Practical Manual ---
Chemical Analysis and EXPERIMENT 24 DETERMINATION OF
Quality Assurance
SAPONIFICATION VALUE
IN OILS AND FATS
Structure
24.0 Objectives
24.1 Introduction
24.2 Principle
24.3 Requirements
24.4 Procedure
24.5 Calculation
24.6 Results and Inference
24.7 Precautions
24.0 OBJECTIVES
After attending to this experiment, we shall be able to:
• learn to perform determination of saponification value in oils and fats.
24.1 INTRODUCTION
The number of milligrams of potassium hydroxide required to saponify completely one
gram of oil or fat. When fat is saponified by refluxing with a known excess of alcoholic
potassium hydroxide solution, the triglycerides hydrolyze, glycerol and soap are formed.
The alkali consumed for this hydrolysis is a measure of the saponification value, which
is determined by titrating the excess alkali with standard hydrochloric acid.
24.2 PRINCIPLE
The material is saponified by refluxing with a known excess of alcoholic potassium
hydroxide solution. The alkali consumed for saponification is determined by titrating
the excess alkali with standard hydrochloric acid.
24.3 REQUIREMENTS
Apparatus
Conical Flasks -250 to 300 ml capacity.
Reflux Condenser-at least 65 cm long.
Water-Bath or Electric Hot-Plate with Rheostat Control
Reagents
Alcoholic Potassium Hydroxide Solution - Dissolve 35 to 40 g of KOH in 20 ml of
distilled water, and add sufficient aldehyde-free rectified spirit to make up to 1000 ml.
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Allow to stand overnight, decant the clear liquid and keep in a bottle closed tight with Determination of
a cork or rubber stopper. Saponification Value in
Oils and Fats
Aldehyde-Free Rectified Spirit -Reflux 1.2 litres of rectified spirit for 30 min. in a
round-bottom flask with 10 g of KOH and 6 g of granulated aluminium (or aluminium
foil). Distil and collect one litre after discarding the first 50 ml.
Phenolphthalein Indicator Solution - Dissolve 1.0 g of phenolphthalein in 100 ml of
rectified spirit.
Note - When testing oils or fats which give dark-coloured soap solutions, the observation
of the end point of the titration may be facilitated either (a) by using thymolphthalein, or
alkali blue 6B in place of phenolphthalein or (b) by adding 1 ml of a 0.1 % (w/v)
solution of methylene blue in water to each 100 ml of phenolphthalein indicator solution
before the titration.
Standard Hydrochloric Acid (0.5 N).
24.4 PROCEDURE
Melt the sample, if it is not already liquid, and filter through a filter paper to remove any
impurities and the last traces of moisture. Make sure that the sample is completely dry.
Mix the sample thoroughly, and weigh accurately by difference about 1.5 to 2.0 g of
the sample in a conical flask. Add 25 ml of the alcoholic KOH solution and connect the
reflux air condenser to the flask. Heat the flask on a water-bath or an electric hot plate
for not more than 1 hr. Boil gently but steadily until the sample is completely saponified
as indicated by absence of any oily matter and appearance of clear solution. After the
flask and condenser have cooled somewhat, wash down the inside of the condenser
with about 10 ml of hot ethyl alcohol neutral to phenolphthalein. Add about 1 ml of
phenolphthalein indicator solution, and titrate with standard hydrochloric acid. Prepare
and conduct a blank determination at the same time.
24.5 CALCULATION
56.1 (B − S) × N
Saponification value = ——————
W
Where,
B = volume, in ml, of HCl required for the blank,
S = volume, in ml, of HCl required for the sample,
N = normality of HCl, and
W = weight, in g, of the material taken for the test.
24.6 RESULTS AND INFERENCE
The mean of the results of two determinations should be reported. The difference
between the results of two determinations carried out simultaneously or in rapid
succession by the same analyst (repeatability) shall not exceed 0.5. The saponification
value of commonly used edible oils is given as below.
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Practical Manual --- Type of Oil Sap. Value Type of Oil Sap. Value
Chemical Analysis and
Quality Assurance
Coconut oil 250-264 Safflower oil 189-195
Cottonseed oil 190-198 Sunflower oil 188-194
Groundnut oil 188-195 Soybean oil 189-195
Mustard oil 169-177 Rice bran oil 180-195
Sesame oil 188-193 Palm oil 195-205
24.7 PRECAUTIONS
• Alcoholic KOH should be prepared overnight.
• Refluxing should not be done for more than one hour.
• Condenser should be carefully washed with alcohol.
• Blank determination should be carried out simultaneously along with the sample.
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