I.

EXPERIMENT TITLE : Making Soap

II. EXPERIMENT DATE : Tuesday, 10th April 2018 at 10.00 a.m. –
16.00 p.m
III. EXPERIMENT PURPOSE :
1. Making the flow chart of making soap
2. Determine the reaction equation on making soap
3. Explaining the difference soap product made using base NaOH and KOH
4. Making soap emulsion
5. Explaining about process make water soap emulsion with oil
6. Determine the quality of oil based on peroxide number
IV. BASIC THEORY
The soap is an alkali metal salt (usually a sodium salt) of fatty acids.
Soaps contain C16 and C18 salts, but may also contain some carboxylates
with lower atomic weights. The soap is produced by the process of
sulphinification. Namely hydrolysis fat to fatty acids and glycerol under
alkaline conditions. Commonly used base conditions are NaOH and KOH.
Fatty acids that bind to sodium or potassium are then called soap. But
sometimes also use NH4OH. Soaps made with NaOH are slower to dissolve
in water than with soaps made using KOH. The strong alkali soap (NaOH,
KOH) has a pH value between 9.0 to 10.8 whereas a soap made with weak
alkali (NH4OH) will have a lower pH value of 8.0 to 9.5 (Fessenden &
Fessenden, 1986).
A soap molecule contains a long hydrocarbon chain plus ions. The
hydrocarbon portion of the molecule is hydrophobic and soluble in non-
polar substances. While the tip of the ion is hdrophilik and soluble in water.
Because of the hydrocarbon chain, a whole soap molecule does not form
micelles, ie a bunch of (50-150) water molecules whose hydrocarbon chains
cluster with their ionn ends facing the water (Fessenden & Fessenden, 1986).
Aqueous solutions of soap always ionized form of alkyl carboxylate
anion, which is active as washers so soap sodium alkyl carboxylate anion-
called active substances. The RCOO group has a double character, the alkyl
group R is hydrophobic (water-repellent) while the carboxylate-COO group
is hydrophilic (Hart, Craine, & Hart, 2003).
 Soap is the reaction product of a fatty acid with an alkali metal. The
resulting saponification results in a mixture of soap, glycerol, and the
residual alkali or fatty acid derived from fat which has been hydrolyzed by
alkali. The mixture is condensed, the period can be separated from the soap
by salting, if the soap is sodium soap, the process of salting can be done by
adding a saturated NaCl salt solution. After salting the soap solution up to
the surface of the NaCl salt solution, it can be separated from the glycerol
and salt solution by filtering from the saline solution. The thick soapy mass
is washed with cold water to neutralize the excess alkali or separate the
mixed salt NaCl. The thick soap is then molded into hand soap or chips and
pieces. Glycerol can be separated from the remaining saline NaCl solution
by vacuum distillation. NaCl salt can be recovered by way of castration and
can be used again (Fessenden & Fessenden, 1986).
Salt is also needed in the manufacture of soap that serves as a core
forming in the compaction process. The added salt is usually NaCl. By
adding NaCl it will form the core of soap and accelerate the formation of
soap solids. The salt used should be pure, not containing Fe, Cl, or Mg. If a
liquid soap is made, no salt is required. Some ingredients are needed as
antioxidants, which are materials that can stabilize soaps so they do not
become rancid. Sodium silicate, sodium hyposulfite, and sodium thiosulfate
are known to be used as antioxidants. Stanous chloride is also a very
powerful antioxidant and can also whiten the soap or as a bleaching agent.
While for additional ingredients of perfume, commonly used is patchouli
alcohol, cresol, pyrethrum, and sulfur. In the laundry soap is also used
organic solvents such as petroleum naphta and cyclohexanol. In this case
what needs to be known is that the soapy nature of soap is caused because
soap is a surfactant compound which can reduce surface tension while
emulsifying impurities. Grouping surfactant oil as anionic, cationic or
neutral depending on the nature of the hydrophilic group. The soap with its
carboxylate group is an anionic surfactant that is antibacterial (Prime &
Judge, 2009).
Soap is a kind of surfactant (surface active material), a compound that
lowers the surface tension of the water. This property causes the soap
solution to enter the fiber, Eliminates and expels dirt and oil. After dirt and
oil from the surface of the fiber, the soap helps to wash it because of its
chemical structure. The final part of the chain (ionnya) is hydrophilic (fun
water) while the carbon chain is hydrophobic (hate water). The hydrocarbon
chain is soluble in oil particles that are not water soluble. The ion is
dispersed or emulsified in water so it can be washed (Sari, Kasih, & Sari,
2010).
Soap serves to emulsify dirt in the form of oil or other impurities. The
soap is made through the process of saponification of fats or oils using an
alkaline solution by liberating glycerol. Fats or oils used can be animal fats,
vegetable oils, waxes, or marine fish oil.At this time the soap technology
has been growing rapidly.Sabun with the type and shape varies can be
obtained easily on the market such as bath soap, laundry soap either for
clothes or for household utensils, to soap used in industry.All oils or fats can
basically be used to make soap.The properties of the resulting soap are
determined by the amount and the composition of the fatty acid component
used. The corresponding fatty acid composition in the manufacture of soap
is limited by the length of the chain and the degree of saturation. Generally,
a chain length of less than 12 carbon atoms is avoided because it may
irritate the skin, otherwise the chain length of more than 18 carbon atoms
forms a soluble soap that is difficult to cause foam. Too large parts of
unsaturated fatty acids produce soaps that are easily oxidized when exposed
to air (Maripa, Kurniasih, & Ahmadi, 2015).
The requirement of the quality of bath soap specified by Indonesian
National Standard (SNI) for soap circulating in the market only covers the
chemical properties of bath soap, that is the minimum fatty acid content of
71%, maximum free fatty acid 2.5%, free alkali is calculated as maximum
NaOH 0 , 1%, non-soluble substance in alcohol maximum 2.5%, maximum
water content 15%, and mineral oil (negative). While the soap physical
properties such as cleaning, foam stability, hardness, and color do not have
SNI standards (Maripa, Kurniasih, & Ahmadi, 2015).
Based on SNI quality standards, mineral oil in a solid bath soap should
be no more than 0.05%, which is indicated by the absence of turbidity when
titrated with water. Soap that meets the standards according to SNI is a soap
with a concentration of 30% NaOH soap with a concentration of NaOH25%
and 35% does not meet the SNI. The presence of mineral oil is thought to be
due to fatty acid decarboxylation into alkanes groups. Decarboxylation may
be carried out thermally, photochemically, or catalytically with the aid of a
catalyst. Both open and aromatic acid chains can undergo a decarboxylation
reaction (Setiadi, 2010).

