I. Experiment Tittle: Making Soap II. Experiment Date: Tuesday, April 10 2018 (At 10.20 A.M - 4.20 P.M) Iii. Experiment Purpose
I. Experiment Tittle: Making Soap II. Experiment Date: Tuesday, April 10 2018 (At 10.20 A.M - 4.20 P.M) Iii. Experiment Purpose
I. Experiment Tittle: Making Soap II. Experiment Date: Tuesday, April 10 2018 (At 10.20 A.M - 4.20 P.M) Iii. Experiment Purpose
Classification of lipids
Simple lipids
They consist of two types of structural moieties.
They include: glyceryl esters that is esters of glycerol and fatty acids: e.g.
triacylglycerols, mono- and diacylglycerols; cholesteryl esters that is esters
of cholesterol and fatty acids; waxes which are esters of long-chain alcohols
and fatty acids, so including esters of vitamins A and D; ceramides that is
amides of fatty acids with long-chain di- or trihydroxy bases containing 12–
22 carbon atoms in the carbon chain: e.g. sphingosine.
Complex lipids
They consist of more than two types of structural moieties.
They include: phospholipids that is glycerol esters of fatty acids; phosphoric
acid, and other groups containing nitrogen; phosphatidic acid that is
diacylglycerol esterified to phosphoric acid; phosphatidylcholine that is
phosphatidic acid linked to choline, also called lecithin;
phosphatidylethanolamine; phosphatidylserine; posphatidylinositol;
phosphatidyl acylglycerol in which more than one glycerol molecule is
esterified to phosphoric acid: e.g. cardiolipin and diphosphatidyl
acylglycerol; glycoglycerolipids that is 1,2-diacylglycerol joined by a
glycosidic linkage through position sn-3 with a carbohydrate moiety;
gangliosides that is glycolipids that are structurally similar to ceramide
polyhexoside and also contain 1-3 sialic acid residues; most contain an
amino sugar in addition to the other sugars; sphingolipids, derivatives of
ceramides;
sphingomyelin that is ceramide phosphorylcholine; cerebroside: they are
ceramide monohexoside that is ceramide linked to a single sugar moiety at
the terminal hydroxyl group of the base); ceramide di- and polyhexoside that
is linked respectively to a disaccharide or a tri- or oligosaccharide;
cerebroside sulfate that is ceramide monohexoside esterified to a sulfate
group.
Derived lipidsThey occur as such or are released from the other two major
groups because of hydrolysis that is are the building blocks for simple and
complex lipids.
They include:
fatty acids and alcohols; fat soluble vitamins A, D, E and K; hydrocarbons;
sterols. (Bloor W.R. Proc Soc Exp Biol Med, 17, 138, 1920; Christie W.W.
in “Lipid Analysis” Pergamon Press, Oxford, 1982; Pomeranz Y. and
Meloan C.L. in “Food Analysis; Theory and Practice” 4th ed., AVI,
Westport, Connecticut, 1994; Akoh C.C. and Min D.B. “Food lipids:
chemistry, nutrition, and biotechnology” 3th ed. 2008.)
Fats and oils are naturally occurring mixtures of triacylglycerols, also called
triglycerides. They differ in that fats are solids at room temperature and oils
are liquids. We generally ignore this distinction and refer to both groups as
fats.
fatty acids. As these examples indicate, most naturally occurring fatty acids
possess an even number of carbon atoms and an unbranched carbon chain.
The carbon
chain may be saturated or it can contain one or more double bonds. When
double bonds
are present, they are almost always cis. Acyl groups containing 14–20 carbon
atoms are the most abundant in triacylglycerols. A few fatty acids with trans
double bonds (trans fatty acids) occur naturally, but the major source of trans
fats comes from partial hydrogenation of vegetable oils in, for example, the
preparation of margarine. The same catalysts that catalyze the hydrogenation
of the double bonds in a triacylglycerol also catalyze their
stereoisomerization. The mechanism for conversion of a cis to a trans double
bond follows directly from the mechanism of catalytic hydrogenation
(Section 6.1) once one realizes that all of the steps in the mechanism are
reversible.
Fatty acids occur naturally in forms other than as triacylglycerols, and we’ll
see
numerous examples as we go through the chapter. One recently discovered
fatty acid
derivative is anandamide.
