LAB SCALE SOAP PRODUCTION

SUMMARY

The objectives of this experiment of lab scale soap production is to study the lab scale
soap production using the saponification reaction of fatty acid, calculate and determine the
pH value and moisture content (%) of the soap that has been produced and lastly to produce
average good quality of soap bar using basic formulation from palm oil. Saponification is
chemical reaction of fat towards soap production which is soap are produced during the
chemical reaction. In this experiment, steps of analysis data had been done based on the
objectives which is to synthesize a sample of hard soap and tested the soap produced. NaOH
is the substances used to determine the pH of the soap in analysis which it is known as a
strong alkaline where it can dissociate fully in water. pH of the soap in experiment is 14
which it is very strong alkali. For the saponification value, it can be deduced that the smaller
the molar mass of the fat, the higher the saponification value after three samples being
measured. The average saponification value is 4.114. The moisture content and volatile
matter is calculated for all three sample is 3.2%, 2.8% and 3%. The average moisture content
of the soap bar is 3% which it shows that the soap has good moisture content which it means
that the soap that has been produced has an average of water content. The moisture content
need to be lowered as it will show slightly alkaline where high moisture content in soap could
lead to reaction of excess water with un-saponified fat to give the free fatty acid and glycerol
in a process called hydrolysis of soap. Due to the pH value of soap is too alkaline, weighing
of sodium chloride and sodium hydroxide need to carry out twice to make sure the precision
of the weight.

OBJECTIVES

The objectives of this experiment are:

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

To produce average quality of soap bar using basic formulations from palm oil.
FLOW CHART

Preparation of ingredients
The ingredients required for this experiment are listed below:
Refined Bleached Deodorized Palm Oil (RBDPO)
Sunflower oil
Sodium Hydroxide (NaOH)
Sodium Chloride (NaCl)
Ethylene diamine tetra acetatic acid (EDTA) 0.1%
Water
Fragrance

Experimental Procedure
1. Blended oil is melted in a water bath at 70 80oC until homogeneous.
2. Reactor or mixer machine is swiched on and warmed up the machine for 5 minutes.
3. Blended oil is added into the mixer and start the mixer for 10 minutes.
4. Slowly, half of NaOH solution is added into mixer for neutralization taking place.
5. After 10 minutes, half of NaCI solution is added into the mixer.
6. Then, half of EDTA is added into the mixer.
7. Remaining of NaOH, NaCl and EDTA solution are added into the mixer and let the
reaction take place for 20 minutes
8. After that, all the materials in the mixer is taken and put it in flat plate. Let the material
under aircond condition for 5 minutes or until it become semi solid.
9. Material is cut into piece and cover it with tissue, after that stamp it with stamper to
produce shape and company name to the soap.

Analysis
pH Value
Saponification Value
Moisture Content
INTRODUCTION AND THEORY

Soap is a salt of a fatty acid. It used by household for washing, bathing, and other
types housekeeping, where soaps act as surfactants, emulsifying oils to enable them to be
carried away by water. It usually comes in termed a bar which is in solid formed. Basically
the production of soap involved treating vegetable or animal oils and fats with strong base
such as sodium hydroxides in an aqueous solution. Fats and oils are composed of
triglycerides which is three molecule of fatty acid attach to molecule of glycerol. The alkaline
solution, that is often called lye refers almost exclusively to soap made with sodium
hydroxide, brings about a chemical reaction known as saponification.

In this process, the triglyceride fats first hydrolyse into three fatty acids and the
combine with alkali to form crude soap. Crude soap is an amalgam of various soap salts,
excess fat or alkali, water and glycerine. The glycerine, a useful by-product, can remain in the
soap product as a softening agent.

Much soap are mixtures of sodium or potassium salts of fatty acids which can be
derived from oils or fats by reacting them with an alkali (such as sodium or potassium
hydroxide) at 80 l00C in a process known as saponification. The fats are hydrolysed by
the base, yielding glycerol and crude soap. Historically, the alkali used was potassium
hydroxide made from the deliberate burning of vegetation such as bracken, or from wood
ashes.

As the soap has been produced, there are few considerations that must be taken to
measure the average quality of soap. The considerations that must be taken are pH value
saponification value and moisture content. The pH value is determined the degree of acidity
or alkalinity of the soap. Around 5.5-7.5 are the average range for a good soap. Then
saponification value is the number of mg of potassium hydroxide required to saponify 1g of
fat, to neutralise the free fatty acids and the fatty acids combined as glycerides. Next, the final
consideration is the moisture content in soap basically, moisture content is the amount of
water left in the soap after being dried in the oven. The amount of moisture content should be
around 5-7% in order to produce good quality soap.