Acid Numbers
The acid number is the number of milligram KOH needed to neutralize
free fatty acids from one gram of oil or fat. The acid number indicates the
amount of free fatty acids in the oil and is expressed by mg of base per 1
gram of oil. The acid number is also an important parameter in determining
the quality of oil. This number indicates the amount of free fatty acids
present in the oil due to hydrolysis reaction in the oil especially during
processing. Fatty acids are the basic skeletal structures for most lipid
materials (Anwar, et al., 1994).
Acid numbers are used to measure the amount of free fatty acids
contained in oils or fats. That is by dissolving a number of oils or fats in
alcohol ether and given the indicator fenolftalein (PP). Further titrated with
a solution of 0.5 N KOH until a fixed pink color changes. The amount of
acid depends on the purity and age of oil or fat (Ketaren, 1996).
𝑉 𝑥 𝑁 𝑥 𝑀𝑟 𝐾𝑂𝐻
𝐴𝑐𝑖𝑑 𝑁𝑢𝑚𝑏𝑒𝑟
𝑊
Where is :
V: total mL of standard KOH solution
N: normality of standard KOH solution
W: weight of oil or fat sample (gram)
Saponification Number
The saponification number is the number of milligrams of KOH required
to store one gram of oil or fat. If some examples of oil or fat are saturated
with excessive KOH solution in alkhol then KOH will react with
triglycerides, ie three KOH molecules react with one molecule of oil or fat.
The remaining alkaline solution is determined by titration using an acid, so
the amount of alkali in question can be known.
Triglyceride potassium soap glycerol

In determining the sizing number of the alkali solution used is the KOH
solution, which is carefully measured into a tube using a burette or a pipette.
The saponification number may be defined by a reduction in the number of
milliard equivalents of the alkaline alcohol solution employed, multiplied by
the molecular weight of the alkali solution, divided by the sample weight in
grams (Ketaren, 1996).

𝑉 𝑥 𝑁 𝐻𝐶𝑙 𝑥 𝑀𝑟 𝐻𝐶𝑙
Saponification Number =
𝑊
V. TOOLS AND MATERIALS
A. Tool
1. Test tube 6 pieces
2. Pipette 5 pieces
3. Glass Measure 1 piece
4. Ohauss balance sheet 1 piece
5. Beaker glass 10 mL 2 pieces
6. Beaker glass 250 mL 1 piece
7. spatula 1 piece
8. Steam bath 1 piece
9. Spiritus burner 1 piece
10. Triangle 1 piece
11. Boiling stones 1 piece
12. Burning gauze 1 piece
13. Reflux 1 piece
14. Vial 12 pieces
15. Thermometer 1 piece
16. Molds of soap 1 piece
17. Statif and Clamp 1 piece
18. Burette 1 piece

B. Materials
1. Oil (palm, bulk, coconut) 66 grams
2. NaOH 4.2 grams
3. Stearic Acid 3 grams
4. Glycerin 12 grams
5. Olive oil 3 mL
6. Dyes sufficiently
7. Parfume sufficiently
8. Ethanol 75 mL
9. 10. PP Indicator 30 drops
10. KOH solution is 0,1 N sufficiently
11. HCl solution 0,5 N sufficiently
VI. LANES WORK
1. Making Soap

1,4 grams of NaOH

- Entered into test tube

- Diluted with 3,3 ml aquadest
NaOH solution

10 grams coconut oil 10 grams bulk oil 10 grams palm oil

- Entered into test tube

- Added 1 gram of stearic acid
- Heated until 70oC
- Waited until stearic acid melt
Brown mixture
Brown mixture

- Waited until the themperature

50oC
- Added NaOH solution
- Added 12 ml alcohol and 4
gram glycerin
- Heated and stirred until clear
- Added 1 ml of olive oil
- Added dye and perfume suffic
- Poured into mold
Solid soap

2. Character of Soap Emulsion

3 ml of aquadest 3 ml of aquadest

- Entered into test tube - Entered into test tube

- Added 5 drops oil
- Added 2 ml of soap emulsion
- Observed the separation
- Written the result
Time
- Added 5 drops oil
- Shaken until get emulsion
- Observed the separation
- Written the result
Time
 3. Acid Number
10 grams coconut oil 10 grams bulk oil 10 grams palm oil

- Entered into erlenmeyer flask

- Added 25 ml of ethanol
- Added 5 drops of PP indicator
- Titrate with standart solution
KOH 0,1 N
KOH volume

- Calculated the acid number

Acid number

4. Saponification Number
2 grams coconut oil 2 grams bulk oil 2 grams palm oil

- Entered into erlenmeyer flask

- Added 25 ml of 0,5 N KOH
solution
- Waited until cool
- Added PP indicator
- Titration with standart HCl 0,5 N
HCl volume

- Calculated the saponification

number
Saponification number

Reactions

1. Making Soap

Source: http://mixing-expert.com/wp-content/uploads/2013/08/untitled.jpg
2. Character of Soap Emulsion

Source: http://nsb.wikidot.com/local--files/c-9-5-5-4/Emulsion%202.jpg

3. Acid Number
H2C O C17H35 OH

H2C
HC O C17H35
+ 3 C2H5OH (aq) C17H35COOC2H5 (l) + CH OH

H2C O C17H35 H2C

(l) (aq)
OH

4. Saponification Number
H2C O R1 OH
O
H2C
HC O R2
+ 3 KOH (aq) 3 R C + CH OH
OK
H2C O R3 H2C
(l) (aq)
OH
VII. EXPERIMENT RESULT

No. Result of observation

Experiment procedure Assumption/reaction Conclusion
exp Before After
1. Making soap  NaOH : solid  Padatan NaOH NaOH (s) + H2O(l)  NaOH(aq) From the

1,4 grams NaOH  Aquadest : + aquadest : experiment we

colorless solution larutan NaOH know, the soap
- Entered into reaction tube  Coconut oil +
 Coconut oil : that made by
- Diluted with 3,3 mL
aquadest colorless solution stearic acids = coconut oil is

 Bulk oil : orange not dissolve, tranparant that

NaOH Solution stearic acid soap made by
solution
 Palm oil : soft upper layer palm oil and bulk

yellow solution  Bulk oil + oil.

