EUROPEAN COMMISSION

Brussels, 19.10.2026

SWD(2026) 317 final

COMMISSION STAFF WORKING DOCUMENT

Accompanying the document

Proposal for a
COUNCIL DECISION

on the position to be taken on behalf of the European Union in the Council of Members of the International Olive Council as regards the trade standard applying to olive oils and olive pomace oils and two methods of analysis

{COM(2026) 562 final}

DRAFT DECISION No DEC III.X/123-VI/2026

REVISING THE TRADE STANDARD APPLYING TO OLIVE OILS AND

OLIVE-POMACE OILS

DECISION DEC-III.X/123-VI/2026

REVISING THE TRADE STANDARD APPLYING TO OLIVE OILS AND OLIVE- POMACE OILS

The Council of Members of the International Olive Council,

Having regard to the International Agreement on Olive Oil and Table Olives, 2015, and in particular Article I "Objectives of the Agreement" concerning the standardisation of national and international legislation relating to the physico-chemical and organoleptic characteristics of olive oils, olive pomace oils and table olives in order to avoid any barriers to trade, and Chapter VI "Standardisation provisions";

Having regard to the recommendation made by the Committee on Chemistry and Standardisation at its 18th meeting, within the framework of the 123rd session of the Council of Members;

Considering the work carried out by chemists concerning the application of methods and studies carried out on olive oils presenting non-standard parameters;

Considering the unanimous position agreed by the chemists at their meeting on 24 and 25 March 2026 regarding:

-The replacement of the flash point with residual hexane content, with a limit of 1,000 mg/kg.

-The replacement of the FOSFA International method with the ISO 9832 method.

-The inclusion of the method for the determination of triacylglycerol composition and the composition and content of diacylglycerols in vegetable oils by capillary gas chromatography (COI/T.20/Doc. No. 32/Rev. 1).

-The inclusion of the method for the determination of the fatty acid composition in olive oils and olive pomace oils by gas chromatography (COI/T.20/Doc. No. 33/Rev.2).

-The inclusion of the revised method for the determination of acidity in olive oils and olive pomace oils (COI/T.20/Doc. No. 34/Rev. 2).

Príncipe de Vergara, 154 - 28002 Madrid - Spain                     E-Mail: iooc@internationaloliveoil.org

Tel: +34 915 903 638                                     Internationaloliveoil.org

Decides

1.To adopt the Trade Standard for Olive Oils and Olive-Pomace Oils COI/T.15/NC No. 3/Rev. 23, attached to this decision, which replaces and repeals the previous version (COI/T.15/NC No. 3/Rev. 22) of June 2026.

2.Members shall, in accordance with their respective legislations, take all appropriate measures to apply the adopted standard and shall communicate these measures to the Executive Secretariat as soon as they have been implemented.

3.Non-member countries engaged in international trade in olive oils and olive pomace oils are invited to take the adopted standard into consideration and to align their regulations with its provisions.

Príncipe de Vergara, 154 - 28002 Madrid - Spain                     E-Mail: iooc@internationaloliveoil.org

Tel: +34 915 903 638                                     Internationaloliveoil.org

Trade Standard

Applying to Olive Oils

and Olive Pomace Oils

COI/T.15/NC. No. 3/Rev. 223
June 2026
English / Original: French

Index

Abbreviation List    2

Trade Standard Applying to Olive Oils and Olive Pomace Oils    3

1.Scope    3

2.Designations and Definitions    3

3.Purity Criteria    5

4.Quality Criteria    10

5.Food Additives    13

6.Contaminants    13

7.Hygiene    13

8.Packing    13

9.Container Filling Tolerance    14

10.Labelling    14

11.Methods of Analysis and Sampling    17

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Trade Standard Applying to Olive Oils and Olive Pomace Oils

1.Scope

This standard applies to olive oils and olive pomace oils that are the object of international trade or of concessional or food aid transactions.

2.Designations and Definitions

2.1.Olive Oils

2.1.1.    Virgin olive oils

Virgin olive oils are oils which are obtained from the fruit of the olive tree (Olea europaea L.) solely by mechanical or other physical means under conditions, particularly thermal conditions, that do not lead to alterations in the oil, and which have not undergone any treatment other than washing, decantation, centrifugation and filtration. Virgin olive oils shall be classified and designated as follows:

2.1.1.1.Virgin olive oils fit for consumption as they are:

1.Extra virgin olive oil: virgin olive oil which has an free acidity, expressed as oleic acid, of not more than 0.80 grams per 100 grams and the other physico–chemical and organoleptic characteristics of which correspond to those fixed for this category in this standard.

2.Virgin olive oil: virgin olive oil which has an free acidity, expressed as oleic acid, of not more than 2.0 grams per 100 grams and the other physico–chemical and organoleptic characteristics of which correspond to those fixed for this category in this standard.

3.Ordinary virgin olive oil: virgin olive oil which has an free acidity, expressed as oleic acid, of not more than 3.3 grams per 100 grams and the other physico–chemical and organoleptic characteristics of which correspond to those fixed for this category in this standard. 1

2.1.1.2.Virgin olive oils that must undergo processing prior to consumption:

Lampante virgin olive oil: virgin olive oil which has an free acidity expressed as oleic acid, of more than 3.3 grams per 100 grams and/or the physico–chemical and organoleptic characteristics of which correspond to those fixed for this category in this standard. It is intended for refining or for technical use.

2. 1. 2.    Refined olive oil

Refined olive oil: olive oil obtained from virgin olive oils by refining methods which do not lead to alterations in the initial glyceridic structure. It has an free acidity, expressed as oleic acid, of not more than 0.30 grams per 100 grams and its other physico–chemical and organoleptic characteristics correspond to those fixed for this category in this standard. 2

2. 1. 3.    Olive oil composed of refined olive oil and virgin olive oils

Olive oil composed of refined olive oil and virgin olive oils: oil consisting of a blend of refined olive oil and virgin olive oils fit for consumption as they are. It has an free acidity, expressed as oleic acid, of not more than 1.00 gram per 100 grams and its other physico–chemical and organoleptic characteristics correspond to those fixed for this category in this standard.