Triacontyl hexadecanoate
Fatty acids normally occur naturally as esters; fats, oils, phospholipids, and
waxes all are unique types of fatty acid esters. There is, however, an
important class
of fatty acid derivatives that exists and carries out its biological role in the
form
of the free acid. This class of fatty acid derivatives is described in the
following
section. Ester Hydrolysis in Base: Saponification Unlike its acid-catalyzed
counterpart, ester hydrolysis in aqueous base is irreversible. Ester hydrolysis
in base is called saponification, which means “soap making.” Over 2000
years ago, the Phoenicians made soap by heating animal fat with wood ashes.
Animal fat is rich in glycerol triesters, and wood ashes are a source of
potassium carbonate. Basic hydrolysis of the fats produced a mixture of long-
chain carboxylic acids as their potassium salts.
In one of the earliest kinetic studies of an organic reaction, carried out in the
nineteenth century, the rate of hydrolysis of ethyl acetate in aqueous sodium
hydroxide was found to be first order in ester and first order in base.
Overall, the reaction exhibits second-order kinetics. Both the ester and the
base are
involved in the rate-determining step or in a rapid step that precedes it.
Soaps are water-soluble sodium or potassium salts of fatty acids. Soaps are
made from fats and oils, or their fatty acids, by treating them chemically with
a strong alkali. The fats and oils used in soapmaking come from animal or
plant sources. Each fat or oil is made up of a distinctive mixture of several
different triglycerides. In a triglyceride molecule, three fatty acid molecules
are attached to one molecule of glycerine. There are many types of
triglycerides; each type consists of its own particular combination of fatty
acids. Fatty acids are the components of fats and oils that are used in making
soap. They are weak acids composed of two parts: A carboxylic acid group
consisting of one hydrogen (H) atom, two oxygen (O) atoms, and one carbon
(C) atom, plus a hydrocarbon chain attached to the carboxylic acid group.
Generally, it is made up of a long straight chain of carbon (C) atoms each
carrying two hydrogen (H) atoms.
V. Tools and Materials
Tools :
Beaker Glass 250 mL 1 piece
Reaction Tube 2 pieces
Measure glass 10 mL 1 piece
Measure glass 100 mL 1 piece
Erlenmeyer Flask 3 pieces
Buret 1 piece
Reflux 1 piece
Stative and clamps 1 set
Hot plate 1 piece
Bunsen heater 1 piece
Pipette 10 pieces
Container of soap 9 pieces
Spatula 1 piece
Tripod 1 piece
Thermometer 1 piece
Boiling stone 3 pieces
Stopwatch 1 piece
Plastic pipe sufficiently
Materials :
Coconut oil 22 mL
Palm oil 22 mL
Bulk oil 22 mL
KOH 0,1 N Sufficiently
NaOH Sufficiently
Olive oil 3 mL
NaOH solid 1,4 grams
Aquadest sufficiently
HCl 0,5 N sufficiently
NaOH Solution
3 mL of 3 mL of
aquadest aquadest
Tim
Time
e
3. Acid Number
Volume Of
KOH
- Calculated the acid
number
4. Saponification Number
Volume Of HCl
+
HC OH R1 C O Na
10 grams 10 grams 10 grams H2C OH
O
Palm oil +
stearic acid =
two layer :
upper=stearic
acid grain
(white)
Lower=coconut
oil(yellow
solution)
+ heated until
70oC= yellow
solution
+ cooled until
50oC = two
layer
upper = white
foam
lower = yellow
solution
+ NaOH =
yellow solution
and white cold
+alcohol +
glycerin +
stirred = yellow
solution and
white cold
+heated +stirred
= yellow
solution
+ olive oil +
parfume =
yellow solution
+fragnance
Poured into
container +
Let it room
temperature =
solid, yellow
soap with
fragnance
Bulk oil +
stearic acid =
two layer :
upper=stearic
acid grain
(white)
Lower=coconut
oil(yellow
solution)
+ heated until
70oC= yellow
solution
+ cooled until
50oC = two
layer
upper = white
foam
lower = yellow
solution
+ NaOH =
yellow solution
and white cold
+alcohol +
glycerin +
stirred = yellow
solution and
white cold
+heated +stirred
= yellow
solution
+ olive oil +
parfume =
yellow solution
+fragnance
Poured into
container +
Let it room
temperature =
solid, yellow
soap with
fragnance
2. Character of Soap Emulsion Aquadest + The time of il to
Aquadest = coconut oil = separated is fastly
colorless form two layer than the oil with
Lower = soap solution
3 mL of 3 mL of
Coconut oil = colorless
aquadest aquadest
colorless solution annd
upper = oil
- Entered into reaction - Entered into Palm oil = solution )
tube reaction tube yellow
- Added 5 drops oil - Added 5 Aquadest +
- Added 2 mL of soap drops oil Bulk oil = palm oil = form
solution - Shaked until yellow two layer
- Shaked until get get emulsion Upper = light
emulsion - Observed the Soap solution yellow solution
