Textual Amendments
This method describes the determination of free fatty acids in olive oils and olive pomace oils. The content of free fatty acids is expressed as acidity calculated as the percentage of oleic acid.
A sample is dissolved in a mixture of solvents and the free fatty acids present titrated using a potassium hydroxide or sodium hydroxide solution.
All the reagents should be of recognized analytical quality and the water used either distilled or of equivalent purity.
Neutralize precisely at the moment of use with the potassium hydroxide solution (3.2), with the addition of 0,3 ml of the phenolphthalein solution (3.3) per 100 ml of mixture.
The exact concentration of potassium hydroxide solution (or sodium hydroxide solution) must be known and checked prior to use. Use a solution prepared at least five days before use and decanted into a brown glass bottle with a rubber stopper. The solution should be colourless or straw coloured.
If phase separation is observed when using aqueous solution of potassium hydroxide (or sodium hydroxide), replace the aqueous solution by an ethanolic solution.
The solution may also be prepared without distillation as follows: to 1 000 ml of ethanol (or water) add 4 ml of aluminium butylate and leave the mixture for several days. Decant the supernatant liquid and dissolve the required quantity of potassium hydroxide (or sodium hydroxide). The solution is ready for use.
Usual laboratory equipment including:
Analytical balance;
250 ml conical flask;
10 ml burette class A, graduated in 0,05 ml, or equivalent automatic burette.
When the sample is cloudy, it should be filtered.
Take a sample depending on the presumed acidity in accordance with the following table:
Expected acidity (oleic acidity g/100 g) | Mass of sample (g) | Weighing accuracy (g) |
---|---|---|
0 to 2 | 10 | 0,02 |
> 2 to 7,5 | 2,5 | 0,01 |
> 7,5 | 0,5 | 0,001 |
Weigh the sample in the conical flask (4.2).
Dissolve the sample (5.2) in 50 to 100 ml of the previously neutralized mixture of diethyl ether and ethanol (3.1).
Titrate while stirring with the 0,1 mol/l solution of potassium hydroxide (or sodium hydroxide) (3.2) (see Note 4) until the indicator changes (the colour of the coloured indicator persists for at least 10 seconds).
Carry out a second determination only if the first result is higher than the specified limit for the category of the oil.
Acidity as a percentage of oleic acid by weight is equal to:
where:
=
the volume of titrated potassium hydroxide solution (or sodium hydroxide) used, in millilitres;
=
the exact concentration in moles per litre of the titrated solution of potassium hydroxide (or sodium hydroxide) used;
=
282 g/mol, the molar mass in grams per mole of oleic acid;
=
the mass of the sample, in grams.
Oleic acidity is reported as follows:
to two decimal places for values from 0 up to and including 1;
to one decimal place for values from 1 up to and including 100.]