2.2.Olive Pomace Oil

Olive pomace oil 3  is the oil obtained by treating olive pomace with solvents or other physical treatments, to the exclusion of oils obtained by re-esterification processes and of any mixture with oils of other kinds. It is marketed in accordance with the following designations and definitions:

2. 1. Crude olive pomace oil

Crude olive pomace oil: olive pomace oil, the physico–chemical and organoleptic characteristics of which correspond to those fixed for this category in this standard. It is intended for refining for use for human consumption, or it is intended for technical use.

2.2.2. Refined olive pomace oil

Refined olive pomace oil: oil obtained from crude olive pomace oil by refining methods which do not lead to alterations in the initial glyceridic structure. It has an free acidity expressed as oleic acid, of not more than 0.30 grams per 100 grams and its other physico–chemical and organoleptic characteristics correspond to those fixed for this category in this standard. 4

2.2.3. Olive pomace oil composed of refined oil and virgin olive oils

Olive pomace oil composed of refined olive pomace oil and virgin olive oils: oil consisting of a blend of refined olive pomace oil and virgin olive oils fit for consumption as they are. It has an free acidity of not more than 1.00 gram per 100 grams and its other physico–chemical and organoleptic characteristics correspond to those fixed for this category in this standard. 5  In no case shall this blend be called "olive oil".

3.Purity Criteria

The identity characteristics comprising the purity criteria shall be applicable to olive oils and olive pomace oils.

The limits established for each criterion include the precision values of the attendant recommended method.

3.1.    Fatty acid composition as determined by gas chromatography (% m/m methyl esters):

3.2.    Trans fatty acid content (% trans fatty acids)

3.3.    Sterol and tripertene dialcohol composition

3.3. 1.    Desmethylsterol composition (% total sterols)

3.3.2.    Total sterol content (mg/kg)

·Virgin olive oils

·Refined olive oil    > 1000*

·Olive oil (ROO+VOOs)

·Crude olive pomace oil    > 2500

·Refined olive pomace oil    > 1800

·Olive pomace oil (ROPO+VOOs)    > 1600

3.3.3.    Erythrodiol and uvaol content (% total sterols)

3.4.    Wax content (mg/kg)

3.5.    Maximum difference between the actual and theoretical ECN 42 triacylglycerol content (%)

3.6.    Stigmastadiene content (mg/kg)

·Extra virgin olive oil and virgin olive oil        < 0.05

·Ordinary virgin olive oil            < 0.10

·Lampante virgin olive oil            < 0.50

3.7.    Content of 2-glyceryl monopalmitate (%)

·Edible virgin olive oils and olive oil (ROO+VOOs):

C16:0 < 14.00%; 2P < 0.9%

C16:0 > 14.00%, 2P < 1.0%

·Non-edible virgin olive oils and refined olive oils:

C16:0 < 14.00%; 2P < 0.9%

C16:0 > 14.00%, 2P < 1.1%

·Olive pomace oil (ROPO+VOOs)    < 1.2%

·Crude and refined olive pomace oils    < 1.4%

3.8.    Unsaponifiable matter (g/kg)

·Olive oils    < 15

·Olive pomace oils    < 3

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4. QUALITY CRITERIA

The limits established for each criterion and designation include the precision values of the attendant recommended method

*    It is not obligatory for the criteria in 4.1, 4.2 and 4.3 to be concurrent; one is sufficient.

**    Or when the median of the defect is less than or equal to 3.5 and the median of the fruity attribute is equal to 0.0.

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*    This determination is solely for application by commercial partners on an optional basis.

**    Commercial partners in the country of retail sale may require compliance with these limits when the oil is made available to the end consumer.

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5.FOOD ADDITIVES

5.1.Virgin olive oils and crude olive pomace oil

None permitted.

5.2.Refined olive oil, olive oil (ROO+VOOs), refined olive pomace oil and olive pomace oil (ROPO+VOOs)

Alpha-tocopherol permitted to restore natural tocopherol lost in the refining process.

Maximum level: According to the Good Manufacturing Practices (GMP).

6.CONTAMINANTS

6.1.Heavy metals

The products covered by this standard shall comply with the maximum levels of the General Standard for Contaminants and Toxins in Food and Feed (CODEX STAN 193-1995).

6.2.Pesticide residues

The products covered by this standard shall comply with those maximum residue limits established by the Codex Alimentarius Commission for these commodities.

7.Hygiene

7.1.It is recommended that the products intended for human consumption covered by the provisions of this standard be prepared and handled in accordance with the appropriate sections of the General Principles of Food Hygiene (CAC/RP 1- 1969), and other relevant Codex texts such as Codes of Hygienic Practice and Codes of Practice.

7.2.The products intended for human consumption should comply with any microbiological criteria established in accordance with the Principles for the Establishment and Application of Microbiological Criteria (CAC/GL 21-1997).

8.PACKING

Olive oils and olive pomace oils intended for international trade shall be packed in containers complying with the General Principles of Food Hygiene recommended by the Codex Alimentarius Commission (CAC/RCP 1 - 1969), and other relevant texts such as Codes of Hygienic Practice and Codes of Practice.

The containers used may be:

8.1.Tanks, containers, vats, which permit the transportation in bulk of olive oils and olive pomace oils;

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8.2.Metal drums, in good condition, hermetically-sealed, which should be internally covered with a suitable varnish;

8.3.Metal tins and cans, lithographed, new, hermetically-sealed, which should be internally covered with a suitable varnish;

8.4.Demi-johns, glass bottles or bottles made of suitable macromolecular material.

9.Container Filling Tolerance

The volume occupied by the contents shall under no circumstances be less than 90% of the capacity of the container, except in the case of tin containers with a capacity of, or less than, 1 L in which the volume occupied shall under no circumstances be less than 80% of the capacity of the container; this capacity is equal to the volume of distilled water at 20oC which the container can hold when full.

10.Labelling

In addition to the appropriate sections of the Codex General Standard for the Labelling of Pre-packaged Foods (CODEX STAN 1-1985) and the guidelines applying to food not intended for direct sale to consumers, the specific provisions providing the following information shall be applied:

10.1.On containers intended for direct sale to consumers

10.1.1.Name of the product

The labelling on each container shall indicate the specific designation of the product contained, complying in every way with the relevant provisions of this standard.