- Observed the separation coconut oil = Lower =
separation - Written the colourless clourless
- Written the result result solution
Soap solution
Tim palm oil = white Aquadest + bulk
Time solution oil = form 2
e
layer
Soap solution Lower = light
bulk oil = solution
yellowish Upper = oil
Time to
separated
Aquadest +
coconut oil +
soap solution =
form two layer
Lower =
colorless
solution
upper = white
foam
Aquadest +
palm oil + soap
solution= form
two layer
Upper = turbid
solution
Lower =
clourless
solution
Aquadest + bulk
oil = form 2
layer
Lower = turbid
solution
Upper = oil
Time to
separated
3. Acid Number Coconut oil = Volume of The value of acid number The acid number
colourless KOH ( coconut allowed according to SNI-04- of palm oil equal
10 grams 10 grams 10 grams solution oil )= 0,7 mL 7182-2006, ie 0, 8 mg KOH / with coconut oil
coconut bulk oil palm oil (light pink gram of oil. (Anonym,2015) which are lower
oil Palm oil = solution) than the acid
yellow number of bulk
Volume of oil,.
- Entered into Bulk oil = KOH (palm
rerlenmeyer flask yellow oil)= 0,7 mL
- Added 25 mL of ethanol (light yelow-
- Added 5 drops of PP Ethanol = pink solution)
indicator colourless
- Titration with standart solution Volume of
KOH ( bulk
PP indicator = oil)= 0,8 mL
Volume Of colourless (light yelow-
KOH solution pink solution)
1. Making Soap
The Title of this experiment is making soap which have purpose to know how to
make the flow chart of making soap, determine the reaction equation on making soap,
explaining the difference soap product made using NaOH, making soap emulsion,
explaining about process make water soap emulsion with oil, and the last is determine
the quality of oil based on peroxide number.This experiment consist of five sub-title,
that are making soap that have purpose to know the flow work of making soap;
character of soap emulsion that have purpose to know the character of the soap emulsion
and explain the process of forming a soap water emulsion with oil; Acid number that
have purpose to determine the quality of oil based on the acid number; And the last
saponification number that have purpose to determine the quality of oil based on the
saponification number.
The first experiment is making soap from three kind of oil, that are coconut oil,
palm oil, and bulk oil. The purpose of fixed the kind of oil as the manipulation variable
is to know the characteristic of soap using many kind of oil, because every oil have its
own characteristic. Coconut oil is colourless. The first procedure is prepared solution of
NaOH. NaOH is white crystal, balanced 0.4 grams than entered into beaker glass. Then
added 3,3 mL of clourless aquadest. Stirred it until diluted. And colourless NaOH
solution ready to used. Then prepared a clean test tube, given label “tube 1”, also
prepared 1 gram of grain stearic acid. Then entered coconut oil into tube 1. Added 1
gram of stearic acid into tube 1. The function of added stearic acid is to make the soap
become solid and stabilize the foam. Then the solution heated until 70˚C, its heated until
70˚C because the melting point of stearic acid is 70˚C or can be said that on that
temperature the stearic acid had been diluted into coconut oil. If it heated up to 70˚C, oil
will oxidized become brown solution, it have connection with peroxide number, the
value of disturbance oil caused by autooxydation. There is no colour changing on
coconut oil after heated. Cooled it until 50˚C. While waiting the temperature decrease,
measured 12 mL of ethanol and 4 mL of glycerin using graduated cylinder. On 50˚C, the
solution formed two layer. Upper layer is white solid foam, meanwhile the lower layer is
colourless solution. Then moved the solution into beaker glass, added colourless NaOH
solution, colourless ethanol and colourless glycerin. The function of adding NaOH is to
hydrolized coconut oil because NaOH is strong acid, so it will formed glycerol and salt
of fat acid or soap. The reaction is,
In this experiment do not used KOH because if it used KOH will formed liquid
soap. Meanwhile the function of ethanol is to make the transparant soap, which have the
characteristic easy diluted into water and fats. Glycerin make the skin smooth. The
colour of solution is colourless solution with white glob. Heated it until clear. While
heating, kept stirred it to make the solution go easier to diluted. After diluted, the colour
of this solution changing become yellowish. On hot condition added 1 mL of colurless
olive oil and parfume sufficiently. Fastly, poured liquid soap into container. Waited it
until become solid.
