Professional Documents
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Oleh:
JURUSAN KIMIA
Acid Number =
Saponification Number =
Whereas,
N HCl = normality of HCl
V HCl = volume of HCl
Mr HCl = molecular relative mass of HCl
W = weight of samples
(Winarno, 1991)
6. Fats and Oils
Fat and oil commonly used in making soap are triglycerides
with three irregular fatty acids which are esterified with glycerol. Each
fat contains a number of fatty acid molecules with a long carbon chain
between C12 (lauric acid) to C18 (stearic acid) in saturated fats and so
is unsaturated fat. The triglyceride mixture is processed into soap
through the saponification process with sodium hydroxide solution to
free glycerol (Baysinger, 2004).
Most of the fats and oils contained in nature are mixed
triglycerides, meaning that the three parts of the fatty acids from the
glycerides are not the same. Almost all of the fatty acids in nature
have an even number of carbon atoms because this acid is
biosynthesized from a two-carbon acetyl group in acetyl coenzyme A
(Fessenden and Fessenden, 1986).
More than 100 different fatty acids are known and about 40
occur widely. Palmitic acid (C16) and stearic acid (C18) are the most
abundant saturated fatty acids; oleic and linoleic acids (both C18) are
the most abundant unsaturated ones. Oleic acid is monounsaturated
because it has only one double bond, whereas linoleic, linolenic, and
arachidonic acids are polyunsaturated fatty acids because they have
more than one double bond. Linoleic and linolenic acids occur in
cream and are essential in the human diet; infants grow poorly and
develop skin lesions if fed a diet of nonfat milk for prolonged periods.
Linolenic acid, in particular, is an example of an omega-3 fatty acid,
which has been found to lower blood triglyceride levels and reduce
the risk of heart attack. The name omega-3 means that there is a
double bond three carbons in from the noncarboxyl end of the chain
(McMurry, 2016).
1. Types of Fats and Oils
Tallow (Cow Fat)
Tallow is beef fat or lamb produced by the meat
processing industry as a by-product. Tallow with
good quality is usually used in making low quality
bath and tallow soaps used in making laundry soap.
Oleate and stearic are the most common fatty acids in
tallow. The amount of FFA from tallow ranges from
0.75 to 7.0%. Titer points in tallow are generally
above 40 ° C. Tallow with a titer point below 40 ° C
is known as grease. The main contents of tallow are:
oleic acid 40-45%, palmitic acid 2437%, stearic acid
14-19%, myristic acid 2-8%, linoleic acid 3-4%, and
lauric acid 0.2%.
Palm Oil
Palm oil is reddish orange because of the carotenoid
dyestuff so if it is to be used as a raw material for
making soap it must be blanched first. Soap made
from 100% palm oil will be hard and hard to foam.
Therefore, if it is to be used as raw material for
making soap, palm oil must be mixed with other
ingredients. The fatty acid content is 42-44% palmitic
acid, 35-40% oleic acid, 10% linoleic acid, 0.3%
linolenic acid, 0.3% arachidonic acid, 0.3% lauric
acid, and 0.5 myristic acid -1%.
Coconut Oil
Coconut oil is a vegetable oil that is often used in the
soap making industry. Coconut oil is pale yellow and
is obtained through the extraction of dried fruit flesh
(copra). Coconut oil has a high saturated fatty acid
content, especially lauric acid around 44-52%, so
coconut oil is resistant to oxidation which causes a
rancid odor.
Marine Oil
Marine oil comes from marine mammals (whales) and
marine fish. Marine oil has a high content of
unsaturated fatty acids (oleic acid), so it must be
partially hydrogenated before being used as raw
material.
Castor Oil
Castor oil is clear and can be used as cosmetics, the
raw material for making biodiesel and soap. Castor oil
has a density of 0.957-0.963 kg/liter, iodine number
82-88 g I2/100 g, saponification number 176-181 mg
KOH/g. Castor oil contains a component of glyceride
or known as an ester compound. The composition of
castor oil fatty acids consisted of 86% riccinoleic
acid, 8.5% oleic acid, 3.5% linoleic acid, 0.5-2.0%
stearic acid, 1-2% dihydroxy stearate acid.
