydrophilic (water-soluble) such as –COONa
(Davidsohn, 2019). As shown in Figure 2, the hydrophobic tail will attach itself to the dirt in
surface whereas the hydrophilic head will attracted to the water.

Figure 2: Hydrophobic and hydrophilic

The ingredients of soap have evolved ever since the first soap that are made of plant
saps of certain plant that was called “soap plant” (Chlorogalum pomeridianum). Nowadays,
fats and oils that react with lye, which is sodium hydroxide, NaOH can produce soap.
Generally, commercialised soaps that are made in this experiment are made of the mixture of
chemicals including sodium tallowate, sodium cocoate, sodium palmate and similar
ingredients, all of which are the results of reacting solid fats (tallow, coconut oil, and palm
kernel oil respectively) with lye (Simon Quellen Field, 2020). The physical of the soaps is also
depending on the type of lye being used. Sodium hydroxide, NaOH usually form solid soap or
hard soap while potassium hydroxide, KOH tends to be used in liquid soap or soft soap
production.

The process started with the mixture of oil is heated up at the temperature of 70 oC to
90 oC for 30 minutes. After 30 minutes, 50 % of the diluted NaOH is put into the mixture of
oil and rest for 15 minutes so that the mixture is being mixed well. Then, 50% NaCl plus EDTA
50% also been mixed together and are rest for 30 minutes. After 30 minutes all the balance
chemical is being put manually for 10 to 15 minutes until the soap is semi solid.
 The procedures mentioned make the second objective for this experiment achievable
because the percentage of materials that have been used is the same as the industry. If the
composition of basic formulation from palm oil is being change, the soap will also change
based on what is being the less or more and the state of the soap also will be changed for
instance too hard or too soft.

There are three analysis that have been carried out in this experiment to evaluate the
soap product which is:

i) pH value
ii) Saponification value
iii) Moisture content in %

For first analysis which is pH value, it is determined by using pH paper and the value
of pH based on pH scale value spectrum as shown in Figure 3 and recorded in Table 2.

Figure 3: pH scale (C. Ophardt, 2003)

Based on Table 2, analysis result for pH value shown that average pH for the soap
sample is 11.8. The pH scale shown that the soap produced in this experiment have basic
characteristics. As soap is usually being used on the human skin, good soap supposedly has the
pH around 6 which is slightly acidic to match the human skin which has the pH of 5.5 so that
there is not allergy or irritation reaction will occur (Sharod, 2014). But the average pH for cold
process soap is supposedly around 9-10 as the alkalinity characteristics helps to clean the skin
well (Ramirez et al., 2015). Even though the high pH soap may irritate the skin, it is important
to note that brief exposure to slightly alkaline soap does not harm skin as healthy skin can
rebalance the pH back in a very short amount of time.

As this analysis used pH strip to measure the pH value of the soap, there are few
problems arise from this method. The nature of soap can interfere with the indicator dyes used
to manufacture the strips which can throw the reading off by several points. Yet, because of
the limited pH analysis method, using a higher quality of pH strip can ease the variable under
control but using pH strips is not the most ideal method of checking the pH of a soap.

Second analysis is determination of saponification value which defined as a measure of

the alkali reactive groups in industrial oil and derivatives. Figure 4 shows the condensed
formula of the saponification process.

Figure 4: Saponification Process

To carried out the saponification analysis, the weighted sample that has been
determined based on saponification values of 170 to 200 is put into a conical flask. The mass
of the sample is altered accordingly so that about half the ethanolic potassium hydroxide
solution is neutralized. Then the portion of ethanolic potassium hydroxide solution and some
boiling add is pipetted into the flask together. Reflux condenser is connected to the flask and
the flask is set up on the heating device and is boiled. While boiling, the flask is shaken from
time to time for 60 minutes or 120 minutes if the oils and fats have a high melting point
which are difficult to saponify. The hot solution then is being added for about 0.5 to 1 mL of
phenolphthalein indicator and was titrated with the standard volumetric hydrochloric acid
solution until the pink color of the indicator turn colorless. For control analysis, blank test of
the same procedure is being carried out but omitting the test portion.
 The saponification value (SV) is being calculated by the equation below and is
recorded in the Table 2