 Stearic acid : stearic acid : not The soap can

white grain dissolve, upper made by reaction

between oil with
 Olive oil : layer

colorless solution  Palm oil + an alkaline

solution.
 Esetiatl oil : stearic acid: not

brownish orange dissolve, upper

solution layer
  NaOH solution :  Coconut oil +
colorless solution stearic acid +
10 grams 10 grams 10 grams
 Glyserin : light hetaed : stearic
coconut bulk oil palm oil
oil yellowish acid dissolve,
solution colorless
- Entered into reaction tube solution
- Added 1 grams of stearic acid
- Heated until 70°C. Until  Bulk oil +
stearic acid melt stearic acid +

Brown hetaed : stearic

Mixture acid dissolve,
- Waited until the temperature brownish
50°C.
- Added NaOH solution orange solution
- Added 12 mL alcohol and 4  Palm oil +
grams glyserin
- Stirred stearic acid +
- Heated and stirred until hetaed : stearic
clear
- Added 1 mL of olive oil acid dissolve,
- Added dye and parfume light yellow
sufficiently
- Poured into container solution
 Coconut oil
Solid Solid Solid after heated +
soap soap soap
NaOH +
 alcohol +
glrcerin :
colorless
solution
 Palm oil after
heated + NaOH
+ alcohol +
glrcerin : light
yellow solution
 bulk oil after
heated + NaOH
+ alcohol +
glrcerin : orange
solution
 the result of
palm oil, bulk
oil and coconut
oil + olive oil :
pregnant smell
2. Characteristic of soap solution  Aquadest :  Aquadest + Soap is an emulsifying agent that Bulk is good
3 mL of aquadest colorless solution palm : light has 2 poles (polar and non polar emulsifier for oil

- Entered into reaction tube  Soap solution yellow solution poles). Polar polar soap will go to and aquades than
- Added 5 drops oil bulk oil :  Aquadest + the oil, in the presence of that palm oil and
- Added 2 mL of soap solution
- Shaked until get emulsion brownish orange coconut : character, the oil liquid in the soap coconut oil. The
- Observed the separation solution colorless will form the emulsion. The higher high quality of
- Written the result
 Soap solution solution of emulsion is the lowest of quality soap is coconut oil
Time palm oil : light  Aquadest + the soap. (Anwar, et al., 1994) > palm oil > bulk
yellow solution bulk : brownish oil

 Soap solution orange solution

3 mL of aquadest coconut oil :  Aquadest +
- Entered into reaction tube
colorless solution palm + shaken :
- Added 5 drops oil
- Shaked until get emulsion  Palm oil : light light yellow
- Observed the separation
yellow solution solution, there
- Written the result
 Coconut oil : is foam
Time
colorless solution t= 18
 Bulk oil :  Aquadest +
brownish orange coconut oil +
solution shaken :
colorless
solution, there
 is foam
t = 16 second
 Aquadest +
bulk oil +
shaken :
brownish
orange
solution, there
is foam
t = 28 second

 Aquadest +
bulk oil + soap
solution :
orange solution
 Aquadest +
palm oil + soap
solution : light
yellow solution
 Aquadest +
coconut oil +
 soap solution :
colorless
solution
 Aquadest +
bulk oil + soap
solution +
shaken : turbid,
white emulsion
t = 30 second
 Aquadest +
palm oil + soap
solution +
shaken : turbid,
white emulsion
t = 28 second
 Aquadest +
coconut oil +
soap solution +
shaken : turbid,
white emulsion
t = 22 second
3. Acid number  Coconut oil :  Coconut oil + Acid number is posing the quantity Acid Numbers:
colorless ethanol : of free fat acids into oil and was bulk oil> palm
10 grams 10 grams 10 grams
coconut oil bulk oil palm oil solution colorless stated by mg of base per 1 gram of oil> coconut oil.
 Bulk oil : orange solution oil (buckle,1987)
solution  Bulk oil + The biger the value of acid The higher the
- Entered into  Palm oil : light ethanol : orange number, the worse the quality of acid number, the
rerlenmeyer flask
- Added 25 mL of yellow solution solution oil and the lower the value of acid lower the quality
ethanol  Ethanol :  Palm oil + number, the better the quality of (Abdry, 2008).
- Added 5 drops of PP
indicator colorless ethanol : light oil (Sudarmaji,1996) So, oil quality:
- Titration with standart solution yellow solution coconut oil> palm
solution KOH 0,1 N
 Pp indicator : oil> bulk oil

Volume Of KOH colorless  Coconut oil +

solution ethanol + pp
 KOH solution : indicator :
colorless colorless
solution solution
 palm oil +
ethanol + pp
indicator : light
yellow
colorless
 solution
 bulk oil +
ethanol + pp
Volume Of KOH
indicator :
- Calculated the acid orange solution
number

 Coconut oil +
Acid Acid Acid ethanol + pp
Number Number Number indicator +
titration with
KOH : soft pink
 palm oil +
ethanol + pp
indicator +
titration with
KOH :soft pink
 bulk oil +
ethanol + pp
indicator +
titration with
KOH: soft pink
 V KOH
titration with
palm oil: 3,1
ml
 V KOH
titration with
coconut oil :
2,9 ml
 V KOH
titration with
bulk oil : 3,5
ml
 The acid
number of
bulk oil : 1,96
 The acid
number of
coconut oil :
1,624
 The acid
 number of
palm oil :
1,736
4. Saponification number\  Coconut oil :  Coconut oil + The amount of saponification is From the
colorless solution KOH solution : defined as the amount of KOH experiment,
2 grams 2 grams 2 grams  Bulk oil : orange colorless milligram required to infuse 1 saponification
coconut oil bulk oil palm oil
solution  palm oil + gram of oil. The higher number of coconut

- Entered into erlenmeyer
flask
- Added 25 mL of KOH
solution 0,5 N
 Palm oil : soft KOH solution : saponification number, the higher oil>palm oil> bulk
light yellow the quality of soap. (Anwar, et al., oil.
yellow solution
 KOH solution : solution 1994) Based on theories

colorless solution  bulk oil + KOH that the higher

Volume Of  PP indicator : solution : saponification

HCl colorless solution orange solution number, the
- Calculated the  HCl 0,5N :  Coconut oil + quality of soap
Saponification
number colorless solution KOH solution higher too. So, the

