COMMISSION STAFF WORKING DOCUMENT Accompanying the document Proposal for a COUNCIL DECISION on the position to be taken on behalf of the European Union within the Council of Members of the International Olive Council (IOC), as regards two methods of analyses and the IOC Trade Standard for olive oil and olive pomace oil
Date: 2024-05-08
Institutions: Directorate-General for Agriculture and Rural Development, European Commission
Subjects: commodity agreement, international organisation, multilateral agreement, olive, olive oil, quality control of agricultural products

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  EN 

   EUROPEAN COMMISSION  Brussels, 8.5.2024  SWD(2024) 122 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 within the Council of Members of the International Olive Council (IOC), as regards two methods of analyses and the IOC Trade Standard for olive oil and olive pomace oil {COM(2024) 194 final}  
 
 
DRAFT DECISION No DEC-III.X/118-VI/2023 

REVISING THE METHOD FOR THE ORGANOLEPTIC ASSESSMENT   
OF VIRGIN OLIVE OIL 

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DRAFT DECISION No DEC-III.X/118-
VI/2023 

REVISING THE METHOD FOR THE ORGANOLEPTIC ASSESSMENT 
OF VIRGIN OLIVE OIL 

THE COUNCIL OF MEMBERS OF THE INTERNATIONAL OLIVE COUNCIL, 

Having regard to the 2015 International Agreement on Olive Oil and Table Olives, in particular 
to Article 1 “Objectives of the Agreement” with respect to standardisation and research, as 
regards  to  achieving  uniformity  in  national  and  international  legislation,  and  in  particular 
Chapter VI “Standardisation Provisions”; 

Having regard to Resolution No. RES-2/71-IV/94 of 17 November 1994 on the adoption by 
the  IOC  of  method  COI/T.20/Doc.  No.  15  and  Decision  No.  DEC-III.6/107-VI/2018  on  the 
revision  of  the  method  “Organoleptic  assessment  of  virgin  olive  oil”  COI/T.20/Doc.  No. 
15/Rev.10; 

Considering  the  decision  of  the  organoleptic  assessment  experts  and  panel  leaders 
recognised by the Council and appointed by the Members to revise document T.20/Doc. No. 
15/Rev. 10 “Method for the organoleptic assessment of virgin olive oil”; 

Considering the proposal made by the Chemistry and Standardisation Committee at its 13th 
meeting with a view to revising the method; 

Considering the unanimous position of the organoleptic experts at the meeting of 26 and 
27 September 2023; 

DECIDES 

1. 

2. 

To  revise  the  document  T.20/Doc.  No.  15/Rev.  10  “Method  for  the  organoleptic 
assessment of virgin olive oil”. 
Method  T.20/Doc.  No.  15/Rev.  11  replaces  and  revokes  method  T.20/Doc.  No. 
15/Rev. 10. 

Madrid (Spain), 23 November 2023 

Mr Kaled Musa Al Henefat 

Chair of the International Olive Council 

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INTERNATIONAL 

OLIVE 

COUNCIL 

COI/T.20/Doc. No 15/Rev. 10 11 
June 2018 2024 

ENGLISH 
Original: FRENCH 

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

SENSORY ANALYSIS OF OLIVE OIL 

METHOD FOR THE ORGANOLEPTIC 
ASSESSMENT OF VIRGIN OLIVE OIL 

1. 

PURPOSE 

The purpose of this international method is to determine the procedure for assessing the 
organoleptic characteristics of virgin olive oil and to establish the method for its classification on 
the basis of those characteristics. 

2. 

FIELD OF APPLICATION 

The method described is only applicable to virgin olive oils and to the classification of 
such oils according to the intensity of the defects perceived and of the fruitiness, as determined 
by a group of tasters selected, trained and monitored as a panel. 

It also provides indications for optional labelling. 

3. 

GENERAL BASIC VOCABULARY FOR SENSORY ANALYSIS 

Refer to the standard COI/T.20/Doc. no. 4 "Sensory Analysis:  General Basic 

Vocabulary". 

4. 