Olive Oil
Olive oil comes from the extraction of olives. High
quality olive oil has a yellowish color. Soap derived
from olive oil has properties that are hard but soft for
the skin. Olives naturally contain several non-soaped
compounds such as phenols, tocopherols, sterols,
pigments, and squalenes. Olive oil also contains triacil
glycerol, most of which is in the form of oleic
monounsaturated fatty acids. The oleic acid content
can reach 55-83 percent of the total fatty acids in
olive oil.
F. Equipments and Materials
a. Equipments
Test tube 6 pieces
Pipette 8 pieces
Measuring flask 1 pieces
Analytical balance 1 piece
Beakers glass 2 pieces
Reflux condenser 1 piece
Burette 2 pieces
Thermometer 1 piece
Spiritus burner 1 piece
Heating mantle 1 piece
Stative 1 piece
Clamp 1 piece
Spatula 1 piece
Hose 1 piece
b. Materials
Palm oil 17 grams
Bulk oil 17 grams
Coconut oil 17 grams
Aquades sufficiently
Ethanol 75 ml
Stearic acid 3 grams
KOH 0,5 N sufficiently
KOH 0,1 N sufficiently
NaOH 1,4 grams
Glycerin 12 mL
Olive oil 3 mL
HCl 0.5 N sufficiently
Alcohol 36 grams
Phenolphtalein Indicator sufficiently
Parfume sufficiently
G. Procedure
1. Soap Making
Making of NaOH Solution
NaOH
- Weighed 1,4 grams
- Dissolved in 3,3 mL of water
- Waited until cool
NaOH solution
Reaction: NaOH (s) + H2O (l) NaOH (aq)
- Weighed 10 grams
- Added 1 grain of stearic acid
- Heated until 70oC
Brownish
colored mixture
- Let it until temperature of 50oC
- Added NaOH solution and stirred
continuously
- Added 12 grams of alcohol and 4
grams of glycerin
- Heated until 50oC
- Stirred
Clear solution
- Let it until cool
- Added 1 mL of olive oil
- Poured into a mold
Soap
Reaction:
Soap Emulsion Properties
a. Making Soap Solution
Soap
- Weighed 0,1 grams
- Dissolved with 6 mL of water
Soap solution
b. Soap Emulsion
3 mL aquades + 3 mL aquades +
5 drops of 5 drops of
coconut oils coconut oils
Soap emulsion
3 mL aquades + 3 mL aquades +
5 drops of palm 5 drops of palm
oils oils
Soap emulsion
3 mL aquades + 3 mL aquades +
5 drops of bulk 5 drops of bulk
oils oils
Soap emulsion
Acid Number
a. Palm oil
Palm oils
- Weighed 5 gram
- Put into erlenmeyer
- Added 25 mL of ethanol
- Added 5 drops of phenolphtalein
- Titrated with 0,1 N of saturated KOH
- Repeated until 3 times
- Calculated the acid number
Acid number
b. Coconut oil
Coconut oils
- Weighed 5 gram
- Put into erlenmeyer
- Added 25 mL of ethanol
- Added 5 drops of phenolphtalein
- Titrated with 0,1 N of saturated KOH
- Repeated until 3 times
- Calculated the acid number
Acid number
c. Bulk oil
Bulk oils
- Weighed 5 gram
- Put into erlenmeyer
- Added 25 mL of ethanol
- Added 5 drops of phenolphtalein
- Titrated with 0,1 N of saturated KOH
- Repeated until 3 times
- Calculated the acid number
Acid number
Reaction:
Saponification Number
a. Coconut oils
2 grams of coconut oils
- Entered into erlenmeyer
- Added 25 mL of 0,5 N KOH
- Refluxed for 30 minutes
-Waited until cool
- Added PP indicator
- Titrated with 0,5 N HCl
- Observed the changes
- Calculated the HCl volume
- Calculated the saponification number
Saponification number
b. Palm oils
2 grams of palm oils
- Entered into erlenmeyer
- Added 25 mL of 0,5 N KOH
- Refluxed for 30 minutes
-Waited until cool
- Added PP indicator
- Titrated with 0,5 N HCl
- Observed the changes
- Calculated the HCl volume
- Calculated the saponification number
Saponification number
c. Bulk oils
2 grams of bulk oils
- Entered into erlenmeyer
- Added 25 mL of 0,5 N KOH
- Refluxed for 30 minutes
-Waited until cool
- Added PP indicator
- Titrated with 0,5 N HCl
- Observed the changes