+ reflacted : quaity of soap

colorless coconut oil>palm

Saponific Saponific Saponific
ation ation ation  palm oil + oil>bulk oil
Number Number Number
KOH solution
+ reflacted:
light yellow
 solution
 bulk oil + KOH
solution +
reflacted:
orange solution
 Result of palm
oil after result +
added PP
indicator : light
yellow solution
 Result of bulk
oil after result +
added PP
indicator :
orange solution
 Result of
coconut oil
after result +
added PP
indicator :
colorless
 Result of palm
oil after result +
added PP
indicator +
titration with
hcl: light
yellow solution
 Result of bulk
oil after result +
added PP
indicator +
titration with
HCl : orange
solution
 result of
coconut oil
after result +
added PP
indicator +
titration with
HCl : colorless
 solution
 V KOH for
palm oil :0,9
ml
 V KOH for
bulk oil : 1 ml
 V KOH for
coconut oil :
3,2 ml
 Saponification
number of
bulk
oil :0,4027
 Saponification
number of
palm
oil :0,1132
 Saponification
number of
coconut oil :
0,1825
VIII. ANALYSIS AND EXPLANATION
1. Making Soap
Safonification is a process of making soap that takes place by reacting
fatty acids, especially triglycerides with alkalis that produce soap and
byproducts of glycerol. Soap is a salt (sodium) that has a long carbon
sequence. The fat broodstock is called Fatty acids consisting of long
hydrocarbon chains (C-12 to C-18) that bind to form carboxyl groups. The
soap has its unique properties, that is, in its structure where both ends of the
structure have different properties. At one point there is a lipophilic fatty acid
sodium hydrocarbon (attracted to or dissolved fat and oil) or a base called a
nonpolar tip while at the other end which is a carboxylic ion is hydrophilic
(interested in or dissolved in water) or polar end (Parlan & Wahyudi, 2003).
a. Making Soap Using Palm Oil
In experiments that have been done that is making soap, first is weigh 10
grams palm oil the solution is yellow solution in a film roll bottle using a
previously calibrated ohauss balance, the color of palm oil is yellow because
the content of carotene dyes, but it can also occur due to absorption proes in
unsaturated oil (Ketaren, S. 1986). Then adding with stearic acid 1 gram, the
addition of stearic acid is to increase the hardness of the soap and stabilize the
foam. The oil is heated at 70°C so stearic acid melts, in this heating the oil
should not be heated too hot because the temperature is too hot it will oxidize
become brownish. It is closely related to the peroxide number that is the value
to determine the degree of damage to oils or fats caused by autooksidation.
After a stereic acid dissolve and temperature already showing 70oC using a
thermometer, then taking up using the wood clip, wait until the mixed
temperature (steamed palm oil & stearic acid) to 50oC prepare a NaOH
solution made using 1,4 grams of NaOH solids dissolved in 3,3 mL of
aquades, NaOH solids dissolved immediately in 3,3 mL of aquades because
NaOH is easily melted in open space because it absorbs CO2. when
 dissolving the solids of NaOH in a beaker should be soaked in water given
the nature of NaOH is exothermic (absorbing heat).

NaOH (s) + H2O(l)  NaOH(aq)

After the temperature reach 50oC, pour the NaOH solution into a mixture
solution (palm oil + stearic acid) after heated and stirred mixture solution
using a spatula to produce a precipitate (yellow ++ solid). Adding NaOH after
the mixed temperature (palm oil + stearic acid) reach to 50oC (due to) other
than that NaOH solution is as acid neutralizer considering NaOH is alkaline.
The base used is NaOH to obtain a solid soap. Then added 12 mL of alcohol
and then added 4 mL of glycerin the two solutions are colorless, the glycerin
solution slightly thicker than the alcohol produced by the mixture that is not
homogeneous and produces precipitate (yellow solid +++) and there are white
solution mixture considering the residual color of the sample. The reaction is :
O

H2C O CH C17H35

O
OH OH OH

C17H35
KOH 3C17H35COOC2H5 (l) + CH2
HC O CH + 3C2H6OH(aq) C
H
CH2 (l)

H2C O CH C17H35 (l)

The mixture solution is heated again in the steam bath and stirred
continuously using the spatula until the mixture becomes the clearest colored
solution as before. the addition of alcohol and glycerin in the manufacture of
soap is intended to obtain a transparent solid soap results, considering that
alcohol serves as a solvent that is soluble in fat and water so that the resulting
soap is very soluble in water, easy to foam, and can decrease the hardness of
water. Also as a moisturizer on the skin and easy to rinse.
The next step of the solution is taking up from the steam bath using
wooden clamps slowly, prepare 1 mL of olive oil, and parfume in accordance
with the taste of our group coincidence that smell of is choco vanila. The
function of adding olive oil itself is an activator to soften the skin when The
 addition of parfume is mean to add the smell. Pour the solution into pre-
prepared mold. Soap produced by using palm oil will be obtained hard results
and soap is difficult to foam so that if it will be used as raw material for
making soap, palm oil should be mixed with other materials. The reaction that
occurs in the manufacture of soap is a reaction saponification where the
reaction occurs when oil is added with an alkaline solution (NaOH).
O

H2C O C R1 H2C OH
O O

HC O C R2 3 NaOH HC OH + 3 Na O C R
O

H2C O C R3 H2C OH

oil glycerol soap

b. Making Soap Using Coconut Oil

In experiments that have been done that is making soap, first is weigh 10
grams coconut oil the solution is colorless (clear) in a film roll bottle using a
previously calibrated ohauss balance, the colorless solution of color in the oil
is due to the absence of the extracted pigment during coconut oil extraction
process (Ketaren, S. 1986). Then adding with stearic acid 1 gram, the addition
of stearic acid is to increase the hardness of the soap and stabilize the foam.
The oil is heated at 70°C so stearic acid melts, in this heating the oil should
not be heated too hot because the temperature is too hot it will oxidize
become brownish. It is closely related to the peroxide number that is the value
to determine the degree of damage to oils or fats caused by autooksidation.
After a stereic acid dissolve and temperature already showing 70oC using a
thermometer, then taking up using the wood clip, wait until the mixed
temperature (steamed coconut oil & stearic acid) to 50oC. Then prepare a
NaOH solution made using 1,4 grams of NaOH solids dissolved in 3,3 mL of
aquades, NaOH solids dissolved immediately in 3,3 mL of aquades because
NaOH is easily melted in open space because it absorbs CO2 when dissolving
the solids of NaOH in a beaker glass should be soaked in water given the
nature of NaOH is exothermic (absorbing heat).
 NaOH (s) + H2O(l)  NaOH(aq)