10.1.1.1.Designations of olive oils

·Extra virgin olive oil

·Virgin olive oil

·Ordinary virgin olive oil 14

·Refined olive oil12

·Olive oil (ROO+VOOs) 15

10.1.1.2.Designations of olive pomace oils

·Refined olive pomace oil1

·Olive pomace oil (ROPO + VOOs)2

10.1.2.Net contents

The net contents shall be declared by volume in the metric system ("Système International" units).

10.1.3.Name and address

The name and address of the manufacturer, packer, distributor, importer, exporter or seller shall be declared.

10.1.4.Country of origin

The name of the country of origin shall be declared. When the product undergoes substantial processing in a second country, thecountry in whichsuchprocessingiscarriedoutshall be considered as the countryoforiginfor labelling purposes.

10.1.5.Geographical indications and designations of origin

10.1.5.1.Geographical indications

The labels of virgin olive oils may state their geographical indication (country, region or locality) when they have been empowered to do so by their country of origin and when such virgin olive oils have been produced, packed and originate exclusively in the country, region or locality mentioned.

10.1.5.2.Designations of origin

The labels of extra virgin olive oils may indicate their designation of origin (country, region or locality) when they have been awarded such a designation, in accordance with the terms provided under the regulations of their country of origin and when such extra virgin olive oil has been produced, packed and originates exclusively in the country, region or locality mentioned.

10.1.6.Lot identification

Each container shall be embossed or otherwise permanently marked in code or in clear to identify the producing factory and the lot.

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10.1.7.Date marking and storage conditions

10.1.7.1.Date of minimum durability

In the case of pre-packaged products intended for the end consumer, the date of minimum durability (preceded by the words "best before end") shall be declared by the month and year in uncoded numerical sequence. The month may be indicated by letters in those countries where such use will not confuse the consumer; if the shelf life of the product is valid to December, the expression "end (stated year)" may be used as an alternative.

10.1.7.2.Storage instructions

Any special conditions for storage shall be declared on the label if the validity of the date of minimum durability depends thereon.

10.2.On forwarding packs of oils intended for human consumption

In addition to the details noted under section 10.1., the following inscription shall appear:

·Number and type of containers held in pack.

10.3.On containers allowing the transportation in bulk of olive oils and olive pomace oils

The labelling on each container shall include:

10.3.1.1.Name of the product

The name shall indicate the specific designation of the product contained, complying in every way with the provisions of this standard.

10.3.1.2.Net contents

The net contents shall be declared by weight or volume in the metric system ("Système International" units).

10.3.1.3.Name and address

The name and address of the manufacturer, distributor or exporter shall be declared.

10.3.1.4.Country of origin

The name of the exporting country shall be declared.

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11.METHODS OF ANALYSIS AND SAMPLING

The methods of analysis and sampling given below are international referee methods. The latest version of these methods should be used.

The methods of analysis and sampling given below are international referee methods. The latest version of these methods should be used.

11.1Sampling

According to ISO 5555, "Animal and vegetable fats and oils - Sampling".

11.2Preparation of the test sample

According to ISO 661, "Animal and vegetable fats and oils - Preparation of the test sample".

11.3Determination of the fatty acid composition and trans fatty acid content

According to COI/T.20/Doc. No. 33/Rev.12, “Determination of fatty acid methyl esters composition in olive oils and olive pomace oils by gas-chromatography”

11.4Determination of the sterol composition and content and alcoholic compounds

According to COI/T.20/Doc. No. 26/Rev. 5, “Determination of the composition and content of sterols, triterpenic dialcohols and aliphatic alcohols by capillary column gas chromatography”.

11.5Determination of the difference between the actual and theoretical ECN 42 triacylglycerol content

According to COI/T.20/Doc. No. 20/Rev. 4, "Determination of the difference between actual and theoretical content of triacylglycerols with ECN 42", or AOCS 5b- 89.

11.6Determination of the stigmastadiene content

According to COI/T.20/Doc. No. 11/Rev.4, "Determination of stigmastadienes in vegetable oils", or COI/T.20/Doc. no. 16/Rev.2, "Determination of sterenes in refined vegetable oils", or ISO 15788-1 or AOCS Cd 26-96.

11.7Determination of the content of 2-glyceryl monopalmitate

According to COI/T.20/Doc. No. 23/Rev.1, "Determination of the percentage of 2-glyceryl monopalmitate" or to ISO 12872.

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11.8Determination of the unsaponifiable matter

According to ISO 3596, “Determination of the unsaponifiable matter – Method using diethyl ether extraction”, or AOCS Ca 6b-53 or ISO 18609

The results should be expressed in g/unsaponifiable matter per kg/oil.

11.9Determination of the organoleptic characteristics

According to COI/T.20/Doc. No. 15/Rev.11, "Organoleptic assessment of virgin olive oil".

11.10Determination of the free acidity

According to COI/T.20/Doc. No. 34/Rev.12, “Method for the determination of acidity in olive oils and olive pomace oils Determination of free fatty acids, cold method”.

11.11Determination of the peroxide value

According to COI/T.20/Doc. No. 38 and COI/T.20/Doc. No. 35/Rev.1, “Determination of the peroxide value”, ISO 3960, or AOCS Cd 8b-90.

11.12Determination of the absorbency in ultra-violet

According to COI/T.20/Doc. No. 19/Rev.5, "Spectrophotometric investigation in the ultraviolet", or ISO 3656 or AOCS Ch 5- 91.

11.13Determination of the moisture and volatile matter

According to ISO 662, "Determination of the moisture and volatile matter".

11.14Determination of the insoluble impurities in light petroleum

According to ISO 663, "Determination of the insoluble impurities".

11.15Determination of the flash point residual hexane content

According to ISO 9832:2002, “Technical residual hexane content in animal and vegetable oils” the FOSFA International method.

11.16Detection of trace metals

According to ISO 8294, "Determination of copper, iron and nickel by direct graphite furnace atomic absorption spectrometry".

11.17Determination of the alpha-tocopherol

According to ISO 9936, “Determination of tocopherols and tocotrienols contents – Method using high-performance liquid chromatography”.