The colour of bulk oil is yellow. The first procedure is prepared solution of
NaOH. NaOH is white crystal, balanced 0.4 grams than entered into beaker glass. Then
added 3,3 mL of clourless aquadest. Stirred it until diluted. And colourless NaOH
solution ready to used. Then prepared a clean test tube, given label “tube 2”, also
prepared 1 gram of white grain stearic acid. Then entered bulk oil into tube 2. Added 1
gram of stearic acid into tube 1. The function of added stearic acid is to make the soap
become solid and stabilize the foam. Then the solution heated until 70˚C, its heated until
70˚C because the melting point of stearic acid is 70˚C or can be said that on that
temperature the stearic acid had been diluted into bulk oil. If it heated up to 70˚C, oil
will oxidized become brown solution, it have connection with peroxide number, the
value of disturbance oil caused by autooxydation. There is no colour changing on bulk
oil after heated. Cooled it until 50˚C. While waiting the temperature decrease, measured
12 mL of ethanol and 4 mL of glycerin using graduated cylinder. On 50˚C, the solution
formed two layer. Upper layer is white solid foam, meanwhile the lower layer is yellow
solution. Then moved the solution into beaker glass, added colourless NaOH solution,
colourless ethanol and colourless glycerin. The function of adding NaOH is to
hydrolized bulk oil because NaOH is strong acid, so it will formed glycerol and salt of
fat acid or soap. The reaction is
In this experiment do not used KOH because if it used KOH will formed liquid
soap. Meanwhile the function of ethanol is to make the transparant soap, which have the
characteristic easy diluted into water and fats. Glycerin make the skin smooth. The
colour of solution is yellow solution with light yellow glob. Heated it until clear. While
heating, kept stirred it to make the solution go easier to diluted. After diluted, the colour
of this solution changing become mustard yellow. On hot condition added 1 mL of
colurless olive oil and parfume sufficiently. Fastly, poured liquid soap into container.
Waited it until become solid.
The colour of palm oil is yellow. The first procedure is prepared solution of
NaOH. NaOH is white crystal, balanced 0.4 grams than entered into beaker glass. Then
added 3,3 mL of clourless aquadest. Stirred it until diluted. And colourless NaOH
solution ready to used. Then prepared a clean test tube, given label “tube 3”, also
prepared 1 gram of white grain stearic acid. Then entered palm oil into tube 3. Added 1
gram of stearic acid into tube 2. The function of added stearic acid is to make the soap
become solid and stabilize the foam. Then the solution heated until 70˚C, its heated until
70˚C because the melting point of stearic acid is 70˚C or can be said that on that
temperature the stearic acid had been diluted into palm oil. If it heated up to 70˚C, oil
will oxidized become brown solution, it have connection with peroxide number, the
value of disturbance oil caused by autooxydation. There is no colour changing on palm
oil after heated. Cooled it until 50˚C. Waiting the temperature decrease, measured 12
mL of ethanol and 4 mL of glycerin using graduated cylinder. On 50˚C, the solution
formed two layer. Upper layer is white solid foam, meanwhile the lower layer is yellow
solution. Then moved the solution into beaker glass, added colourless NaOH solution,
colourless ethanol and colourless glycerin. The function of adding NaOH is to
hydrolized palm oil because NaOH is strong acid, so it will formed glycerol and salt of
fat acid or soap. The reaction is
In this experiment do not used KOH because if it used KOH will formed liquid
soap. Meanwhile the function of ethanol is to make the transparant soap, which have the
characteristic easy diluted into water and fats. Glycerin make the skin smooth. The
colour of solution is yellow solution with light yellow glob. Heated it until clear. While
heating, kept stirred it to make the solution go easier to diluted. After diluted, the colour
of this solution changing become mustard yellow. On hot condition added 1 mL of
colurless olive oil and parfume sufficiently. Fastly, poured liquid soap into container.