After the temperature reach 50oC, pour the NaOH solution into a mixture
solution (coconut oil + stearic acid) after heated and stirred mixture solution
using a spatula to produce a precipitate ( white solid ++ ). Adding NaOH after
the mixed temperature (coconut oil + stearic acid) reach to 50oC due to other
than that NaOH solution is as acid neutralizer considering NaOH is alkaline.
The base used is NaOH to obtain a solid soap. Then added 12 mL of alcohol
and then added 4 mL of glycerin the two solutions are colorless, the glycerin
solution slightly thicker than the alcohol produced by the mixture that is not
homogeneous and produces precipitate (white solid +++) and there are white
solution mixture considering the residual color of the sample. The reaction is :
O

H2C O CH C17H35

O
OH OH OH

C17H35
KOH 3C17H35COOC2H5 (l) + CH2
HC O CH + 3C2H6OH(aq) C
H
CH2 (l)

H2C O CH C17H35 (l)

The mixture solution is heated again in the steam bath and stirred
continuously using the spatula until the mixture becomes the clearest colored
solution as before. the addition of alcohol and glycerin in the manufacture of
soap is intended to obtain a transparent solid soap results, considering that
alcohol serves as a solvent that is soluble in fat and water so that the resulting
soap is very soluble in water, easy to foam, and can decrease the hardness of
water. Also as a moisturizer on the skin and easy to rinse.
The next step of the solution is taking up from the steam bath using
wooden clamps slowly, prepare 1 mL of olive oil, and parfume in accordance
with the taste of our group coincidence that smell of is choco vanila. The
function of adding olive oil itself is an activator to soften the skin when The
addition of parfume is mean to add the smell. Pour the solution into pre-
prepared mold. Soap produced by using palm oil will be obtained hard results
 and soap is difficult to foam so that if it will be used as raw material for
making soap, palm oil should be mixed with other materials. The reaction that
occurs in the manufacture of soap is a reaction Saponifikasi where the
reaction occurs when oil is added with an alkaline solution (NaOH).
O

H2C O C R1 H2C OH
O O

HC O C R2 3 NaOH HC OH + 3 Na O C R
O

H2C O C R3 H2C OH

oil glycerol soap

c. Making Soap Using Bulk Oil

In experiments that have been done that is making soap, first is weigh 10
grams coconut oil the solution is yellow solution (++) in a film roll bottle
using a previously calibrated ohauss balance, the color of bulk oil is yellow
solution ++ due to the presence of carotene dye stuffs can also occur due to
absorption proes in unsaturated oils (Ketaren, S. 1986). Then adding with
stearic acid 1 gram, the addition of stearic acid is to increase the hardness of
the soap and stabilize the foam. The oil is heated at 70°C so stearic acid melts,
in this heating the oil should not be heated too hot because the temperature is
too hot it will oxidize become brownish. It is closely related to the peroxide
number that is the value to determine the degree of damage to oils or fats
caused by autooksidation. After a stereic acid dissolve and temperature
already showing 70oC using a thermometer, then taking up using the wood
clip, wait until the mixed temperature (steamed bulk oil & stearic acid) to
50oC. Then prepare a NaOH solution made using 1,4 grams of NaOH solids
dissolved in 3,3 mL of aquades, NaOH solids dissolved immediately in 3,3
mL of aquades because NaOH is easily melted in open space because it
absorbs CO2 when dissolving the solids of NaOH in a beaker glass should be
soaked in water given the nature of NaOH is exothermic (absorbing heat).

NaOH (s) + H2O(l)  NaOH(aq)

 After the temperature reach 50oC, pour the NaOH solution into a mixture
solution (bulk oil + stearic acid) after heated and stirred mixture solution
using a spatula to produce a precipitate (yellow solid +++ ). Adding NaOH
after the mixed temperature (bulk oil + stearic acid) reach to 50oC due to
other than that NaOH solution is as acid neutralizer considering NaOH is
alkaline. The base used is NaOH to obtain a solid soap. Then added 12 mL of
alcohol and then added 4 mL of glycerin the two solutions are colorless, the
glycerin solution slightly thicker than the alcohol produced by the mixture
that is not homogeneous and produces precipitate (yellow solid ++++) and
there are white solution mixture considering the residual color of the sample.
The reaction is :
O

H2C O CH C17H35

O
OH OH OH

C17H35
KOH 3C17H35COOC2H5 (l) + CH2
HC O CH + 3C2H6OH(aq) C
H
CH2 (l)

H2C O CH C17H35 (l)

The mixture solution is heated again in the steam bath and stirred
continuously using the spatula until the mixture becomes the clearest colored
solution as before. the addition of alcohol and glycerin in the manufacture of
soap is intended to obtain a transparent solid soap results, considering that
alcohol serves as a solvent that is soluble in fat and water so that the resulting
soap is very soluble in water, easy to foam, and can decrease the hardness of
water. Also as a moisturizer on the skin and easy to rinse.
The next step of the solution is taking up from the steam bath using
wooden clamps slowly, prepare 1 mL of olive oil, and parfume in accordance
with the taste of our group coincidence that smell of is choco vanila. The
function of adding olive oil itself is an activator to soften the skin when The
addition of parfume is mean to add the smell. Pour the solution into pre-
prepared mold. Soap produced by using palm oil will be obtained hard results
and soap is difficult to foam so that if it will be used as raw material for
making soap, palm oil should be mixed with other materials. The reaction that
occurs in the manufacture of soap is a reaction Saponifikasi where the
reaction occurs when oil is added with an alkaline solution (NaOH).
O

