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SOP: Ester Value of Essential Oils

GIFSQ — Global Institute for Food Safety & Quality

Principle

The esters in the oil are saponified by refluxing with a known excess of alcoholic KOH; the unused alkali is back-titrated with standard HCl, and the alkali consumed is converted to the ester value and to the percentage of esters using the molecular weight of the ester.

Apparatus required

  • Conical flask of 250 ml capacity with ground glass joint
  • Condenser which fits the flask

Reagents

a. 0.5 N alcoholic KOH solution: dissolve 33 g of KOH in 1000 ml of rectified spirit, allow to stand, and decant or filter; adjust to 0.5 N using alcohol.

b. 0.1 N alcoholic KOH solution.

c. 0.5 N HCl.

d. Phenolphthalein indicator.

Procedure

Weigh the sample into the conical flask accurately (±1 mg), depending upon the expected ester value — if the value is below 50, the weight of material required is 4.5 to 5.0 g; for every increase of 20 in the ester value up to 140, reduce the weight taken by 0.5 g, and thereafter by 0.2 to 0.3 g

↓

Add 25 ml of 0.5 N alcoholic KOH solution and 10 drops of phenolphthalein indicator, and reflux for 1 hr unless otherwise specified (see the analytical conditions for bergamot oil below)

↓

Cool and titrate the excess alkali with 0.5 N HCl using phenolphthalein as indicator

↓

Carry out a blank determination in the same way except for the material

Calculation

Ester value = ((Blank titre − Sample titre) × N of HCl × 56.1) / Weight of sample

% Esters = (Ester value × Molecular wt of ester) / 561

Where,

  • Blank titre = ml of 0.5 N HCl used in the blank titration
  • Sample titre = ml of 0.5 N HCl used in the sample titration
  • N of HCl = normality of the HCl solution
  • Weight of sample = weight of the oil taken

Analytical conditions:

OilWt of sample (g)Reflux time (min)Factor for calculation: g of ester per ml of 0.5 N KOH
Bergamot oil2.0300.09815 as linalyl acetate

References

Ranganna, S., Handbook of Analysis and Quality Control for Fruit and Vegetable Products, 2nd edition.

  1. Methods of Sampling and Test for Natural and Synthetic Perfumery Material (First Revision), IS: 326—1968, ISI, New Delhi.
  2. EOA Specifications and Standards, EOA No. 1, Essential Oil Association of USA, Inc.