Soaps are key components of most lubricating greases, which are usually emulsions
of calcium soap or lithium soap and mineral oil. Many other metallic soaps are also useful,
including those of aluminium, sodium, and mixtures of them. Such soaps are also used as
thickeners to increase the viscosity of oils. In ancient times, lubricating greases were made by
the addition of lime to olive oil.
RESULT

Table 1: Formulation of soap bar

Material Weight (g)

RBDPO 700

Cooking oil 300

NaOH 120

NaCl 24

EDTA 2.4

Water 244ml

Artificial colour Blue

(Refer appendix for calculation)

Table 2: Result of analysis

Analysis Sample 1 Sample 2 Sample 3 Average

pH value 14 14 14 14

Saponification value 4.488 1.683 6.171 4.144

4

Moisture content (%) 3.2 2.8 3.0 3.0

(Refer appendix for calculation)

The saponification value (SV) can be calculated by the formula below:

56.10 (0 )
=

Where,

M is molarity of standardized HCL solution (0.5M)

 0 is volume of titrant of blank sample (22.8 ml)

is volume of titrant of test sample (ml)

m is mass of test portion (5g)

Sample calculation:

Sample 1

56.10 0.5(23.8 23.0)

=
5

= 4.488

The moisture content can be calculated by the equation below:

% & = 100%

Where,

m is the mass of petri dish

is the mass of the petri dish and sample (g)

is the mass of the petri dish and test sample after drying

Sample calculation:

Sample 1

64.3 63.98
% & = 100%
64.3 54.31

= 3.2 %
DISCUSSION

Soaps are water soluble sodium or potassium salt of fatty acid. It is used with
water for the purpose of cleaning and washing. Soap is made up by a long hydrocarbon chain
(Helmenstine, 2017). The molecule of soap has two different ends. One ends of soap is
hydrophilic, the other end is hydrophobic. The hydrophobic molecule will attach to the oil
and the hydrophilic molecule with be exposed to water (Williams, 2017).

Figure 1: Structure of soap

Soap is produced by saponification process where hydrolysis of fats in chemical

reaction happen. A lab scale soap production was conducted with an objectives to calculate
weight of material used in the formulation of soap and to produce average quality of soap bar
using basic formulation from palm oil.

To make soap RBDPO is mixed with cooking oil and is stirred for 30 minutes
with temperature range of 70 C to 80 C. Next, add of NaOH and stirred for 10 to 15
minutes. Add of NaCl and stirred for another 10 minutes and add of NaOH for 10 to 15
minutes. The mixture will started to changed colour and the texture will turn to semi solid.
After that, pour in EDTA into the mixture and continue to stir until the texture of the mixture
turn to mash potato like texture. Fragrance and artificial colour is added, but it is optional.
Then, the mixture is put in a mold and let to set.

On the other hands, a three sample is prepared and tested for pH value, saponification
value and moisture content. First the pH value of the samples is tested using a litmus paper. It
is found that all of the three sample have pH of 14. The produced soap is a very strong alkali.
The range of pH to consider soap is safe to use is between neutral to slightly alkali (pH 7-10).
A pH value above 10 indicates that the soap is harsh and mat contain free lye (lye that does
not react with soap). Soap with a pH value above 10 can caused burn to skin if used. The high
pH of the produced soap is due to error in measuring the ingredient. (Evans, 2017).

Saponification value is referred as the number of milligrams of lye (sodium

hydroxide) required to completely saponify one gram of fat. (Mixon, 2017). Therefore,
saponification value of soap is depend on how much lye is used. To calculate the
saponification value of the produced soap an analysis is done. 5g of sample it put into three
round bottom flask and 25ml of ethanolic potassium hydroxide is added. The solution is
connected to a reflux condenser and boil gently. It is left for 60 minutes to 2 hours if the oil
and fats having a high melting point that make it difficult to saponify. Next, three drops of
phenolphthalein is indicator is added. The solution is then titrated with standard volumetric
sodium hydroxide until the pink colour turns colourless. The volume of titrant for all three
samples are Vt1 is 23.0 ml, Vt2 is 23.5 ml and Vt3 is 22.7 ml. The volume of titrant for blank
sample is 23.8 ml. Using the formula saponification value is calculated, the saponification
value for the samples are 4.488, 1.683, and 6.171. The average saponification value is 4.114.
Thus, for this soap bar, 4.114mg of sodium hydroxide is needed to completely saponify one
gram of fat.

Moisture content is how much water content in the material. For lab scale soap
production the moisture content of soap must not exceed 0.3. Therefore, the freshly prepared
soap is weight around 10 g approximately is placed on heated petri dish. It is then put in a
desiccators for the oil to cool down and then it is heated in the oven at 103 C for 2 hours and
30 minutes. After that, it is allowed to cool to room temperature and the moisture content is
calculated. If it exceed 0.3% it is heated back for 30 minutes intervals.