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11.18Determination of traces of heavy metals

·Determination of lead: according to ISO 12193 or AOCS Ca 18c-91 or AOAC 994.02.

·Determination of arsenic: according to AOAC 952.13 or AOAC 942.17 or AOAC 985.16.

11.19Determination of the content of waxes and alkyl esters

According to COI/T.20/Doc. No. 28/Rev.4, “Determination of the content of waxes, fatty acid methyl esters and fatty acid ethyl esters by capillary gas chromatography“.

11.20Determination of phenolic compounds

According to COI/T.20/Doc. No. 29/Rev.2, “Document to declare the use of IOC methods for phenolic compounds determination”

11.21Determination of the coherence of TAG composition with the fatty acid composition: Screening method (not legal in nature and cannot downgrade an oil)

According to COI/T.20/Doc. No. 25/Rev.2, “Method for the evaluation of the coherence of TAG composition with the fatty acid composition”.

11.22Determination of the methanol and ethanol content in virgin olive oils.

According to COI/T.20/Doc. No. 36, “Method of determination of ethanol and methanol content on virgin olive oils”.

11.23Determination of the triacylglycerols and di-acylglycerols

According to COI/T.20/Doc. No. 32/Rev.1, “Method of determination of composition of triacylglycerols and composition and content of di-acylglycerols by capillary gas chromatography, in vegetable oils”.

11.24. Determination of volatile compounds

According to COI/T.20/Doc. No. 37, “Method of determination of volatile compounds in virgin olive oils by SPME-GC-FID/MS”.

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DRAFT DECISION DEC-III.X/123-VI/2026

Adopting the method of analysis for the determination of acidity in olive oils and olive pomace oils

DECISION NO DEC-III.X/123-VI/2026

Adopting the method of analysis for the determination of
acidity in olive oils and olive pomace oils

The Council of Members of the International Olive Council

Having regard to the International Agreement on Olive Oil and Table Olives, 2015, and in particular its Article 1 "Objectives of the Agreement" relating to standardisation and research aimed at harmonising national and international legislation, as well as physicochemical and organoleptic analysis in order to improve knowledge of the composition and quality characteristics of olive products;

Having regard to the recommendation made by the Committee on Chemistry and Standardisation at its 18th meeting, within the framework of the 123rd session of the Council of Members;

Considering the unanimous position agreed by the chemist experts at their meeting of 24 and 25 March 2026, with a view to the duly justified revision of the said method;

Decides

To revise document COI/T.20/Doc. No. 34/Rev. 1 “Determination of free fatty acids, cold method”. Document COI/T.20/Doc. No. 34/Rev. 2, “Method for the determination of acidity in olive oils and olive pomace oils”, replaces and repeals method COI/T.20/Doc.No. 34/Rev. 1.

Lisbon, 30 June 2026

Tawfik EL ACHCHABI

Chair of the International Olive Council

COI/T.20/Doc. No 34/Rev. 2
June 2026
English / Original: English
Distr.: Restricted

METHOD OF ANALYSIS

Determination of FREE FATTY ACIDS acidity, COLD METHOD

in olive oils and olive pomace oils TITRIMETRIC OR POTENTIOMETRIC DETERMINATION

1.Scope and Field of Application

This document describes a method for the determination of free fatty acids in olive oils and olive pomace oils, using either titrimetric endpoint detection with a suitable indicator or potentiometric endpoint detection. The free fatty acid content is expressed as acidity, calculated as a percentage of oleic acid.

2.Principle

A sample is dissolved in a mixture of solvents and the free fatty acids present are titrated using a potassium hydroxide or sodium hydroxide solution.

3.Reagents

All the reagents should be of recognizsed analytical quality and the water used either distilled or of equivalent purity.

3.1.    Diethyl ether; and 95 % ethanol (v/v) :, mixture of equal parts by volume. Neutralizse precisely at the moment of use with the potassium hydroxide solution (3.2), with the addition of 0.3 mlL of the phenolphthalein indicator solution (3.3) per 100 mlL of mixture.

Ethanol may be replaced by propanol-2 (99 %) and diethyl ether may be replaced by ter-butylmethylether or petroleum ether 161.

Note 1: Diethyl ether is highly inflammable and may form explosive peroxides. Special care should be taken in its use.

Note 2: If it is not possible to use diethyl ether, a mixture of solvents containing ethanol and toluene may be used. If necessary, ethanol may be replaced by propanol-2.

3.2.    Potassium hydroxide or sodium hydroxide, titrated ethanolic or aqueous solution, c(KOH) about 0.1 mol/lL or, if necessary, c(KOH) about 0.5 mol/lL. Commercial solutions are available. The exact concentration of the 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 an aqueous solution of potassium hydroxide (or sodium hydroxide), replace the aqueous solution by an ethanolic solution 172.

3.3.    Phenolphthalein, 10 g/lL solution in 95 to 96 % ethanol (v/v), alkali blue 6B or thymolphthalein, 20 g/Ll solution in 95 to 96 % ethanol (v/v). In the case of strongly coloured oils, alkali blue or thymolphthalein shall be used.

4.Apparatus

Usual laboratory equipment, including:

4.1Analytical balance, capable of being read reading to the nearest 0.,001 g;

4.2250 mlL conical flask;

4.310 ml b Class A Bburette class A (10 mLl or 5 mLl), graduated in 0,.05 ml mL or 0,02 mlL, or an equivalent automatic burette.

4.4Automatic titrator with processor, dosing device, stirrer and electrodes (4.5), or a potentiometer.

If other apparatus is used, the procedure shall be optimized for the relevant apparatus. The apparatus shall be able to perform a dynamic titration (fast at the beginning, slow near the endpoint). This is necessary to minimize the titration time whilst achieving a slow titration near the endpoint. If a different apparatus is used, the procedure shall be optimised accordingly. The apparatus must be capable of performing a dynamic titration—fast at the start and slower near the endpoint.

This is necessary to minimise titration time while ensuring accuracy near the endpoint.

4.5Combined pH electrode for non-aqueous acid/base titrations.

4.6Beaker of 250 mL, of capacity 250 ml, and of a tall form.

5.PROCEDURE

5.1Preparation of the test sample

When the sample is cloudy, it should shall be filtered.