SPECIFIC VOCABULARY FOR VIRGIN OLIVE OIL 

4.1.  Negative attributes 

Fusty/muddy 

Sediment  Characteristic flavour of oil obtained from olives piled or stored in such conditions as 
to have undergone an advanced stage of anaerobic fermentation, or of oil which has 
been left in contact with the sediment that settles in underground tanks and vats and 
which has also undergone a process of anaerobic fermentation. 

Musty-humid- 
Earthy 

Characteristic flavour of oils  obtained from fruit in which large numbers  of fungi    
and  yeasts  have  developed  as  a  result  of  its  being  stored  in  humid  conditions  for 
several days or of oil obtained from olives that have been collected with earth or mud 
on them and which have not been washed. 
Characteristic flavour of certain oils reminiscent of wine or vinegar. 

  EN 

Winey- 
vinegary 

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COI/T.20/Doc. No 15/Rev. 10 11 
page 2 

Acid-sour 

This flavour is mainly due to a process of aerobic fermentation in the olives or in 
olive paste left on pressing mats which have not been properly cleaned and leads 
to the formation of acetic acid, ethyl acetate and ethanol. 

Rancid 

Flavour of oils which have undergone an intense process of oxidation. 

Frostbitten olives 
(wet wood)  Characteristic flavour  of  oils  extracted from olives which have been injured  by 

frost while on the tree. 

4.2. 

Other negative attributes 

Heated or 
burnt 

Characteristic flavour of oils caused by excessive and/or prolonged 
heating during processing, particularly when the paste is thermally mixed, if this 
is done under unsuitable thermal conditions. 

Hay–wood  Characteristic flavour of certain oils produced from olives that have dried out. 

Rough 

Thick, pasty mouthfeel sensation produced by certain old oils. 

Greasy 

Flavour of oil reminiscent of that of diesel oil, grease or mineral oil. 

Vegetable 
water 

Flavour acquired by the oil as a result of prolonged contact with 
vegetable water which has undergone fermentation processes. 

Brine 

Flavour of oil extracted from olives which have been preserved in brine. 

Metallic 

Esparto 

Flavour that is reminiscent of metals. It is characteristic of oil which has been in 
prolonged contact with  metallic surfaces during crushing, mixing, pressing or 
storage. 

Characteristic flavour of oil obtained from olives pressed in new esparto mats. The 
flavour may differ depending on whether the mats are made of green esparto or 
dried esparto. 

Grubby 

Flavour of oil obtained from olives which have been heavily attacked by the grubs 
of the olive fly (Bactrocera oleae). 

Cucumber 

Flavour produced when an oil is hermetically packed for too long, particularly in 
tin containers, and which is attributed to the formation of 2,6-nonadienal. 

4.3. 

Positive attributes 

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COI/T.20/Doc. No 15/Rev. 10 11 
page 3 

Fruity 

Set of olfactory sensations characteristic of the oil which depends on the variety 
and comes from sound, fresh olives, either ripe or unripe. It is perceived directly 
and/or through the back of the nose. 

Bitter 

Characteristic  primary  taste  of  oil  obtained  from  green  olives  or  olives  turning 
colour. It is perceived in the circumvallate papillae on the “V” region of the tongue. 

Pungent Biting tactile sensation characteristic of oils produced at the start of the crop year, 
primarily  from  olives  that  are  still  unripe.  It  can  be  perceived  throughout  the 
whole of the mouth cavity, particularly in the throat. 

4.4.  OPTIONAL TERMINOLOGY FOR LABELLING PURPOSES 

Upon request, the panel leader may certify that the oils which have been assessed comply 
with the definitions and ranges corresponding solely to the following expressions according to the 
intensity and perception of the attributes. 

Positive attributes (fruity, bitter and pungent): According to the intensity of perception: 

-  Robust, when the median of the attribute is more than 6.0; 
- Medium, when the median of the attribute is between 3.0 and 6.0; 
- Delicate, when the median of the attribute is less than 3.0. 

Fruitiness     Set of olfactory sensations characteristic of the oil which depends on the variety  of 
olive and comes from sound, fresh olives in which neither green nor ripe fruitiness 
predominates. It is perceived directly and/or through the back of the nose. 