H2C O C R1 H2C OH
O O

HC O C R2 3 NaOH HC OH + 3 Na O C R
O

H2C O C R3 H2C OH

oil glycerol soap

2. Character of Soap Emulsion

In the second experiment, the objective was to determine the emulsion
properties of each oil with the addition of emulsifier. The purpose of the
addition of emulsifier is to reduce the surface tension between the two phases
(interfacial stress) so as to facilitate the formation of the emulsion.
Experiments were carried out on three types of soap is soap from palm oil,
coconut oil, and bulk oil. In this experiment each oil sample contained 2 test
tubes with different treatments to compare the results. Different treatment is
first tube with addition of emulsifier (soap) and second tube is not added
emulsifier.
a. Coconut oil
In the first tube 3 ml of aquades were put into the test tube and added
5 drops of coconut oil and a solution of 2 ml of soap (coconut oil) was
added and shaken until the solution separated. Cloudy solution is formed
and white emulsion occurs. The time required for the separating solution is
22 seconds, the solution is formed into two layers, the top layer of oil and
the bottom layer of the aquaduct. That means the soap is made to have a
perfect emulsion. Soap is a surfactant material. This material can reduce
the surface tension of the solution, so in the presence of this process the
emulsion properties will increase. This is due to the nature of the soap
structure which has two poles of hydrophilic poles and a hydrophobic pole.
 Where the hydrophilic pole will go to the water layer, while the
hydrophobic pole to the air layer. Given these properties, the liquid in the
water will form an emulsion.
In the second tube 3 ml of aquades were put into the test tube and
added 5 drops of coconut oil. Then shaken and silenced until the solution
separates. Colored solution is formed and there are bubbles. The time
required for the separating solution is 16 seconds, the solution is formed
into two layers, the top layer of oil and the bottom layer of the aquaduct.
After the results obtained, the formation of two layers on the second tube
takes a shorter time than the first tube. This is because in the second tube
there is no emulsifier, which is a substance that helps maintain oil stability.
b. Palm Oil
In the first tube 3 ml of aquades were inserted into the test tube and
added 5 drops of palm oil and a solution of 2 ml of soap (oil palm) was
added and shaken until the solution separated. Cloudy solution is formed
and white emulsion occurs. The time required for the separating solution is
28 seconds, the solution is formed into two layers ie the top layer of oil
and the bottom layer of the aquades. That means the soap is made to have
a perfect emulsion. Soap is a surfactant material. This material can reduce
the surface tension of the solution, so in the presence of this process the
emulsion properties will increase. This is due to the nature of the soap
structure which has two poles of hydrophilic poles and a hydrophobic pole.
Where the hydrophilic pole will go to the water layer, while the
hydrophobic pole to the air layer. Given these properties, the liquid in the
water will form an emulsion.
In the second tube 3 ml of aquades were put into the test tube and
added 5 drops of palm oil. Then shaken and silenced until the solution
separates. Young yellow solution is formed and there are bubbles. The
time required for the separating solution is 18 seconds, the solution is
formed into two layers, the top layer of oil and the bottom layer of the
aquaduct. After the results obtained, the formation of two layers on the
second tube takes a shorter time than the first tube. This is because in the
 second tube there is no emulsifier, which is a substance that helps maintain
oil stability.
c. Bulk Oil
In the first tube 3 ml of aquades were put into the test tube and 5 drops
of bulk oil were added and the soap solution (bulk oil) was prepared 2 ml
then shaken and allowed to dissolve until the solution separated. Cloudy
solution is formed and white emulsion occurs. The time required for the
separating solution is 30 seconds, the solution is formed into two layers,
the top layer of oil and the bottom layer of the aquaduct. That means the
soap is made to have a perfect emulsion. Soap is a surfactant material. This
material can reduce the surface tension of the solution, so in the presence
of this process the emulsion properties will increase. This is due to the
nature of the soap structure which has two poles of hydrophilic poles and a
hydrophobic pole. Where the hydrophilic pole will go to the water layer,
while the hydrophobic pole to the air layer. Given these properties, the
liquid in the water will form an emulsion.
In the second tube 3 ml of aquades were put into a test tube and 5
drops of bulk oil were added. Then shaken and silenced until the solution
separates. The orange solution is formed and there are bubbles. The time
required for the separating solution is 28 seconds, the solution is formed
into two layers ie the top layer of oil and the bottom layer of the aquades.
After the results obtained, the formation of two layers on the second tube
takes a shorter time than the first tube. This is because in the second tube
there is no emulsifier, which is a substance that helps maintain oil stability.
3. Acid Number
The third experiments is acid number. The objective of experiment
is to determine the qualify of oil based on the acid number The acid
number is the number of milligram KOH needed to neutralize free fatty
acids from one gram of oil or fat. (Anwar, dkk, 1994). The first step is 10
gram of coconut oil colorless solution, 10 grams of bulk oil orange
solution, and 10 grams of palm oil light yellow solution entered into 3
different erlenmeyer flask. Then added 2 ml of ethanol. The result is
 coconut oil colorless solution, bulk oil is orange solution and palm oil is
light yellow solution. the function of ethanol as a solvent, to dissolve the
oil or fat in order to react with the alkaline solution. added 5 drops of pp
indicator. The function of pp indocator is make it easier to observation
because pp indicator when titrated with KOH produces soft pink. The
changing of soft pink solution indicates that free fatty acids have been
neutralized by KOH solution. after that titration with standart solution
KOH 0,1N. The result is soft pink solution. The volume of KOH that we
need to titration with coconut oil is 2,9 ml, bulk oil is 3,5 ml and palm oil
is 3,1 ml.

Based on calculation, we get the acid number of bulk oil is 1,96, the acid
number of palm is 1,736 and the acid number of of coconut oil is 1,624. The
bigger value of acid number, the worse quality of oil and the lower value of
acid number, the better quality of oil. The acid number of coconut oil is
bigger, so palm oil have better quality than bulk and coconut oil. The higher
quality coconut oil>palm oil> bulk oil

The reaction is

H2C O C17H35 OH

H2C
HC O C17H35
+ 3 C2H5OH (aq) C17H35COOC2H5 (l) + CH OH

H2C O C17H35 H2C

(l) (aq)
OH

4. Saponification Number
a. Using Palm Oil
The experiment was used to find the saponification number of palm oil by
weighing palm oil as much as 2 gram plus KOH alcoholic 0,5 N and refluxed
for 30 minutes which yielded yellow solution. The use of reflux aims to speed
up the reaction process in accordance with the law of the reaction rate, the
greater the temperature the reaction rate will run faster, then the solution is
ditetesi with PP that serves as indicator of the resulting solution turns pink to
change this color indicate the advantages of KOH so reacting with PP
produces a pink color. Further titrated with a solution of 0.5N HCl to the
equivalent point that the solution changed to the initial color of yellow with
the volume of HCl used is 1 mL, so it can be calculated the number of
saponification using equation
𝑉 𝑥 𝑁 𝑥 𝑀𝑟 𝐻𝐶𝑙
Saponification number : and obtained the saponification number
𝑤

of palm oil is 0,1825

The reaction is:

H2C O R1 OH
O
H2C
HC O R2
+ 3 KOH (aq) 3 R C + CH OH
OK
H2C O R3 H2C
(l) (aq)
OH
b. Using Coconut Oil

The experiment was used to find the saponification number of coconut oil
by weighing palm oil as much as 2 gram plus KOH alcoholic 0,5 N and
refluxed for 30 minutes which yielded yellow solution. The use of reflux aims
to speed up the reaction process in accordance with the law of the reaction
rate, the greater the temperature the reaction rate will run faster, then the
solution is ditetesi with PP that serves as indicator of the resulting solution
turns pink to change this color indicate the advantages of KOH so reacting
with PP produces a pink color. Further titrated with a solution of 0.5N HCl to
the equivalent point that the solution changed to the initial color of yellow
with the volume of HCl used is 0,9 mL, so it can be calculated the number of
saponification using equation
𝑉 𝑥 𝑁 𝑥 𝑀𝑟 𝐻𝐶𝑙
Saponification number : and obtained the saponification number
𝑤

of coconut oil is 0,1132

The reaction is:
 H2C O R1 OH
O
H2C
HC O R2
+ 3 KOH (aq) 3 R C + CH OH
OK
H2C O R3 H2C
(l) (aq)
OH
c. Using Bulk Oil

The experiment was used to find the saponification number of bulk oil by
weighing palm oil as much as 2 gram plus KOH alcoholic 0,5 N and refluxed
for 30 minutes which yielded yellow solution. The use of reflux aims to speed
up the reaction process in accordance with the law of the reaction rate, the
greater the temperature the reaction rate will run faster, then the solution is
drop with PP that serves as indicator of the resulting solution turns pink to
change this color indicate the advantages of KOH so reacting with PP
produces a pink color. Further titrated with a solution of 0.5N HCl to the
equivalent point that the solution changed to the initial color of yellow with
the volume of HCl used is 3,2 mL, so it can be calculated the number of
saponification using equation
𝑉 𝑥 𝑁 𝑥 𝑀𝑟 𝐻𝐶𝑙
Saponification number : and obtained the saponification number
𝑤

of bulk oil is 0,4027.

The reaction is:
H2C O R1 OH
O
H2C
HC O R2
+ 3 KOH (aq) 3 R C + CH OH
OK
H2C O R3 H2C
(l) (aq)
OH

Based on the experiment proving the saponification number of of bulk oil

> palm oil >coconut oil. This is accurate with the theory.
IX. CONCLUSION
1. The soap may be prepared by reacting an alkali with oil or fat.
2. The quality of the oil can be determined by looking at the time of the
formation of the emulsion. The order of soap quality from the best is soap
derived from coconut oil, palm oil, and bulk oil.
 3. The quality of oil is inversely proportional to the acid number. The best
oil quality sequence is coconut oil, palm oil, and bulk oil
4. The quality of oil is directly proportional to the amount of saponification.
The best quality of oil sequence is coconut oil, palm oil, and oil.
X. ANSWER OF QUESTION
1. How to make solid and soft soap (in the form of lines work / flow chart)?
 Solid soap
1,4 grams of NaOH

- Entered into test tube

- Diluted with 3,3 ml aquadest
NaOH solution

10 grams of oil

- Entered into test tube

- Added 1 gram of stearic acid
- Heated until 70oC
- Waited until stearic acid melt
Brown mixture

- Waited until the themperature

50oC
- Added NaOH solution
- Added 12 ml alcohol and 4
gram glycerin
- Heated and stirred until clear
- Added 1 ml of olive oil
- Added dye and perfume suffic
- Poured into mold
Solid soap

 Soft / liquid soap

1,4 grams of KOH

- Entered into test tube

- Diluted with 3,3 ml aquadest
KOH solution

10 grams of oil
 - Entered into test tube
- Added 1 gram of stearic acid
- Heated until 70oC
- Waited until stearic acid melt

Brown mixture

- Waited until the themperature

50oC
- Added KOH solution
- Added 12 ml alcohol and 4
gram glycerin
- Heated and stirred until clear
- Added 1 ml of olive oil
- Added dye and perfume suffic
- Poured into mold
Solid soap

2. Write the complete reaction of soap making?

Source: http://mixing-expert.com/wp-content/uploads/2013/08/untitled.jpg
3. How does the flowchart make soap emulsions?

3 ml of aquadest 3 ml of aquadest

- Entered into test tube - Entered into test tube

- Added 5 drops oil
- Added 2 ml of soap emulsion
- Observed the separation
- Written the result
Time
- Added 5 drops oil
- Shaken until get emulsion
- Observed the separation
- Written the result
Time

4. Explain how the process of soap emulsion takes place?

 Emulsifiers are emulsifying agent in order to form stable emulsions. Soap
is an example of an emulsifier.
Lines work:
a. Water and oil are liquids that do not blend into each other, but want to
separate from each other because they have different densities.
b. In an emulsion there are usually three main parts:
1. The dispersed portion comprising fat
2. The second part is called the dispersing medium also known as the
continous phase, which usually consists of water
3. The third part is an emulsifier that serves to keep the oil grains were
still suspended in water.
When oil and water are shaken together, it will form fatty grains and form
an emulsion, but when allowed oil particles will rejoin and separate from
water molecules. Here is the emulsifier function. With the emulsifier it
will be able to form a membrane around the dispersed granules, thus
preventing the reunion of the grains.

5. Make a problem formulation when making soap using alkali NaOH with
KOH with concentration, practice procedure and the same tools and
materials

 How do soap-making products use alkaline NaOH?

 How to make soap using alkali KOH?

6. Identify the variables involved (variable manipulation, response, and

control)

 Control variables: mass of alcohol, glycerol mass, and volume of olive

oil.

 Variable manipulation: oil sample.