Waited it until become solid.
First, prepare six test tube that entered 3 mL of. The tube I (there 3 tube) added
5 drops coconut oil, palm oil and bulk oil in each test tube form two layer at upper its oil
and lower its aquadest then shaked strongly until get emulsion. Then, waited it until the
solution seprated and calculated the time. The time of the solution to separated are, the
coconut oil is 56 seconds, palm oil is 48 seconds and the bulk oil is 45 seconds. Then
the tube II added 5 drops coconut oil, palm oil and bulk oil in each test tube. After that
added 2 mL of soap solution in each test tube. Then, shaked strongly until get emulsion.
Then, waited it until the solution separated. The time of the solution to separated are the
coconut oil is 01.45 minutes, palm oil is 02.30 minutes and bulk oil is 04.06 minutes.
The solution form two layer, in coconut oil in upper form white foam and colourless
solution, in palm oil form white foam and turbid solution and in bulk oil form white
foam and turbid solution
From this data we know that bulk oil is lowest to separated it means that bulk oil
is good emulsion. The good emulsion can bonding C groups of oil and OH groups of
aquades strongly, therefore oil and water are difficult to separated because of the bond.
3. Acid Number
The purpose of this experiment is to measure the amount of free fatty acid in
lipid. Acid number are showing the number of free fatty acids in the oil caused
hydrolyze reaction of oil. The greater this number means the higher free fatty acid
content, while the free fatty acids contained in the sample can be derived from
hydrolysis processes or because of poor processing. Because the hydrolysis process can
take place with the addition of acid and assisted by heat. The reaction occurring in the
hydrolysis process is as follows. The higher the acid number the lower the quality
(Julianty, 2008)
In this experiment we used coconut oil, palm oil and bulk as samples. The each
sample are weighed 10 grams then entered into erlenmeyer flask then added 25 mL of
ethanol. The function of adding ethanol, to dissolve lipid in the sample in order to react
with base. After that added 5 drops of PP indicators to indicate that the solution is base
and to determine the aquivalent point. Then titration with KOH 0,1 N. After titration, the
sample coconut oil form pink solution, sample palm oil form yellow-pink solution and
bulk oil form yellow pink solution. the used of KOH is to determine the free fatty acids
of oils. The volume of KOH required of coconut oil is 0,7 mL, with palm oil is 0,7 mL
and with bulk oil is 0,8 mL.
After calculated, obtained results free fatty acids of palm oil is 0,392; coconut oil
is 0,392 and bulk oil is 0,448. The value of acid number allowed according to SNI-04-
7182-2006, ie 0, 8 mg KOH / gram of oil. If the acid number exceeds the limit specified
by SNI, then the oil is not suitable for use. So based on the data obtained, for three
samples the oil still has an acid number that can be tolerated in accordance with the
standard of SNI. (Anonym, 2015).
4. Saponification Number
Saponification value is expressed by potassium hydroxide in mg required to
saponify one (1) gram of fat. It depends on the kind of fatty acid contained in the fat.
Measurement of saponification value is performed according to the below listed official
test methods. Here we test a sample of fatty acid. The sample is first saponified by
adding 0.5mol/L potassium hydroxide ethanol, and then the excessive potassium
hydroxide is titrated with 0.5mol/L hydrochloric acid until the endpoint is reached. EP is
determined by the maximum inflexion point on titration curve.