Green fruitiness Set of olfactory sensations characteristic of the oil which is reminiscent of 
green fruit, depends on the variety of olive and comes from green, sound, fresh 
olives. It is perceived directly and/or through the back of the nose. 

Ripe fruitiness Set of olfactory sensations characteristic of the oil which is reminiscent of ripe 
fruit, depends on  the  variety of  olive  and comes from sound, fresh olives.  It is 
perceived directly and/or through the back of the nose. 

Well balanced Oil which does not display a lack of balance, by which is meant the olfactory– 
gustatory  and  tactile  sensation  where  the  median  of  the  bitter  and/or  pungent 
attributes is two points higher than the median of the fruitiness. 

Mild oil 

Oil for which the median of the bitter and pungent attributes is 2.0 or less. 

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List of expressions according to the intensity of perception: 

COI/T.20/Doc. No15/Rev. 10 11 
page 4 

Expressions subject to production 
of an organoleptic test certificate 
Fruitiness 

Ripe fruitiness 

Green fruitiness 

Delicate fruitiness 

Medium fruitiness 

Robust fruitiness 

Delicate ripe fruitiness 

Medium ripe fruitiness 

Robust ripe fruitiness 

Delicate green fruitiness 

Medium green fruitiness 

Robust green fruitiness 

Delicate bitterness 

Medium bitterness 

Robust bitterness 

Delicate pungency 

Medium pungency 

Robust pungency 

Well balanced oil 

Mild oil 

Median of the attribute (Me) 

- 

- 

- 

≤ 3.0 

3.0 < Me ≤ 6.0 

> 6.0 

≤ 3.0 

3.0 < Me ≤ 6.0 
> 6.0 

≤ 3.0 

3.0 < Me ≤ 6.0 
> 6.0 

≤ 3.0 

3.0 < Me ≤ 6.0 

> 6.0 

≤ 3.0 

3.0 < Me ≤ 6.0 
> 6.0 

The median of the bitter attribute and the median 
of the pungent attribute are not more than 2.0 
points above the median of the fruitiness. 
The median of the bitter attribute and the median 
of the pungent attribute are 2.0 or less. 

5. 

GLASS FOR OIL TASTING 

Refer to the standard COI/T.20/Doc. no. 5, “Glass for Oil Tasting” (currently under revision). 

6. 

TEST ROOM 

Refer to the standard COI/T.20/Doc. No. 6, “Guide for the Installation of a Test Room” 
(currently under revision). 

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7. 

ACCESSORIES 

The following accessories, which are required by tasters to perform their task properly, 

shall be supplied in each booth and shall be within easy reach: 

COI/T.20/Doc. No15/Rev. 10 11 
page 5 

- 

- 

- 

- 

- 

- 

- 

glasses (standardised) containing the samples, code numbered, covered with 
a watch-glass and kept at 28 ºC ± 2 ºC; 

profile sheet (see Figure 1)  on  hard  copy, or  on  soft copy provided that  the 
conditions of the profile sheet are met, together with the instructions for its use 
if necessary; 

pen or indelible ink; 

trays with slices of apple, and/or water, (natural or sparkling carbonated water), and/or 
rusks; bread, bread sticks or natural yoghourt; 

glass of water at ambient temperature; 

sheet recalling the general rules listed in sections 9.4 and 10.1.1; 

spittoons. 

8. 

PANEL LEADER AND TASTERS 

8.1. Panel leader 

The panel leader must be a suitably trained person with an expert knowledge of the kinds 
of oils which he or she will come across in the course of their work. They are the key  figure in 
the panel and responsible for its organisation and running. 

The  work  of  the  panel  leader  calls  for  basic  training  in  the  tools  of  sensory  analysis, 
sensory skill, meticulousness in the preparation, organisation and performance of the tests and 
skill and patience to plan and execute the tests in a scientific manner. 

They are the sole person responsible for selecting, training and monitoring the tasters in 
order to ascertain their level of aptitude. They are thus responsible for the appraisal of the tasters, 
which must always be objective and for which they must develop specific procedures based on 
tests and solid acceptance and rejection criteria. See standard COI/T.20/Doc. no. 14 “Guide for 
the selection, training and monitoring of skilled virgin olive oil tasters” (COI/T.20/Doc. no. 14 
currently under revision). 