5.2Test portion

Take a sample depending on the presumed acidity in accordance with the following table:

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5.1.    5.3. Titrimetric determination using an indicator

Weigh the sample in the conical flask (4.2).

Dissolve the sample (5.2) in 50 mL to 100 mlL of the previously neutralizsed mixture of diethyl ether and ethanol (3.1).

Titrate while stirring with the 0.1 mol/Ll solution of potassium hydroxide (3.2) 183 (see Note 4) until the indicator changes (the colour of the coloured indicator persists for at least 10 seconds). 194

Note 4: If the quantity of 0.1 mol/l potassium hydroxide solution required exceeds 10 ml, use the 0.5 mol/l solution or change the sample mass according to the expected free acidity and the proposed table.

Note 5: If the solution becomes cloudy during titration, add enough of the solvents (3.1) to give a clear solution.

Carry out a second determination only if the first result is higher than the specified limit for the oil category of the oil.

5.2.    Potentiometric determination

Weigh the sample into a 250 mL beaker (4.6).

Add 50 mL to 100 mL of the neutralised solvent mixture (3.1) and dissolve the sample, if necessary, with gentle warming.

Introduce the combined electrode (4.5) into the solvent mixture and connect it to the automatic titration apparatus (4.4).

6.Expression of Results

Acidity, as percentage of oleic acid by weight is equal to:

where:

- V: = the volume of titrated potassium hydroxide solution used, in milliliters;

- c =: the exact concentration in moles per litre of the titrated solution of potassium hydroxide used;

- M = : 282 g/mol, the molar mass in grams per mole of oleic acid;

- m =: the mass of the sample, in grams.

Oleic acidity is reported as follows:

- (a) to two decimal places for values from 0 up to and including 1;

- (b) to one decimal place for values from 1 up to and including 100

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Precision Values of the Method

Analysis of the collaborative test results

More than 20 twenty laboratories took part in the collaborative test study arranged conducted by the International Olive Council (IOC) in 2014 and 2015.

The test was organized by the Deutsches Institut für Normung (DIN) in 2004/2005. The results obtained were subjected to statistical analysis in accordance with ISO 5725 1 and ISO 5725 2 to give the precision data shown in the tables 1 and 2.

The test was performed study was carried out on five 5 samples in 2014 and 3 three samples in 2015 using titrimetric determination:

- PA 1-2014: crude olive pomace oil

- PA 2-2014: refined olive pomace oil

- PA 3-2014: refined olive oil

- PA 4-2014: extra virgin olive oil (Mario Solinas prizeQualtiy Award) – 2011 crop year

- PA 5-2014: extra virgin olive oil (Mario Solinas prizeQuality Award) – 2014 crop year

- PA 6-2015: 70 % lampante olive oil + 30 % grape seed oil

- PA 7-2015: late harvest extra virgin olive oil

- PA 8-2015: 90 % lampante olive oil + 10 % palm olein

The results of the collaborative tests have been were statistically processed according in accordance to the rules laid down in with the international standards ISO 5725-2. Outliers were examined by applying Cochran’s and Grubbs’ tests to the laboratory results for each determination (replicates a and b) and each sample.

The table lists:

-n: number of participating laboratories

-outliers: number of laboratories with outlying values

-mean: mean of the accepted results (g/100g)

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-Sr: repeatability standard deviation (g/100g)

-RDSDr (%) relative standard deviation for repeatability (Sr x 100/mean)

-r: value below which the absolute difference between two single independent test results obtained with the same method on identical test material in the same laboratory by the same operator using the same equipment within short intervals of time intervals may be expected to lie with a probability of 95% (Sr multiplied by x 2.8) (g/100g)

-SR: reproducibility standard deviation (g/100g)

-RDSDR (%): relative standard deviation for reproducibility (SR x 100/mean)

-R: value below which the absolute difference between two single test results obtained with the same method on identical test material in different laboratories, with by different operators using different equipment may be expected to lie with a probability of 95% (SR multiplied by x 2.8) (g/100g)

As part of the determination of the precision values of the ISO 660 standard, an international collaborative test study was organizsed by the ISO (the International Organizsation for Standardizsation) (ISO), involving 41 laboratories from different international countries using the methods described in clauses 5.1 and 5.2. The results obtained on for olive oils were subjected to statistical analysies in accordance with ISO 5725:1986 and ISO 5725 (all parts), in order to give establish the precision data shown in the followed table below:

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References

-ISO 5725-1:1994 Accuracy (trueness and precision) of measurement methods and results – Part 1: General principles and definitions

-ISO 5725-2:1994 Accuracy (trueness and precision) of measurement methods and results – Part 2: Basic method for the determination of the repeatability and reproducibility of a standard measurement method

-ISO 5725-5:1998 Accuracy (trueness and precision) of measurement methods and results – Part 5: Alternative methods for the determination of the precision of a standard measurement method

-ISO 5725-6:1994 Accuracy (trueness and precision) of measurement methods and results – Part 6: Use in practice of accuracy values

-ISO 660:2020 Animal and vegetable fats and oils — Determination of acid value and acidity

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DRAFT DECISION DEC-III-X/12-V3I/2026

Concerning the method of analysis for the determination of the fatty acid composition in olive oils and olive pomace oils by gas chromatography

Decision DEC-III-X/123-VI/2026

Concerning the method of analysis for the determination of the fatty acid composition in olive oils and olive pomace oils by gas chromatography

The Council of Members of the International Olive Council

Having regard to the International Agreement on Olive Oil and Table Olives, 2015, and in particular its Article 1 “Objectives of the Agreement”, relating to standardisation and research aimed at harmonising national and international legislation, as well as physico-chemical and organoleptic analysis in order to improve knowledge of the composition and quality characteristics of olive products;

Having regard to the recommendation made by the Committee on Chemistry and Standardisation at its 18th meeting, within the framework of the 123rd session of the Council of Members;

Considering the unanimous position agreed by the chemist experts at their meeting of 24 and 25 March 2026, with a view to the duly justified revision of the said method;

Decides

To revise document COI/T.20/Doc. No. 33/Rev. 1 “Determination of the fatty acid composition in olive oils and olive pomace oils by gas chromatography”.