- Calculated the HCl volume
- Calculated the saponification number
Saponification number
Reaction:
KOH (aq) + C17H33COOH (aq) C17H33COOK (aq) + H2O (l)
KOH (aq) + HCl (aq) KCl (aq) + H2O (l)
2. Unsaturated Fats Testing
Chicken fat Butter Cow fat
- Added 1 mL of chloroform
- Added iodine or bromwater drop by
drop
- Shaked until the color of iodine or
bromwater is unchanged
- Counted the drops
Result
Reaction:
CH3(CH2)14COOH + I2
CH3(CH2)14COOH + Br2
- Added 1 mL of chloroform
- Added iodine or bromwater drop by
drop
- Shaked until the color of iodine or
bromwater is unchanged
- Counted the drops
Result
Reaction:
H. Result of Experiment
Result of Observation
No. Procedure Hypothesis/Reaction Conclusion
Before After
1. Making of NaOH Solution - NaOH = - NaOH + NaOH (s) + H2O (l)
NaOH white solid water = NaOH (aq)
- Weighed 1,4 grams - Water = colorless
- Dissolved in 3,3 mL of water colorless solution
- Waited until cool liquid
NaOH solution
Soap solution
Parfume =
colorless
solution
-Olive oil =
green liquid Palm Oil
- added
Palm Oil stearic acid =
- Weighed 10 grams not dissolve
- Added 1 grain of stearic acid - heated 70oC
- Heated until 70oC = yellow
Brownish solution (++)
colored mixture - added
- Let it until temperature of 50oC NaOH =
- Added NaOH solution and stirred become
continuously thicker
- Added 12 grams of alcohol and 4 grams of - added
glycerin alcohol =
o
- Heated until 50 C yellow
- Stirred solution
- added
Clear solution
glycerin =
become
clump
- added olive
oil = become
- Let it until cool clump
- Added 1 mL of olive oil
- Poured into a mold
Soap
Bulk Oil
Bulk Oil - added
- Weighed 10 grams stearic acid =
- Added 1 grain of stearic acid not dissolve
- Heated until 70oC - heated 70oC
Brownish = dissolve
colored mixture - added
o
- Let it until temperature of 50 C NaOH =
- Added NaOH solution and stirred become
continuously thicker
- Added 12 grams of alcohol and 4 grams of - added
glycerin alcohol =
become
thicker
- added
- Heated until 50oC glycerin =
- Stirred become
clump
Clear solution
- added olive
oil = become
clump
3. Soap Emulsion Properties - Coconut Coconut Oil Emulsion can formed An oil emulsion
a. Making Soap Solution oil = - Soap + H2O because oil is a hydrofob with water
Soap colorless = white so they can't dilute well in added a soap
- Weighed 0,1 grams liquid solution water abd there are an solution will be
- Dissolved with 6 mL of water - Palm oil = - H2O + 5 emulgator with liquid phase long separated
Soap solution light yellow drops of oil = as a soap than the oil
liquid unsoluble (2 emulsion with
- Bulk oil = layers) water that do
yellow - time = 6 s not added a
liquid - H2O + 5 soap solution
- Aquades = drops of oil +
colorless soap solution
b. Soap Emulsion liquid = white
3 mL aquades 3 mL aquades solution
+ 5 drops of + 5 drops of - time = 80 s
coconut oils coconut oils
Palm Oil
- Put into test tube 1 - Put into test - Soap + H2O
- Added 2 mL of soap tube 2 = colorless
solution from coconut oils solution
- Shaken strongly to get an emulsion - H2O + 5
- Allowed to stand and observed until water drops of oil =
and oil separated light yellow
- Noted the time taken to separating in the top and
Soap emulsion colorless in
the bottom
- time = 6 s
- H2O + 5
drops of oil +
soap solution
= white
solution with
bubble on top
3 mL aquades 3 mL aquades - time = 50 s
+ 5 drops of + 5 drops of Bulk Oil
palm oils palm oils
- Soap + H2O
- Put into test tube 1 - Put into test = white
- Added 2 mL of soap tube 2 solution
solution from coconut oils - H2O + 5
- Shaken strongly to get an emulsion drops of oil =