Panel leaders are responsible for the performance of the panel and hence for its evaluation, 
of which they must give reliable, objective proof. In any case, they must demonstrate at all times 
that the method and tasters are under control. Periodic calibration of the panel is recommended 
(COI/T.20/Doc. 14/ Rev 4 & 5 currently under revision revision). 

They hold ultimate responsibility for keeping the records of the panel. These records must 
always be traceable. They must comply with the assurance and quality requirements laid down in 
international sensory analysis standards and ensure the anonymity of the samples at all times. 

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COI/T.20/Doc. No15/Rev. 10 11 
page 6 

They  shall  be  responsible  for  inventorying  and  ensuring  that  the  apparatus  and 
equipment  needed to  comply with the specifications of this method is properly cleaned and 
maintained  and  shall  keep  written  proof  thereof,  as  well  as  of  the  compliance  with  the  test 
conditions. 

They shall be in charge of the reception and storage of the samples upon their arrival at 
the laboratory as well as of their storage after being tested. When doing so, they shall ensure at 
all times that the samples remain anonymous and are properly stored, for which purpose they must 
develop  written  procedures  in  order  to  ensure  that  the  entire  process  is  traceable  and  affords 
guarantees. 

In addition, they are responsible for preparing, coding and presenting the samples to the 
tasters according to an appropriate experimental design in line with pre-established protocols, as 
well as for assembling and statistically processing the data obtained by the tasters. 

They shall be in charge of developing and drafting any other procedures that might be 

necessary to complement this standard and to ensure that the panel functions properly. 

They must seek ways of comparing the results of the panel with those obtained by other 
panels  undertaking  the  analysis  of  virgin  olive  oil  in  order  to  ascertain  whether  the  panel  is 
working properly. 

It is the duty of the panel leader to motivate the panel members by encouraging interest, 
curiosity and a competitive spirit among them. To do so, they are strongly recommended to ensure 
a smooth two-way flow of information with the panel members by keeping them informed about 
all the tasks they carry out and the results obtained. In addition, they shall ensure that their opinion 
is not known and shall prevent possible leaders from asserting their criteria over the other tasters. 

They  shall  summon  the  tasters  sufficiently  in  advance  and  shall  answer  any  queries 
regarding the performance of the tests, but shall refrain from suggesting any opinion to them on 
the sample. 

8.1.1 Deputy panel leader 

The panel leader may, on justified grounds, be replaced by a deputy panel leader who may 
stand  in  for  duties  regarding  the  performance  of  the  tests.  This  substitute  must  have  all  the 
necessary skills required of a panel leader. 

8.2. Tasters 

The  people acting as  tasters in  organoleptic tests carried out  on  olive  oils  must  do  so 
voluntarily.  It 
is  therefore  advisable  for  candidates  to  submit  an  application  in  writing. 
Candidates shall be selected, trained and monitored by the panel leader in accordance with their 
skills in distinguishing between similar samples; it should be borne in mind that their accuracy 
will improve with training. 

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COI/T.20/Doc. No15/Rev. 10 11 
page 7 

Tasters must act like real sensory observers, setting aside their personal tastes and solely 
reporting the sensations they perceive. To do so, they must always work in silence, in a relaxed, 
unhurried manner, paying the fullest possible sensory attention to the sample they are tasting. 

Between 8 and 12 tasters are required for each test, although it is wise to keep some 

extra tasters in reserve to cover possible absences. 

9. 

TEST CONDITIONS 

9.1. 

Presentation of the sample 

The oil sample for analysis shall be presented in standardised tasting glasses conforming 

to the standard COI/T.20/Doc. No 5 “Glass for oil tasting”. 

The glass shall contain 14–16 ml of oil, or between 12.8 and 14.6 g if the samples are to 

be weighed, and shall be covered with a watch-glass. 

Each glass shall be marked with a code made up of digits or a combination of letters and 

digits chosen at random. The code will be marked by means of an odour-free system. 

