JAN

2015

EXPERIMENT No: 3
LAB SCALE SOAP PRODUCTION
1.0

OBJECTIVES

The objectives of this experiment are:

2.0

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.

INTRODUCTION

Soap is a surfactant used in conjunction with water for washing and cleaning. It usually comes in
a solid molded form, termed bars The use of thick liquid soap has also become widespread,
especially from soap dispensers in public washrooms. Applied to a soiled surface, soapy water
effectively holds particles in suspension so the whole of it can be rinsed off with clean water. In
the developed world, synthetic detergents have superseded soap as a laundry aid.

Much soap are mixtures of sodium (soda) or potassium (potash) 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 hydrolyzed 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.

Soap is derived from either oils or fats. Sodium tallowate, a common ingredient in many soaps,
is in fact derived from rendered beef fat. Soap can also be made of vegetable oils, such as olive
oil. Soap made entirely from such oils, or nearly so, is called castile soap. The use of the word
"soap" has become such a household name that even cleaning solutions for the body that don't
have soap in the ingredients are referred to as soap.

Cold Process
Cold process is a method of making soap (saponification) which does not require an external
heat source to initiate saponification. (Heat may still by applied in order to melt fats or oils that
are solid at room temperature, and to speed the reaction.) This process is often used by soapers,
or home soapmakers. A Lye solution, either sodium hydroxide or potassium hydroxide and
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EXPERIMENT No: 3
LAB SCALE SOAP PRODUCTION
water, is mixed with an appropriate amount of fats and/or oils to start the saponification process
that leads to soap.

Once the warmed or melted oils or fats and the lye solution have cooled to about 80-90 degrees
Fahrenheit, the lye solution is poured into the oils and stirred. A stick blender is often used to
speed this process. The two thin, clear substances become cloudy and begin to thicken.
Soapmakers refer to the
thickening process as "tracing". After many minutes of stirring, the mixture turns to the
consistency of a thin pudding.

Essential oils, fragrance oils, herbs, oatmeal or other additives are added at light trace, just as the
mixture starts to thicken. Soap is then typically poured into wooden molds lined with heavy wax
paper, covered and/or insulated with towels or blankets and allowed to continue saponification
for 18-24 hours. During this time, it is normal for the soap to go through a "gel phase" where the
opaque soap will turn somewhat transparent for several hours before turning opaque again. The
soap will continue to give off heat for many hours after trace.

After the insulation period the soap is firm enoughto be removed from the mold and cut into
bars. At this time, it is safe to use the soap since the saponification process is complete.
However, most soapmakers prefer to cure the bars for 2-6 weeks, depending on initial water
content, to allow for the bars to harden significantly before using. For successful cold-process
soap making, one needs to measure the exact amount of lye to be used and know the
saponification values ofthe oils being used in the soap. Excess unreacted lye in the soap will
result in a very high pH and can bum or irritate the skin.

Not enough lye, and the soap is greasy and oily. Most soap makers formulate their recipes with
3-15% excess oil so that all of the lye is reacted and that excess fat is left f( skin conditioning
benefits. Other processes used by soapers are the hot process, and the melt and pour process, and
rebatching.

JAN
2015

EXPERIMENT No: 3
LAB SCALE SOAP PRODUCTION
Hot Process
Hot process is a traditional method of making soap, still used by some soapmakers. In the hot
process method, fats and oils are boiled in a lye solution (either sodium hydroxide or potassium
hydroxide). After saponification has occurred, the soap is sometimes precipitated from the
solution by adding salt, after
which the liquid component is drained.

Most modem soapmakers add the correct amount of lye and water to the hot oils and stir until
full saponification occurs- either by taste (a quick touch to the tip of the tongue - I has a very
bright and distinct taste which goes away upon saponification) or by eye (m( experienced soap
makers know what gel stage and full saponification looks like). The hot, soft soap is then
spooned into a mold. Hot process soap can be used right away (co process needs to be insulated
so the saponification can finish).

Historically salt has been added to harden the bars- potassium hydroxide (a.k.a potash) makes a
soft soap. Sodium hydroxide (most commercially available lye) makes a quite satisfactorily hard
bar. Although more time consuming than the cold process, the hot process was used in the time
before pure lye was available, as it can use natural lye solutions such as potash. T; main benefit
of hot processing was that the exact concentration of the lye solution did] need to be known to
perform the process with adequate success. Today's hot process soap makers do use accurate
amounts of lye thereby taking the guesswork out of soap making. Other processes or techniques
used by soapers are the cold process, the melt and
pour process, and rebatching.

Literature
Saponification is the hydrolysis of an ester under basic conditions to form an alcohol and the salt
of a carboxylic acid. Saponification is commonly used to refer to the reaction of a metallic alkali
(base) with a fat or oil to form soap. Saponifiable substances are those can be converted into
soap. The reaction
is stated below:
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EXPERIMENT No: 3
LAB SCALE SOAP PRODUCTION
The lye used is a form of sodium hydroxide (NaOH) which is a caustic base. If NaOH was used,
a hard soap will be formed, whereas a soft soap is formed when potassium hydroxide (KOH) is
used. Vegetable oils and animal fats are fatty esters in the form of triglycerides. The alkali breaks
the ester bond and
releases the fatty acid and glycerol. The soap is salted out by precipitating it with saturated
sodium chloride

3.0

METHODOLOGY

3.1

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

The students have to calculate the weight of each ingredients required based on 1000g of
blended oil used (RBDPO and Sunflower oil). The sample of calculation is provided in the
appendix. The calculations have to be prepared before the experiment and must be included in
the report.