Document COI/T.20/Doc. No. 33/Rev. 2 replaces and repeals its previous version.

Lisbon, 30 June 2026 Tawfik EL ACHCHABI

Chair of the International Olive Council

Príncipe de Vergara, 154 - 28002 Madrid - Spain Tel: +34 915 903 638

E-Mail:  iooc@internationaloliveoil.org

Internationaloliveoil.org

COI/T.20/Doc. No. 334/Rev. 322

June 2026
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Príncipe de Vergara, 154 – 28002 Madrid – Spain Tlf.: +34 915 903 638 Fax: +34 915 631 263 - e-mail:  iooc@internationaloliveoil.org -   http://www.internationaloliveoil.org/

Method of analysis

Determination of the fatty acid composition in olive and olive pomace oils by gas chromatography

1. Scope

This standard document gives guidance on the gas chromatographic determination of free and bound fatty acids in vegetable fats and oils following their conversion into fatty acid methyl esters (FAME).

The bound fatty acids of the triacylglycerols (TAGs) and, depending on the esterification method, the free fatty acids (FFA), are converted into fatty acid methyl esters (FAME), which are determined by capillary gas chromatography.

This method permits determination of FAME from C12 to C24, including saturated, cis- and trans-monounsaturated and cis- and trans-polyunsaturated fatty acid methyl esters. It also allows the quantification of fatty acid ethyl esters (FAEE) present in an oil.

2. Principle

Gas chromatography (GC) is used for the quantitative analysis of FAME. The FAME are prepared according to Part 1 of this method. They are then injected into and vaporised within the injector. The separation of FAME is performed on analytical columns of specific polarity and length. A Flame Ionisation Detector (FID) is used for the detection of the FAME. The conditions of analysis are given in Part 2 of this method.

Hydrogen or helium may be used as the carrier gas (mobile phase) in the gas chromatography of FAME with FID. Hydrogen speeds up separation and gives sharper peaks. The stationary phase is a microscopic layer of a thin liquid film on an inert solid surface made of fused silica. As they pass through the capillary column the volatilised compounds being analysed interact with the stationary phase coating the inner surface of the column. Due to this different interaction of different compounds, they elute at a different time, which is called the retention time of the compound for a given set of analysis parameters. The comparison of the retention times is used for the identification of the different compounds.

Part 1. Preparation of the fatty acid methyl esters from olive oil and olive-pomace oil.

1.Scope

This method specifies the preparation of the methyl esters of fatty acids. It includes methods for preparing fatty acid methyl esters from olive and olive-pomace oils.

2.Field of application

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3.Methodology

3.1.    Trans-esterification with methanolic solution of potassium hydroxide at room temperature.

3.1.1.    Principle

Methyl esters are formed by trans-esterification with methanolic potassium hydroxide as an intermediate stage before saponification takes place.

3.1.2.    Reagents

3.1.2.1. Methanol containing not more than 0.5 % (m/m) water.

3.1.2.2. Hexane, chromatographic quality. (Hexane may be replaced by iso-octane (2,2,4-trimethyl pentane in chromatography grade, according with ISO NF EN ISO 12966-2 Method: Animal and vegetable fats and oils - Gas chromatography of fatty acid methyl esters - Part 2: Preparation of methyl esters of fatty acids. However, this is preferred due to the toxicity of hexane.)

3.1.2.3. Heptane, chromatographic quality. Heptane may be replaced by iso-octane (2,2,4-trimethyl pentane in chromatography grade.

3.1.2.4. Diethyl ether, stabilised for analysis.

3.1.2.5. Acetone, chromatographic quality.

3.1.2.6. Elution solvent for purifying the oil by column/SPE chromatography, mixture hexane/diethyl ether 87/13 (v/v).

3.1.2.7. Potassium hydroxide, approximately 2M methanolic solution: dissolve 11.2 g of potassium hydroxide in 100 mL of methanol.

3.1.2.8. Silica gel cartridges, 1 g (6 mL), for solid phase extraction.

3.1.3.    Apparatus

3.1.3.1.Screw-top test tubes (5 mL volume) with cap fitted with a PTFE joint.

3.1.3.2.Graduated or automatic pipettes, 2 mL and 0.2 mL.

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3.1.4.Purification of oil samples

When necessary, the samples will be purified by passing the oil through a silica gel solid- phase extraction cartridge. A silica gel cartridge (3.1.2.8) is placed in a vacuum elution apparatus and washed with 6 mL of hexane (3.1.2.2); washing is performed without vacuum. Then a solution of the oil (0.12 g approximately) in 0.5 mL of hexane (3.1.2.2) is loaded onto the column. The solution is pulled down and then eluted with 10 mL of hexane/diethyl ether (87:13 V/V) (3.1.2.6). The combined eluates are homogenised and divided in two similar volumes. An aliquot is evaporated to dryness in a rotary evaporator under reduced pressure at room temperature. The residue is dissolved in 1 mL of heptane for fatty acid methyl ester preparation and analysis by GC (3.1.6). The second aliquot is evaporated and the residue is dissolved in 1 mL of acetone for triglyceride analysis by HPLC, if necessary.

3.1.5.Procedure

In a 5 mL screw-top test tube (3.1.3.1) weigh approximately 0.1 g of the oil sample. Add 2 mL of heptane (3.1.2.2), and shake. Add 0.2 mL of the methanolic potassium hydroxide solution (3.1.2.7), put on the cap fitted with a PTFE joint, tighten the cap, and shake vigorously for 30 seconds. Leave to stratify until the upper solution becomes clear. Decant the upper layer containing the methyl esters. The heptane solution is ready for injection into the gas chromatograph. It is advisable to keep the solution in the refrigerator until gas chromatographic analysis. Storage of the solution for more than 12 hours is not recommended.

Part 2. Analysis of fatty acid methyl esters by gas chromatography

1.Scope

This method gives general guidance for the application of capillary column gas chromatography to determine the qualitative and quantitative composition of a mixture of fatty acid methyl esters obtained in accordance with the method specified in Part 1 of this method.

The method is not applicable to polymerised fatty acids.

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2.Reagents

2.1.Carrier gas

Inert gas (helium or hydrogen), thoroughly dried and with an oxygen content of less than 10 mg/kg. 201

Note 3: Hydrogen can double the speed of analysis but is hazardous. Safety devices are available.