 Response variable: the resulting soap

7. Make the practice procedure

 Samples of oil (palm oil, coconut oil and bulk oil) were weighed 10 grams,
then added 1 gram of stearate acid that had been weighed, after which
heated to 70oC until all stearic acid melted. Let the temperature drop to
50oC. While waiting for the temperature decrese, as much as 1,4 grams of
NaOH is dissolved in 3,3 mL of water (exothermic reaction), after all
mixed is awaited until the solution warms. The two results are mixed and
stirred, added 12 grams of alcohol, then added 4 grams of glycerin and
then heated and stirred again so that the solution becomes clear. The clear
solution is awaited warm, added 1 mL of olive oil, added dye, and added
seed oil. Finally, pour in a mold. Allow to dry until obtained soap derived
from palm oil, coconut, and bulk.

REFERENCES

Anwar, dkk.. 1994. Pengantar Praktikum Kimia Organik. Jakarta:

Departemen Pendidikan dan Kebudayaan Direktorat Jenderal
Pendidikan.
Fessenden, R. J., & Fessenden, J. S. 1986. Kimia Organik (Ed. 3).
(Terjemahan: A. H. Pudjaatmaka). Jakarta: Erlangga.
Hart, H., Craine, L. C., & Hart, D. J. 2003. Kimia Organik: Suatu Kuliah
Singkat. (Terjemahan: S. S. Achmadi). Jakarta: Erlangga.
Ismono, et al. 2018. Petunjuk Praktikum Kimia Organik. Surabaya: Jurusan
Kimia FMIPA UNESA.
Ketaren, S.. 1996. Pengantar Teknologi Minyak dan Lemak Pangan. Jakarta:
Universitas Indonesia (UI-Press).
Maripa, B. R., Kurniasih, Y., & Ahmadi. 2015. Pengaruh Konsentrasi NaOH
terhadap Kualitas Sabun Padat Minyak Kelapa (Cocos nucirefa) yang
ditambahkan Sari Bunga Mawar (Rosa L.). (online),
http://lppm.ikipmataram.ac.id/wp-content/uploads/2015/04/Baiq-
 Risni-Maripa-Pengaruh-Konsentrasi-NaOH-terhadap-Kualitas-Sabun-
Padat-dari-Minyak-Kelapa-Pend-Kimia.pdf diakses pada tanggal 14
April 2018.
Parlan & Wahyudi. 2003. Kimia Organik I. Malang: Jurusan Kimia FMIPA
UNESA.
Sari, T. I., Kasih, J. P., & Sari, T. J. (2010). Pembuatan Sabun Padat dan
Sabun Cair dari Minyak Jarak. Jurnal Teknik Kimia , 17 (1), 29-33.
Setiadi, S. (2010). Reaksi Dekarboksilasi Minyak Jarak Pagar untuk
Pembuatan Hidrokarbon Setara Fraksi Diesel dengan Penambahan
Ca(OH)2. Seminar Nasional Teknik Kimia Indonesia, (pp. 1-8).
Bandung.

CALCULATION

 Acid number

Knowed :

V. KOH for coconut oil : 2,9 ml

V. KOH for palm oil : 3,1 ml

V. KOH for bulk oil : 3,5 ml

N KOH : 0,1 N

Mr KOH : 56 gram/mol

Asked :

a. Acid number of palm oil

b. Acid number of bulk oil
c. Acid number of coconut oil

Answer :

a. Acid number of palm oil
b. Acid number of bulk oil
c. Acid number of coconut oil
 Saponification Number
Knowed :
V. HCl for bulk oil
V. HCl for palm oil
V. HCl for coconut oil
Mass of bulk oil
Mass of palm oil
Mass of coconut oil
N HCl
Asked :
Saponification of bulk oil, palm oil and coconut oil
Answer :
a. Saponification of bulk oil
V.Palm oil x N KOH x Mr KOH
= W KOH
3,1 ml x 0,1 N x 56 gram/mol
= 10 gram
= 1,736
V.bulk oil x N KOH x Mr KOH
= W KOH
3,5 ml x 0,1 N x 56 gram/mol
= 10 gram
= 1,96
V.coconut oil x N KOH x Mr KOH
=
W KOH
2,9 ml x 0,1 N x 56 gram/mol
= 10 gram
= 1,624
: 3,2 ml
: 1 ml
: 0,9 ml
: 2 gram
: 2 gram
: 2 gram
: 0,1 N
V.Palm oil x N HCl x Mr HCl
= W HCl
 3,2 ml x 0,1 N x 36,5 gram/mol
= 2 gram

= 0,4027
V.bulk oil x N HCl x Mr HCl
b. Saponification of coconut oil = W HCl
0,9 ml x 0,1 N x 36,5 gram/mol
= 2 gram

= 0,1132
V.coconut oil x N HCl x Mr HCl
c. Saponification of palm oil = W HCl
1 ml x 0,1 N x 36,5 gram/mol
=
2 gram

= 0,1825

ATTACHMENT

Preparations

Preparation tools Preparation substances Preparation the oil

1. Making soap

Measured stearic acid 1 gram of stearic acid Entred each oil into test
tube
Entered stearic acid Entered stearic Entered stearic Heated until the
into palm oil acid into coconut acid into bulk oil temperature reach
oil 70oC

Let it down until the Measured 1 gram NaOH Diluted NaOH

temperature reach 50oC with 3,3 ml
aquades

Added NaOH solution and Heated until not presence Added olive oil and parfume
glycerin into oil and heated precipitate
2. Character of Soap Emulsion

3 ml of aquadest for six test tube

Aquadest + 5 drops of Aquadest + 5 drops of bulk Aquadest + 5 drops of palm

coconut oil oil oil
 The defferent between added
The defferent between added The defferent between added
2 ml of soap solution and not
2 ml of soap solution and not 2 ml of soap solution and not
additions with it additions with it
additions with it
(bulk oil) (palm oil)
(coconut oil)

3. Acid Number

10 grams of coconut oil, Palm oil entered Coconut oil Bulk oil added
palm oil and bulk oil into erlenmyer Added ethanol 25 ml of ethanol
flask 25 ml

Palm oil Aded 25 ml added pp added pp the result

ethanol indicator in indicator in coconut oil
erlenmeyer with erlenmeyer with titration with
 palm oil coconut oil KOH solution

The result palm

The result bulk oil
oil titration with
titration with KOH
KOH

4. Saponification Number

Entered oil in aech Added 25 ml KOH Reflucted until 30

erlenmeyer in each test tube minutes
After refucted Titrated Result