- Allowed to stand and observed until water yellow on top
and oil separated and colorless
- Noted the time taken to separating in the bottom
Soap emulsion - time = 6 s
- H2O + 5
drops oil +
soap solution
= white
solution with
bubble on top
- time = 37 s
3 mL aquades 3 mL aquades
+ 5 drops of + 5 drops of
bulk oils bulk oils
The more longer the time taken to separate, the better quality of oil
so the soap will be better if the time needed to emulsify the oil is getting
longer. Based on the experiment, the order of time taken to separated from
the faster to the slower is bulk oil > palm oil > coconut oil.
3. Acid Number
The third experiment acid number. The purpose of this experiment
is to determine the quality of soap which is shown by the acid number.
Acid number is the number of milligrams of KOH needed to neutralize
free fatty acids from one gram of oil or fat. Acid numbers are used to
measure the amount of free fatty acids contained in oil or fat.
The first step is weighed 5 grams of coconut oil, palm oil, and bulk
oil with analytical balance. Then, put the oils in the three different
erlenmeyer. And then, add 25 mL of ethanol into each erlenmeyer. The
addition of ethanol has a function as a solvent for oil to react with alkaline,
in this case is 0.1 M KOH (colorless solution) base solution. Before doing
the titration, add 5 drops of phenolphtalein (colorless solution) indicator
into the solution. The function of the addition of PP indicator is as a sign
for the end point of the titration, which is when the color of the solution
turns pink. It means that the free fatty acids contained in the oil sample
have been neutralized by the KOH solution. The PP indicator was chosen
because the titrant used was basic (KOH) and the analyte contained acid
which was free fatty acid. The PP indicator is classified as a very weak
acid because it contains a phenol group, in an un-ionized state, the PP
indicator does not change color. But if in an alkaline environment, PP will
ionize more and give a bright color.
The method used is acid-base titration. Titration is based on a
reaction obtained by adding a certain volume of standard solution needed
to react perfectly with an unknown concentration until the equivalent point
is reached. In this titration, 0.1 N KOH was used as a titrant and the
analyte in the form of oil samples consisting of palm oil, coconut oil, and
bulk oil. The acid number is determined by counting the number of
milligrams of KOH required to neutralize free fatty acids contained in 1
gram of oil. The reaction is:
After reach the end point, write down the volume of KOH in every
sample oil. And repeated in three times and calculate the volume average.
Then, we can calculate the acid number using:
Acid number =
The acid number of coconut oil is 2,8 ; then the acid number of
palm oil is 18,3 ; and the acid number of bulk oil is 19,5. Acid number in
oil according to SNI 01-3741-2002 is a maximum of 0.60 mg KOH/g of
oil. The smaller the value of acid number, the better the quality of soap. So
the order of soap quality based on the acid number from the best to the
worst is coconut oil - palm oil - bulk oil.
4. Saponification Number
The next experiment is saponification number. The purpose of this
experiment is to depend the saponification number of each oil. The
saponification number is the number of milligrams of KOH needed to
lather one gram of oil or fat.
The first step is weighed 2 grams of coconut oil, palm oil, and bulk
oil in the analytical balance. Then, entered into three different erlenmeyer.