2.2.Auxiliary gases

2.2.1.Hydrogen (purity ≥ 99.9 %), free from organic impurities.

2.2.2.Air or oxygen, free from organic impurities.

2.2.3.Nitrogen (purity > 99%).

2.3.Reference standard

Mixture of methyl esters of pure fatty acids, or the methyl esters of a fat of known composition, preferably similar to that of the fatty matter to be analysed. Cis and trans isomers of octadecenoic, octadecadienoic and octadecatrienoic methyl esters are useful for the identification of trans isomers of unsaturated acids.

Care should be taken to prevent the oxidation of polyunsaturated fatty acids.

3.Apparatus

The instructions given are for the usual equipment used for gas chromatography, employing capillary columns and a flame-ionisation detector.

3.1.Gas chromatograph

The gas chromatograph shall comprise the following elements.

3.1.1.Injection system

Use an injection system with capillary columns, in which case the injection system should be specially designed for use with such columns. It may be of the split type or the splitless on- column injector type.

3.1.2.Oven

The oven shall be capable of heating the capillary column to a temperature of at least 260 °C and of maintaining the desired temperature to within 0.1°C. The last requirement is particularly important when a fused silica tube is used.

The use of temperature-programmed heating is recommended in all cases, and in particular for fatty acids with less than 16 carbon atoms.

3.1.3.Capillary column

3.1.3.1.Tube, made of a material inert to the substances to be analysed (usually glass or fused silica). The internal diameter shall be between 0.20 to 0.32 mm. The internal surface shall undergo an appropriate treatment (e.g. surface preparation, inactivation) before receiving the stationary phase coating.

A length of 60 m is sufficient for fatty acid and cis and trans isomers of fatty acids.

3.1.3.2.Stationary phase, polar polysiloxane (cyanopropylsilicone) bonded (cross-linked) columns are suitable. 212

Note 4: There is a risk that polar polysiloxanes may give rise to difficulties in the identification and separation of linolenic acid and C20 acids.

The coatings shall be thin, i.e, 0.1 to 0.2 μm.

3.1.3.3.Assembly and conditioning of the column

Observe the normal precautions for assembling capillary columns, i.e. arrangement of the column in the oven (support), choice and assembly of joints (leak tightness), positioning of the ends of the column in the injector and the detector (reduction of dead-spaces). Place the column under a flow of carrier gas (e.g. 0.3 bar (30 kPa) for a column of length 25 m and internal diameter 0.3 mm).

Condition the column by temperature programming of the oven at 3 °C/min from ambient temperature to a temperature 10 °C below the decomposition limit of the stationary phase. Maintain the oven at this temperature for one hour until stabilisation of the baseline. Return it to 180 °C to work under isothermal conditions. 223

Note 5: Suitably pre-conditioned columns are available commercially

3.1.4.Flame ionisation detector and converter-amplifier

3.2.Syringe

The syringe shall have a maximum capacity of 10 μl, graduated in 0.1 μl divisions.

3.3.Data acquisition system

Data acquisition system connected online with the detectors and employed with a software program suitable for peak integration and normalisation.

4.Procedure

The operations described in 4.1 to 4.3 are for the use of a flame-ionisation detector.

4.1.Test conditions

4.1.1.Selection of optimum operating conditions for capillary columns

Owing to the efficiency and permeability of capillary columns, the separation of the constituents and the duration of the analysis are largely dependent on the flow-rate of the carrier gas in the column. It will therefore be necessary to optimise the operating conditions by adjusting this parameter (or simply column head loss) depending on whether the aim is to improve separation or speed up analysis.

The following conditions have proved to be suitable for the separation of FAMEs (C4 to C26). Examples of chromatograms are shown in Annex B:

Injector temperature:    250 °C

Detector temperature:    250 °C

Oven temperature:    165 °C (8 min) to 210 °C at 2 °C/min    
Carrier gas hydrogen:    column head pressure, 179 kPa    
Total flow:    154.0 mL/min;

Split ratio:    1:100

Injection volume:    1 μl

4.1.2.Determination of the resolution (see Appendix Annex A)

Calculate the resolution, R, of two neighbouring peaks I and II, using the formula:

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where:

dr(I) is the retention distance of peak I;

dr(II) is the retention distance of peak II;

tr(I) is the retention time of peak I ;

tr(II) is the retention time of peak II ;

ω(I) is the width of the base of peak I;

ω(II) is the width of the base of peak II;

ω0.5 is the peak width of the specified compound, at mid-height of the peak;

If ω(I) ≈ ω(II), calculate R using the following formulas:

where:

σ is the standard deviation (see Appendix Annex A, Figure 1).

If the distance dr between the two peaks dr(II) - dr(I) is equal to 4σ, the resolution factor R = 1.

If two peaks are not separated completely, the tangents to the inflection points of the two peaks

intersect at point C. In order to completely separate the two peaks, the distance between the two peaks must be equal to:

dr(II) - dr(I) = 6 σ from where R = 1.5 (see Appendix Annex A, Figure 3).

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5.    Expression of Results

5.1.    Qualitative analysis

Identify the methyl ester peaks of the sample from the chromatograms in Annex I B, if necessary by interpolation, or as described in 6.4.1.

5.2.    Quantitative analysis

5.2.1.    Determination of the composition

Calculate the mass fraction (wi) of the individual fatty acid methyl esters, and, where present, the ethyl esters, expressed as a percentage by mass of the total methyl and ethyl esters, as follows:

5.2.2. Method of calculation

5.2.2.1. General case

Calculate the content of a given component i, expressed as a percentage by mass of methyl esters, or of methyl and ethyl esters, by determining from the percentage represented by the area of the corresponding peak relative to the sum of the areas of all the peaks, using the following formula:

where:

Ai is the area under the peak of the individual fatty acid methyl ester i;

ΣA is the sum of the areas under all the peaks of all the individual fatty acid methyl esters or

of methyl and ethyl esters. The results are expressed to two decimal places. 234

Note 6: For fats and oils, the mass fraction of the fatty acid methyl esters is equal to the mass fraction of the triacylglycerols in grams per 100 g. For cases in which this assumption is not allowed, see 5.2.2.2.