JAN
2015

EXPERIMENT No: 3
LAB SCALE SOAP PRODUCTION
3.2

Experimental Procedure
1. Melt the blended oil in a water bath at 70 80oC until homogeneous.
2. Switch on reactor or mixer machine and warming up the machine for 5 minutes.
3. Add in the blended oil into the mixer and start the mixer for 10 minutes.
4. Slowly, add in half of NaOH solution into mixer for neutralization taking place.
5. After 10 minutes, add in half of NaCI solution into the mixer.
6. Then, add in half of EDTA into the mixer.
7. Add in the remaining of NaOH, NaCl and EDTA solution into the mixer and let
the reaction take place for 20 minutes
8. After that, take all the materials in the mixer and put it in flat plate. Let the
material under aircond condition for 5 minutes or until it become semi solid.
9. Cut the material into piece and cover it with tissue, after that stamp it with
stamper to produce shape and company name to the soap.

4.0

ANALYSIS

4.1

pH Value
Check the pH value of soap bar using pH paper and record the value in the table.

4.2

Saponification Value
Theory
The saponification value is a measure of the alkali reactive groups in industrial oil and
derivatives and is expressed as the mg of potassium hydroxide which react with 1 g of
test sample.
The saponification value (SV) can be calculated by the equation below:
SV =

56.10(0 )

Where,

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2015

EXPERIMENT No: 3
LAB SCALE SOAP PRODUCTION
M

is molarity of standardized HCl solution

V0

is volume of titrant of blank (mL)

Vt

is volume of titrant of test sample (mL)

is mass of test portion (g)

Apparatus:

Conical flaks
Reflux condenser
Water bath or hot plate
Burette, 50mL capacity
Pipette, 25mL capacity

Solutions
1. Hydrochloric acid, 0.5M
2. Potassium hydroxide (KOH), 0.5M solution in 95% (v/v) ethanol.
This solution shall be colorless or straw yellow. A stable colourless solution can
be prepared by either of the following procedures.
(a) Reflux 1L of ethanol with 8g of potassium hydroxide and 5g aluminium
pellets for 1hr, then distill immediately. Dissolve the required amount of
potassium hydroxide in the distilled ethanol. Allow to stand for several days,
and then decant the clear supernatant liquid from the potassium carbonate
deposit.
(b) Add 4g of aluminium tert-butylate to 1L of ethanol and allow the mixture to
stand for several days. Decant the supernatant liquid and dissolve in it the
required amount of potassium hydroxide. Allow to stand for several dayds and
then decant the clear supernatant liquid from the potassium carbonate
deposited.
Store this solution in a brown or yellow bottle fitted with a rubber stopper. Do not
use a glass stopper. Decant the solution before use.
3. Phenolphthalein indicator solution
10g/L solution in 95% (v/v) ethanol or alkali blue 6B, 20g/L solution in 95% (v/v)
ethanol.
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2015

EXPERIMENT No: 3
LAB SCALE SOAP PRODUCTION
4. Boiling aid, fat free.

Experimental procedures:
1. Weight to the nearest 5mg about 2g of the test sample into a conical flask.
Note: The test portion of 2g has been determined on the basis of saponification
values of 170 to 200. For other saponification values, the mass should be altered
accordingly so that about half the ethanolic potassium hydroxide solution is
neutralized.
2. Using a pipette, add to the portion 25mL of the ethanolic potassium hydroxide
solution and some boiling aids. Connect the reflux condenser to the flask, place
the flask on the heating device and boil gently, shaking from time to time, for 60
min or for 2hrs in the case of oils and fats having a high melting point and which
are difficult to saponify.
3. Add to the hot solution 0.5mL to 1mL of the phenolphthalein indicator and titrate
with the standard volumetric hydrochloric acid solution until the pink color of the
indicator just disappears. If the solution is strongly colored, use 0.5mL of alkali
blue 6B solution.
4. Carry out a blank test following the procedure specified above using again 25mL
of the following ethanolic potassium hydroxide solution but omitting the test
portion.

JAN
2015

EXPERIMENT No: 3
LAB SCALE SOAP PRODUCTION
4.3

Moisture Content
Theory:
The moisture content can be calculated by the equation below:
% Moisture and volatile matter =

100%

Where,
m

is the mass of the dish (g)

mb

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

md

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

Apparatus:

Air oven

Analytical balance

Petri dishes

Desiccator

Experimental procedures:
1. Dry cleaned petri dishes in the oven at 103oC for at least 15 min and allow
cooling in desiccators. Weigh the dish to the nearest 0.001g.
2. Weigh approximately 10g of the molten oil (test sample) to the nearest 0.001g
into the dish. Return to the desiccators until the oil has thoroughly cooled. Weigh
the dish plus the oil to the nearest 0.001g and place the dish in the middle shelf of
the oven at 103oC for exactly 2.5h.
3. Remove the dish and allow it to cool to room temperature in the desiccators (30 to
45 min) before reweighing to the nearest 0.001g.
4. If the moisture exceeds 0.3%, continued drying (at 30 min interval) to constant
weight is recommended. In this case, the difference between two successive
weighing should not exceed 0.002g. Carry out two determinations of test portions
taken from the same test sample.
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2015

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LAB SCALE SOAP PRODUCTION
Table of Data:
Table 1: Formulation of soap bar
Material

Weight (g)

RBDPO
Sunflower oil
NaOH
NaCl
EDTA
Water
Fragrance

Table 2: Result of analysis

Analysis

Sample 1

Sample 2

Sample 3

Average

pH value
Saponification value
Moisture
(%)

content

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2015

EXPERIMENT No: 3
LAB SCALE SOAP PRODUCTION

APPENDIX 1
Sample of Calculation

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