56.10 𝑋 𝑀(𝑉0 − 𝑉𝑡)

𝑆𝑉 =
𝑚

Where,

M = Molarity of standardized HCl solution

V0 = Volume of titrant of blank (mL)

Vt = volume of titrant of test sample (mL)

m = mass of test portion (g)

Result for saponification value in table shown the average is 0.142. The saponification
value indicates the average molecular weight of a fat or oil. The value show that whether the
oil contain high quantity of lower or higher fatty acid. The more the value, the smaller the
molecular weight. The saponification value also indicates the length of carbon chain. The more
the saponification value, the shorter the carbon chain (Venkey, 2009).

For third analysis which is moisture content, the moisture content of each sample was
obtained, and the average is 16.8. The moisture content is the amount of moisture in the sample
given as a percentage of the sample’s original weight. The standard moisture range of the unit
is 0.0 to 17.0. The moisture content obtained from the experiment are in the range. One of the
objectives of this experiment is to produce average quality of soap bar. Since the moisture
content of the soap bar is in the range of standard moisture content, the soap produced in this
experiment has the average quality for industrial production.

Moisture content analysis is being calculated using the formula below and the value
in % is then recorded in Table 2.

𝑚𝑏 − 𝑚𝑑
% 𝑚𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝑎𝑛𝑑 𝑣𝑜𝑙𝑎𝑡𝑖𝑙𝑒 𝑚𝑎𝑡𝑡𝑒𝑟 = 𝑋 100 %
𝑚𝑏 − 𝑚
Where,

m = the mass of the dish (g)

mb = the mass of the dish and test sample (g)

md = the mass of the dish and test sample after drying (g)
CONCLUSION AND RECOMENDATION

In conclusion, the purpose of the experiment was to identify and calculate the weights
of materials to be used in the formulation of soap and to produce average quality of soap bar
using basic formulation from palm oil. Based on the result of the experiment, it shows the pH
of the soap produced were in alkaline range which is pH greater than 7. Next, the average
moisture content of the soap samples measured was 16.8% which can be considered as
negotiable soap since it was below the range of 17%. Then, the average saponification value
of the soap produced for the experiment obtained was 0.142. There are several
recommendations that can be implemented to improve the result of the experiment. Firstly,
the saponification value needs to be taken for at least three sample and get the average
reading so that the value can be considered more accurate and precise. Next, when mixing the
mixture of the chemical, the temperature does not need to be too hot because it will make the
soap produces became hot even after it undergo drying process which resulting in the soap
not able to properly mould and it can easily shatter.
REFERENCES

Ophardt, C. (2003). PH value. Retrieved November 15, 2020, from

http://chemistry.elmhurst.edu/vchembook/184ph.html

Sharod, N. (2014, December 20). Soap Formulation. Retrieved November 15, 2020, from
https://fliphtml5.com/puvd/tard/basic

Ramirez, Masciarelli J. (2015, February 07). How to Test pH with Red Cabbage. Retrieved
November 15, 2020, from https://www.soapqueen.com/bath-and-body-tutorials/tips-
and-tricks/test-ph-red-cabbage/

Davidsohn, A. S. (2019). Soap and Detergent. Retrieved November 17, 2020, from
Encyclopædia Britannica, inc. website: https://www.britannica.com/science/soap

Simon Quellen Field. (2020). Retrieved November 17, 2020, from Sci-Toys.com website:
https://sci-toys.com/ingredients/soap.html#targetText=Soap&targetText=Today%2C
soaps are made from,left in the soap dish.

Venkey (2009). Estimation of Saponification Value of Oil. Retrieved November 17, 2020,
from Classle website: https://www.classle.net/#!/classle/book/estimation-saponification-
value-oil/