Then add 25 mL of 0,5 N KOH. The function of alcoholic KOH, which is
alcohol which is used to dissolve fatty acids resulting from hydrolysis in
order to facilitate reaction with bases to form soap.
Next is refluxed for 30 minutes. he principle of the reflux method
is that the volatile solvent used will evaporate at high temperatures, but
will be cooled with a condenser so that the solvent that was in the form of
steam will condense on the condenser and down again into the reaction
container so that the solvent will remain there during the reaction. The
solution is refluxed so that alcoholic KOH and oil can blend perfectly and
react quickly. The reflux process can incorporate alcoholic KOH with oil.
Warming up the reflux process will make it easier for oil to converge with
alcoholic KOH. The other function of reflux process is to evaporate and
liquefy volatile substances. It doesn't use water bath because the solvent
that used is volatile. When using water bath it will easy to evaporate and
usually the solvent is also reactive to fire so that it will be dangerous if the
steam is exposed to fire.
After refluxed for 30 minutes, then let the solution cool. After that,
add phenolphtalein as an indicator in titration process with 0,5 N HCl
(colorless solution). Observed the changes when the indicator start to
change its color. Write down the volume of HCl needed in titration of
coconut oil sample, palm oil sample, and bulk oil sample. The reaction is:
KOH (aq) + C17H33COOH (aq) C17H33COOK (aq) + H2O (l)
KOH (aq) + HCl (aq) KCl (aq) + H2O (l)
Then calculate the saponification number using:
- Weighed 10 grams
- Added 1 grain of stearic acid
- Heated until 70oC
Brownish
colored mixture
- Let it until temperature of 50oC
- Added NaOH solution and stirred
continuously
- Added 12 grams of alcohol and 4
grams of glycerin
- Heated until 50oC
- Stirred
Clear solution
- Let it until cool
- Added 1 mL of olive oil
- Poured into a mold
Solid Soap
Coconut oil Palm oil Bulk oil
- Weighed 10 grams
- Added 1 grain of stearic acid
- Heated until 70oC
Brownish
colored mixture
- Let it until temperature of 50oC
- Added KOH solution and stirred
continuously
- Added 12 grams of alcohol and 4
grams of glycerin
- Heated until 50oC
- Stirred
Clear solution
- Let it until cool
- Added 1 mL of olive oil
- Added parfume
Liquid Soap
Soap solution
b. Soap Emulsion
3 mL aquades + 3 mL aquades +
5 drops of 5 drops of
coconut oils coconut oils
Soap emulsion
3 mL aquades + 3 mL aquades +
5 drops of palm 5 drops of palm
oils oils
Soap emulsion
3 mL aquades + 3 mL aquades +
5 drops of bulk 5 drops of bulk
oils oils
Soap emulsion
= = 18,3
2. Coconut Oil
= = 2,8
3. Bulk Oil
= = 19,5
Saponification Number
N HCl = 0,5 N
Mr HCl = 36,5 gr/mol
Sample weight = 2 grams
1. Coconut Oil
= = 91,25
2. Palm Oil
= = 85,775
3. Bulk Oil
= = 58,4
Documentation
1) Soap Making
No Procedure Picture Explanation
1 Making of NaOH solution weighed 1,4
grams NaOH
solid to make
NaOH
solution for 3
different kind
of soap
1,4 grams of
NaOH solid +
3,3 ml of
aquades.
Become
colorless
NaOH
solution
Making Of Soap
2 Making Of Soap weighed 4
grams of
glycerin for
three
differents
kind of soap
weighed 12
grams of
alcohol for
three
differents
kind of soap
olive oil
Coconout Oil
weighed 10
grams of
coconout oil
weighed 1
gram of
steraic acid
10 grams of
coconout oil
+ 1 gram of
steraic acid
10 grams of
coconout oil
+ 1 gram of
steraic acid
and then
heated until
70
let the
mixture until
50
the mixture
after 50 +
NaOH
solution and
strired
added 12
grams of
alcohol and 4
grams of
glycerin
heated until
50
let the
mixture until
cool
added 1 ml of
olive oil and
poured into a
mold.