9.2. 

Test and sample temperature 

The oil samples intended for tasting shall be kept in the glasses at 28o C ± 2o C throughout 
the  test. This  temperature has been chosen because  it  makes it  easier to  observe organoleptic 
differences  than  at  ambient  temperature  and  because  at  lower  temperatures  the  aromatic 
compounds peculiar to these oils volatilise poorly while higher temperatures lead to the formation 
of volatile compounds peculiar to heated oils. See the standard COI/T.20/Doc. No 5 “Glass for 
Oil Tasting” for the method which has to be used for heating the samples when in the glass. 

The test room must be at a temperature between 20o and 25o C (see COI/T.20/Doc. No 6). 

9.3. 

Test times 

The morning is the best time for tasting oils. It has been proved that there are optimum 
perception periods as regards taste and smell during the day. Meals are preceded by a period in 
which olfactory–gustatory sensitivity increases, whereas afterwards this perception decreases. 

However, this criterion should not be taken to the extreme where hunger may distract the 
tasters, thus decreasing their discriminatory capacity; therefore, it is  recommended to hold the 
tasting sessions between 10.00 in the morning and 12.00 noon. 

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COI/T.20/Doc. No15/Rev. 10 11 
page 8 

9.4. 

Tasters: general rules of conduct 

The following recommendations apply to the conduct of the tasters during their work. 

When called by the panel leader to participate in an organoleptic test, tasters should be 

able to attend at the time set beforehand and shall observe the following: 

• 

• 

• 

• 

• 

• 

• 

• 

They shall not smoke or drink coffee at least 30 minutes before the time set for the test. 

They must not have used any fragrance, cosmetic or soap whose smell could linger until 
the time of the test. They must use an unperfumed soap to wash their hands which they 
shall then rinse and dry as often as necessary to eliminate any smell. 

They shall fast at least one hour before the tasting is carried out. 

Should they  feel  physically  unwell,  and  in  particular  if  their  sense  of  smell  or  taste  is 
affected,  or  if  they  are  under  any  psychological  effect  that  prevents  them  from 
concentrating on their work, the tasters shall refrain from tasting and shall inform the panel 
leader accordingly. 

When they have complied with the above, the tasters shall take up their place in the booth 
allotted to them in an orderly, quiet manner. 

They shall carefully read the instructions given on the profile sheet and shall not begin to 
examine the sample until fully prepared for the task they have to perform (relaxed and 
unhurried). If any doubts should arise, they should consult the panel leader in private. 

They must remain silent while performing their tasks. 

They must keep their mobile phone switched off at all times to avoid interfering with the 
concentration and work of their colleagues. 

10. 

PROCEDURE 
CLASSIFICATION OF VIRGIN OLIVE OIL 

FOR  THE  ORGANOLEPTIC  ASSESSMENT  AND 

10.1.  Tasting technique 

10.1.1. The tasters shall pick up the glass, keeping it covered with the watch-glass, and shall bend 
it gently; they shall then rotate the glass fully in this position so as to wet the inside as 
much as possible. Once this stage is completed, they shall remove the watch-glass and 
smell the sample, taking slow deep breaths to evaluate the oil. Smelling should not exceed 
30 s. If no conclusion has been reached during this time, they shall take a short rest before 
trying again. 

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COI/T.20/Doc. No15/Rev. 10 11 
page 9 

When  the  olfactory test has  been  performed,  the  tasters  shall  then  evaluate  the  buccal 
sensations (overall retronasal olfactory, gustatory and tactile sensations). To do so, they 
shall take a small sip of approximately 3 ml of oil. It is very important to distribute the 
oil throughout the whole of the mouth cavity, from the front part of the mouth and tongue 
along the sides to the back part and to the palate support and throat, since it is a known 
fact that the perception of tastes and tactile sensations varies in intensity depending on the 
area of the tongue, palate and throat. 

It should be stressed that it is essential for a sufficient amount of the oil to be spread very 
slowly over the back of the tongue towards the palate support and throat while the taster 
concentrates on the order in which the bitter and pungent stimuli appear. If this is not 
done, both of these stimuli may escape notice in some oils or else the bitter stimulus may 
be obscured by the pungent stimulus. 

