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05 Preparation of Aspirin
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ESTD–(2010) DTECODE:EN3351
InnovativeEngineers’andTeachers’EducationSociety’s
ApprovedbyAICTE,DTE&AffiliatedtoUniversityofMumbai,NAACAccredited
Experiment No.-03
Method for Determination of Acid Value in Oils And Fats
AIM: To determine the Acid value In Oils And Fats.
REQUIREMENTS: Oil sample, Phenolphthatlein indicator, 0.1N KOH solution, Conical flask,
Weighing machine
THEORY:
The acid value is defined as the number of milligrams of Potassium hydroxide required to
neutralize the free fatty acids present in one gram of fat. It is a relative measure of rancidity as
free fatty acids are normally formed during decomposition of triglycerides. The value is also
expressed as per cent of free fatty acids calculated as oleic acid, lauric, ricinoleic and palmitic
acids.The acid value is determined by directly titrating the oil/fat in an alcoholic medium
against standard potassium hydroxide/sodium hydroxide solution.The value is a measure of the
amount of fatty acids, which have been liberated by hydrolysis from the glycerides due to the
action of moisture, temperature and/or lipolytic enzyme lipase.
PREPARATIONS:
a) Phenolphthalein indicator solution:
Dissolve one gram of phenolphthalein in 100mL of ethyl alcohol.
b) Ethyl alcohol:
1) Ninety-five percent alcohol or rectified spirit neutral to phenolphthalein indicator.
2) Ninety-five percent alcohol or rectified spirit neutral to Alkali blue 6B indicator in case of rice
bran oil or rice bran oil based blended oil or fats.
c) Standard aqueous Potassium hydroxide or sodium hydroxide solution 0.1 or 0.5 N. The
solution should be colourless and stored in a brown glass bottle. For refined oils, the strength of
the alkali should be fixed to 0.1 N.
7
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Add:Opp.GajananMaharajTemple,Kanhor,Badlapur(W),Tal:Ambernath,Dist:Thane421503,Mumbai
Web:bharatenggcollege.com Email:info@bharatedu.co.in Phone:7666615915
ESTD–(2010) DTECODE:EN3351
InnovativeEngineers’andTeachers’EducationSociety’s
ApprovedbyAICTE,DTE&AffiliatedtoUniversityofMumbai,NAACAccredited
PROCEDURE:
a) Weigh accurately 2.0g of the cooled oil sample in a 250 mL conical flask.
b) Add 50 mL of freshly neutralised hot ethyl alcohol and about one ml of phenolphthalein
indicator solution.
c) Heat the mixture for about fifteen minutes in water bath (75-80°C)
d) Titrate while hot against standard alkali solution shaking vigorously during the titration.
e) End point using phenolphthalein indicator shall be from colourless to light pink
(Persisting for 15 sec.)
Note: Noting burette reading after “obtaining dark pink colour as end point should be avoided
as it will lead to erroneous result
g) The weight of the oil/fat taken for the estimation and the strength of the alkali used for
titration shall be such that the volume of alkali required for the titration does not exceed
10mL.
OBSERVATIONS:
Solution in Conical flask: 2.0ml Oil sample + Ethyl alcohol
I II III C.B.R
Initial
Final
Difference
8Page
Add:Opp.GajananMaharajTemple,Kanhor,Badlapur(W),Tal:Ambernath,Dist:Thane421503,Mumbai
Web:bharatenggcollege.com Email:info@bharatedu.co.in Phone:7666615915
ESTD–(2010) DTECODE:EN3351
InnovativeEngineers’andTeachers’EducationSociety’s
ApprovedbyAICTE,DTE&AffiliatedtoUniversityofMumbai,NAACAccredited
CALCULATION:
Acid value = (56.1 xV xN)/W
Where,
V = Volume in mL of standard potassium hydroxide or sodium hydroxide used
N = Normality of the potassium hydroxide solution or Sodium hydroxide solution; and
W = Weight in gm of the sample
RESULT:
The acid value of given oil sample is____________.
9Page
Add:Opp.GajananMaharajTemple,Kanhor,Badlapur(W),Tal:Ambernath,Dist:Thane421503,Mumbai
Web:bharatenggcollege.com Email:info@bharatedu.co.in Phone:7666615915
ESTD–(2010) DTECODE:EN3351
InnovativeEngineers’andTeachers’EducationSociety’s
ApprovedbyAICTE,DTE&AffiliatedtoUniversityofMumbai,NAACAccredited
Experiment No.-04
Determination of Saponification value of the given oil/fat
REQUIREMENTS: Oil or fat sample, Conical flask, Water bath,Burette and Pipette, 0.5 N HCl,
Phenolphthalein, 0.5 N alcoholic potassium-hydroxide solution.
THEORY:
PROCEDURE:
About 2 g of the given oil or fat is taken in a conical flask but weighed accurately (w g). The
oil/fat is dissolved in 20 ml of 0.5 N alcoholic potassium-hydroxide solution. Then the reaction
mixture is refluxed on a water-bath for an hour. The resulting solution is cooled and titrated
against a 0.5 N HCl solution adding 1 ml of phenolphthalein. The number of ml of acid required
is noted (a). An exactly identical blank experiment (leaving the fat or oil) is performed. Number
10
Add:Opp.GajananMaharajTemple,Kanhor,Badlapur(W),Tal:Ambernath,Dist:Thane421503,Mumbai
Web:bharatenggcollege.com Email:info@bharatedu.co.in Phone:7666615915
ESTD–(2010) DTECODE:EN3351
InnovativeEngineers’andTeachers’EducationSociety’s
ApprovedbyAICTE,DTE&AffiliatedtoUniversityofMumbai,NAACAccredited
Observation table:
I II III C.B.R
Initial A ml
Final
Difference
Indicator: Phenolphthalein
Color change: Pink to colourless
Observation table:
I II III C.B.R
Initial B ml
Final
Difference
11
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Add:Opp.GajananMaharajTemple,Kanhor,Badlapur(W),Tal:Ambernath,Dist:Thane421503,Mumbai
Web:bharatenggcollege.com Email:info@bharatedu.co.in Phone:7666615915
ESTD–(2010) DTECODE:EN3351
InnovativeEngineers’andTeachers’EducationSociety’s
ApprovedbyAICTE,DTE&AffiliatedtoUniversityofMumbai,NAACAccredited
CALCULATION:
RESULT:
12
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Add:Opp.GajananMaharajTemple,Kanhor,Badlapur(W),Tal:Ambernath,Dist:Thane421503,Mumbai
Web:bharatenggcollege.com Email:info@bharatedu.co.in Phone:7666615915