soap from
coconout oil
Palm Oil
weighed 10
grams of
palm oil
weighed 1
gram of
stearic acid
added 1 gram
of stearic acid
into 10 grams
of palm oil
heated the
mixture until
70
let until the
temperature
of 50
added NaOH
solution and
stirred
continously
added 12
grams of
alcohol and 4
grams of
glycerin
and then
heated until
50
soap from
palm oil
Bulk Oil
weighed 10
grams of bulk
oil
weighed 1
gram of
stearic acid
hadded 1
gram of
stearic acid
and heated
until 70
let the
temperature
of mixture
until 50
the mixture
added 12
grams of
alcohol and 4
grams of
glycerin
heated until
50
3 mL aquades
+ 5 drops of
coconut oil
and shake it
strongly.
b. Palm Oil 3 mL aquades
+ 5 drops of
palm oil + 1
mL soap
solution and
shake it
strongly.
3 mL aquades
+ 5 drops of
palm oil and
shake it
strongly.
3 mL aquades
+ 5 drops of
bulk oil and
shake it
strongly.
Acid Number
4 acid number wighed 5
grams of
palm oil
palm oil + 25
of ethanol + 5
drops of
phenolphtalei
n + titrated
with 16,3 ml
of KOH
Solution
wighed 5
grams of
coconout oil
coconout oil
+ 25 of
ethanol + 5
drops of
phenolphtalei
n + titrated
with 2,5 ml of
KOH
Solution
wighed 5
grams of bulk
oil
bulk oil + 25
of ethanol + 5
drops of
phenolphtalei
n + titrated
with 2,5 ml of
KOH
Solution
Saponification Number
4 saponification number weighed 2
grams of
coconout oil
2 grams of
palm oil + 25
ml of 0,5 N
KOH and
then refluxed
for 30
minutes (· the
same steps is
done for palm
oil and bulk
oil)
the mixture of
coconout oil
+ 5 drops of
pp indicators
the mixture of
coconout oil
+ 5 drops of
pp indicators
after titrated
with 10 ml of
HCl
weighed 2
grams of
palm oil
2 grams of
palm oil + 25
ml of 0,5 N
KOH then
refluxed for
30 minutes
and the.
Added 5
drops of PP
indicator and
titrated with
9,4 ml HCl
solution
.
weighed 2
grams of bulk
oil
the mixture of
bulk oil + 5
drops of pp
indicators
the mixture of
bulk oil + 5
drops of pp
indicators
after titrated
with 6,4 ml
of HCl
2) Unsaturated Fats Testing
No Procedure Picture Explanation
chicken fat
Chicken fat
Chicken fat +
1 ml of
chloroform
Chicken + 1
ml of
chloroform
and 5 drops of
Bromine water
chicken + 1 ml
of chloroform
and 7 drops of
iodine
Margarine
Margarine
Margarine + 1
ml of
Chloroform
Maragrine + 1
ml of
chloroform + 3
drops of
Bromine water
Margarine + 1
ml of
chloroform + 5
drops of iodine
Cow Fat
Cow fat
Cow fat + 1 ml
of chlororom
Cow fat + 1 ml
of chloroform
+ 7 drops of
bromine water
Cow fat + 1 ml
of clororom +
18 drops of
iodine
Bulk Oil
Bulk oil + 1
ml of
chloroform
Bulk oil + 1
ml of
chloroform +
11 drops of
bromine water
Bulk oil + 1
ml of
chloroform +
19 drops of
iodine
Coconout Oil
Coconout oil
Coconout oil +
1 ml of
chloroform
Coconout oil +
1 ml of
chloroform + 6
drops bromine
water
Coconout oil +
1 ml of
chloroform +
18 drops of
iodine
Palm Oil
Palm oil + 1
ml of
chloroform
Palm oil + 1
ml of
chloroform + 8
drops of
Bromine water
Palm oil + 1
ml of
chloroform + 8
drops of iodine
1. Soap Making
2. Fats