Table 3: Data before and after drying

Samples Mass of dish Mass of dish Mass of dish

(g) and samples (g) and samples after
drying (g)

Sample 1 54.31 64.3 63.98

Sample 2 58.3 68.32 68.30

 Sample 3 53.4 63.41 63.00

The moisture content and volatile matter is calculated for all three sample is 3.2%,
2.8% and 3%. The average moisture content of the soap bar is 3%.

There are a few error during the experiment, the amount of sodium hydroxide
should be 20% of the total weight of oil. However, prepared sodium hydroxide is only 120g
than 200g. Next, during flux, it is better to use round bottom flask than a conical flask or a
beaker to avoid quantity loss. During the drying, be sure to calculate the moisture content
correctly to avoid repeating the drying process resulting the soap to be over dry.
CONCLUSION

In conclusion, this experiment manages to get the saponification value of 4.144 and
the pH value of the soap is 14. This experiment is about making soap through the
saponification where hydrolysis of fats in chemical reaction happened. In this experiment, fat
act as hydrophobic tail and sodium ion that attached to fat chain act as hydrophilic head
which is acts as a dirt-carrier. Sodium chloride act to increase the density of soap. EDTA acts
as chelating agent that sequesters metals that the bacteria require in order to grow. The pH
value of soap of experiment is slightly more alkaline than the value allowed in industry which
is in range of 9-11. The artificial colour is added depends on the interest of the person as we
used blue artificial colour.

RECOMMENDATION

As to get better results, here are some recommendations. First, cool the soap for
longer time in order to make soap more solid and easier to handle. Then, when diluting
sodium chloride and sodium hydroxide using distilled water, its better use heated distilled
water to make sure that the reactant soluble in water. Due pH value of soap is too alkaline,
weighing of sodium chloride and sodium hydroxide need to carry out twice to make sure the
precision of the weight. Then, while stirring the mixture either to mix the solution of EDTA,
NaOH and NaCl or to concentrate the artificial colour, make sure to stir continuously until
white soft solid is formed and to spread the colour to entire solutions.

REFERENCES

1. Preparation and Properties of Soap. (2006) Organic Lab Chemistry. [Online]. [Access,
21 October 2017] Available from Seattle central Web:
http://www.seattlecentral.edu/faculty/ptran/bastyr/Summer%2006/organic/Organic%2
0Exp/Experiment4Preparation%20and%20properties%20of%20a%20soap1.pdf

2. Soap. (2008) Soap-making processes. . [Online]. [Access, 21 October 2017] Available

from Wikipedia Web: https://en.wikipedia.org/wiki/Soap

3. What is Soap? (2012) Curios Soapmaking and Cosmetic Making. [Online]. [Access,
21 October 2017] Available from Soap Maker Web: http://curious-
soapmaker.com/what-is-soap.html
4. Soaps & Detergents: Chemistry (2017). Cleaning Institute. [Online]. [Access, 21
October 2017] Available from Cleaning Institute Web:
http://www.cleaninginstitute.org/clean_living/soaps__detergents_chemistry.aspx

5. Helmenstine, A. (2017). What Is Soap Made of and How Does It Clean?. ThoughtCo.
Retrieved 18 October 2017, from https://www.thoughtco.com/how-dos-soap-clean-
606146

6. Williams, G. (2017). Soap - how does it get things clean?. Planet-science.com.

Retrieved 18 October 2017, from http://www.planet-science.com/categories/under-
11s/chemistry-chaos/2011/06/soap---how-does-it-get-things-clean.aspx

7. Evans, C. (2017). Soap Testing for Safety: Soap pH. Soap-made-easy.com. Retrieved
18 October 2017, from http://www.soap-made-easy.com/soap-ph.html

8. Mixon, K. (2017). Certified Lye - Using Lye to Make Soap. Certified-lye.com.

Retrieved 20 October 2017, from http://www.certified-lye.com/lye-soap.html
APPENDICES

Calculation for formula

Sodium Hydroxide (NaOH)

20 % = 20 % ( 700 + 300 )

= 200 (should be used)

Sodium Chloride (NaCl)

20 % = 20% (120 )

= 24

EDTA

10 % = 10% (24 )

= 2.4

Water

The amount of water is equivalent to the weight of NaOH and NaCl added.

120 + 24 = 144

Calculation for saponification value

Sample 1

56.10 0.5(23.8 23.0)

=
5

= 4.488

Sample 2

56.10 0.5(23.8 23.5)

=
5

= 1.638

Sample 3
 56.10 0.5(23.8 22.7)
=
5

= 6.171

4.488+1.638+6.171
= 3

= 4.114

Calculation for moisture & volatile matter

Sample 1

64.3 63.98
% & = 100%
64.3 54.31

= 3.2 %

Sample 2

68.8 68.50
% & = 100%
68.8 58.3

= 2.8%

Sample 3

63.4 63.00
% & = 100%
63.41 53.40

= 3.0 %

3.2 % + 2.8 + 3.0%

=
3

=3%