6.    Peaks (of methyl and ethyl esters) taking into account for the calculation of each fatty acid

Figure 1 of ANEX B gives the typical gas chromatographic profile of an olive-pomace oil containing methyl and ethyl esters of fatty acids, and trans-isomers of methyl esters.

6.1.    For the calculation of the fatty acid composition and Δ ECN42, all the following fatty acids will be taken into account:

Myristic (C14:0)

Palmitic (C16:0). Sum of the areas of the peaks corresponding to the methyl and ethyl esters.

Palmitoleic (C16:1). Sum of the areas of the peaks corresponding to the Δ 9 and Δ 7 isomers of the methyl ester.

Margaric (C17:0).

Margaroleic (C17:1).

Stearic (C18:0).

Oleic (C18:1). Sum of the areas of the peaks corresponding to the Δ 9 and Δ 7 isomers of the

methyl ester, ethyl ester, and trans-isomers of the methyl ester.

Linoleic (C18:2). Sum of the areas of the peaks corresponding to the methyl and ethyl esters, and the trans-isomers of the methyl ester.

Arachidic (C20:0).

Linolenic (C18:3). Sum of the areas of the methyl ester and the trans-isomers of the methyl ester. Eicosenoic (C20:1).

Behenic (C22:0). Lignoceric (C24:0).

Squalene will not be taken into account for the calculation of the total area.

Trans-isomers:

For the calculation of the percentage of trans-C18:1 the peak corresponding to the methyl esters of this fatty acid will be used. For the sum [trans-C18:2 + trans-C18:3], all the peaks corresponding to the trans-isomers of these two fatty acids will be summed. For the calculation of the total area, all the peaks mentioned in 6.1. will be taken into account.Note7: Not all peaks of ethyl esters of fatty acids and trans-isomers of methyl esters may be present in the chromatograms of other oils.

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6.2.    For the calculation of the percentage of trans fatty acids, the following approach shall be applied 245:

The percentage of trans-C18:1 shall be calculated using from the peak corresponding to the methyl esters of this fatty acid, where present in the chromatogram.

The percentage of trans-C18:2 shall be obtained by summing all peaks present or appearing in the chromatogram corresponding to the trans isomers of octadecadienoic acid, including:

otrans-trans octadecadienoic isomers,

ocis-trans and trans-cis octadecadienoic isomers.

The percentage of trans-C18:3 shall be obtained by summing all peaks present or appearing in the chromatogram corresponding to the trans isomers of octadecatrienoic acid, including:

otrans-cis-trans,

ocis-cis-trans,

ocis-trans-cis,

otrans-cis-cis isomers.

The total trans fatty acids (%) shall be recorded as the sum of:

otrans-octadecenoic acid (C18:1),

otrans-octadecadienoic acid (C18:2),

otrans-octadecatrienoic acid (C18:3).

Determination of trans fatty acids

For the calculation of the percentage of trans fatty acids, the following approach shall be applied:

The percentage of trans-C18:1 shall be calculated using the peak corresponding to the methyl esters of this fatty acid, where present in the chromatogram.

The percentage of trans-C18:2 shall be obtained as the sum of all peaks present or appearing in the chromatogram corresponding to the trans isomers of octadecadienoic acid, including:

otrans-trans octadecadienoic isomers,

ocis-trans and trans-cis octadecadienoic isomers.

The percentage of trans-C18:3 shall be obtained by summing all peaks present or appearing in the chromatogram corresponding to the trans isomers of octadecatrienoic acid, including:

otrans-cis-trans,

ocis-cis-trans,

ocis-trans-cis,

otrans-cis-cis isomers.

The results are shall be expressed for as:

trans-octadecenoic acid (C18:1),

sum of :the sum of trans-octadecadienoic acid (C18:2) and trans-octadecatrienoic acid (C18:3).

For the calculation of the total area, all peaks listed in section 6.1 shall be taken into account. For the calculation of the total area, all peaks listed in section 6.1, including lauric acid (C12:0), shall be taken into account,. including lauric acid (C12:0).

8. 7.    Test Report

The test report shall specify the methods used for the preparation of the methyl esters and for the gas chromatographic analysis. It shall also mention all operating details not specified in this Standard Method, or regarded as optional, together with details of any incidents which may have influenced the results.

The test report shall include all the information necessary for complete identification of the sample.

9. 8.    PRECISION

9. 8.1 Results of interlaboratory test

Details of an interlaboratory test on the precision of the method are summarised in Annex C. The values derived from this interlaboratory test may not be applicable to concentration ranges and matrices other than those given.

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9. 8.2 Repeatability

The absolute difference between two independent single test results, obtained using the same method on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time, will in not no more than 5% of cases be greater than r given in tables 1 to 15.

9. 8.3 Reproductibility

The absolute difference between two single test results, obtained using the same method on identical test material in different laboratories with different operators using different equipment, will in not more than 5 % of cases be greater than R given in tables 1 to 15.

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Annex A

Figure 1: with ω0.5 width at half height of the triangle (ABC) and b width at half height of the triangle (NPM).

Figure 2                    Figure 3

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Annex B

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Figure 1: Gas chromatographic profile obtained by the cold methylation method from olive-pomace oil. The chromatographic peaks correspond to the methyl and ethyl esters except where otherwise indicated.

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Figure 2: Gas chromatographic profile obtained by the cold methylation method from for virgin olive oil. The cChromatographic peaks correspond to the methyl and ethyl esters, except where otherwise indicated.

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Figure 3: Specimen chromatogram obtained from by capillary column analysis of the trans fatty acids.

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ANNEX C

Precision values of the method

A: Extra virgin olive oil B: Virgin olive oil

C: Lampante olive oil D: Olive oil

E: Crude olive pomace oil

Table 1: Myristic acid C14:0 from Ring Test COI 2015

Table 2: Palmitic acid C16:0 from Ring Test COI 2015

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Table 3: Palmitoleic acid C16:1 from Ring Test COI 2015

Table 4: Heptadecanoic acid C17:0 - from 2000-2006 recognition data

Table 5: Heptadecenoic acid C17:1 - from 2000-2006 recognition data