R COOH + KOH → R COOK + H2O
KOH + HCl → KCl + H2O
1,5-2 grams of coconut oil, 1,5-2 gram of bulk oil and 1,5-2 grams palm oil
entered into Erlenmeyer flask and added with 25 mL KOH solution 0,5 N.
Reflacted for 30 minutes and waited until cool. The mixture that has been cool
then titrated with HCl 0,5 N with PP indicator. Written the HCl volume for
titration. Then calculated saponification number for each oil.
The reflaction process is used to purify the contain of mixture. So KOH solution
will evaporate and resulting the oil that has been mix with KOH solution.
The saponification number can be obtained from the formula:
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐻𝐶𝑙 𝑥 𝑁 𝐻𝐶𝑙 𝑥 𝑀𝑟 𝑜𝑓 𝐻𝐶𝑙
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
From all oils, the highest saponification number obtained from bulk oil. The
saponification value is the number of milligrams of KOH required to neutralize
the fatty acids resulting from the complete hydrolysis of 1g of fat.
The saponification value gives an indication of the nature of the fatty acids
constituent of fat and thus, depends on the the average molecular weight of the
fatty acids constituent of fat. The greater the molecular weight (the longer the
carbon chain), the smaller the number of fatty acids is liberated per gram of fat
hydrolyzed and therefore, the smaller the saponification number and vice versa.
The highest saponification number is bulk oil. It means that the constituent of
fatty acid in the oil is big. It means that bulk oil is not health to use, if compares
with palm oil and coconut oil because the constituent of fat in this oil is highest
between palm oil and coconut oil.
X. Refferences:
Akoh C.C. and Min D.B. 2008. Food lipids: chemistry, nutrition, and
biotechnology 3th ed.
Anonym. 2015. Penentuan Bilangan Asam Pada Minyak dengan Metode Titrasi
Asam Basa. https://dokumen.tips/documents/penentuan-bilangan-asam.html
Acessed on 16 April 2018 at 20.11 p.m
Bloor W.R. Proc Soc Exp Biol Med, 17, 138, 1920; Christie W.W. in Lipid
Analysis Pergamon Press, Oxford, 1982;
Carey. A. Francis. 2008. Organic Chemistry. Americas, New York, NY 10020:
The McGraw-Hill Companies, Inc.
Fessenden. Fessenden. 1986. Kimia Organik Edisi Ketiga. Jakarta: Erlangga.
Julianty, Riza. 2008.Pengendalian Mutu Argoindustri. Bandung.
https://dokumen.tips/documents/penentuan-bilangan-asam.html Vedca Press.
Acessed on 16 April 2018 at 20.10 p.
Pomeranz Y. and Meloan C.L. in Food Analysis; Theory and Practice 4th ed.,
AVI, Westport, Connecticut, 1994;
Online. http://www.kyoto-kem.com/en/pdf/industry/FatVegetableOil/ETIB-
99307.pdf. Accessed on April 16 2018
Online. http://www.mvla.net/view/27581.pdf. Accessed on April 16 2018
XI. Attachment
1. Question’s Answer
QUESTION
1. How to make hard and soft soap? (on lanes work)
2. Write the reaction of making soap
3. How is the lanes work of soap emulsion
4. Explain how are the process of making soap
5. Make the problem formula if for making soap used NaOH with KOH with the
same concentration, procedure and its tools and materials
6. Identify the variabel (manipulation, respond, and control)
7. Make the procedure
ANSWER
1. Solid Soap
10 grams coconut 10 grams bulk 10 grams palm
oil oil oil
3 ml aquadest 3 mL aquadest
Time Time
4. Soap made through saponification reaction, on this experiment, soap reacted
with NaOH or KOH to form liquid or solid soap.
5. How was the influence of NaOH or KOH with the result of soap ?
6. Manipulation variable : NaOH and KOH
Control variable : the procedure, Tools, volume of palm oil,
aquadest, alcohol, glycerin, dye and perfume
Respond variable : characteristic of soap
7. The lanes work
10 grams palm
oil
Tube 1 Tube 1
3. Documentation
Tools and Materials
Palm Oil Coconut Oil Bulk Oil
Glycerin
Experiment 1
Balanced 1.4 grams of NaOH Oil entered into test tube
Titration process
Coconut Oil before titration
Bulk oil after titration
Palm Oil after titration