Taking short, successive breaths, drawing in air through the mouth, enables the taster not 
only to spread the sample extensively over the whole of the mouth but also to perceive 
the  volatile  aromatic  compounds  via  the  back  of  the  nose  by  forcing  the  use  of  this 
channel. 

N.B. When the tasters do not perceive fruitiness in a sample and the intensity of the classifying negative attribute is 

3.5  or  less  the  panel  leader  may  decide  to  arrange  for  the  tasters  to  analyse  the  sample  again  at  ambient 
temperature  (COI/T.20/Doc.  No  6/Rev  1,  September  2007  currently  under  revision  ,  section  3  –  General 
specifications  for  installation)  while  specifying  the  context  and  concept  of  ambient  temperature.  When  the 
sample reaches room temperature, the tasters should re-assess it to check solely whether fruitiness is perceived. If 
it is, they should mark the intensity on the scale. 

The tactile sensation of pungency should be taken into consideration. For this purpose, it 
is advisable to ingest the oil. 

10.1.2.  When  organoleptically  assessing  a  virgin  olive  oil,  it  is  recommended  that  FOUR 
SAMPLES at the most be evaluated in each session with a maximum of three sessions 
per day, to avoid the contrast effect that could be produced by immediately tasting other 
samples. 

As successive tastings produce fatigue or loss of sensitivity caused by the preceding 
samples, it is necessary to use a product that can eliminate the remains of the oil from 
the preceding tasting from the mouth. 

The  use  of  a  small slice of  apple is  recommended which, after being chewed,  can  be 
disposed  of  in  the  spittoon.  Then  rinse  out  the  mouth  with  a  little  water  at  ambient 
temperature. At least 15 minutes shall lapse between the end of one session and the start 
of the next. 

10.2.  Use of the profile sheet by tasters 

The profile sheet intended for use by tasters is detailed in Figure 1 of this method. 

Each taster on the panel shall smell and then taste 1/ the oil under consideration. They shall 
then enter the intensity with which they perceive each of the negative and positive attributes on 
the 10-cm scale shown in the profile sheet provided. 

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COI/T.20/Doc. No15/Rev. 10 11 
page 10 

Should the tasters perceive any negative attributes not listed in section 4, they shall record 
them  under  the  "others"  heading,  using  the  term  or  terms  that  most  accurately  describes  the 
attributes. 

10.3.  Use of the data by the panel leaders 

The panel leader shall collect the profile sheets completed by each taster and shall review 
the intensities assigned to the different attributes. Should they find any anomaly, they shall invite 
the taster to revise his or her profile sheet and, if necessary, to repeat the test. 

The  panel leader shall enter  the  assessment data  of  each panel member  in  a  computer 
program like that appended to this method with a view to statistically calculating the results of 
the  analysis, based on  the  calculation  of  their median.  See sections 10.4 and Annex  1  of  this 
method.  The  data  for  a  given  sample  shall  be  entered  with  the  aid  of  a  matrix  comprising  9 
columns representing the 9 sensory attributes and n lines representing the n panel members used. 

When a defect is perceived and entered under the "others" heading by at least 50% of the 
panel,  the  panel  leader  shall  calculate  the  median  of  the  defect  and  shall  arrive  at  the 
corresponding classification. 

The value of the robust coefficient of variation which defines classification (defect with 

the strongest intensity and fruity attribute) must be no greater than 20.0%. 

If the opposite is the case, the panel leader must repeat the evaluation of the specific 

sample in another tasting session. 

If this situation arises often, the panel leader is recommended to give the tasters specific 
additional training (COI/T.20/Doc. No 14/Rev. 4, November 2012, £ 5 currently under 
revision)  and  to  use  the  repeatability  index  and  deviation  index  to  check  taster 
performance  (COI/T.20/Doc.  No  14/Rev.  4,  November  2012,  £  6    currently  under 
revision). 

A method of calculation is illustrated in an example in the annex hereto. 

1/ 

 They may refrain from tasting an oil when they notice any extremely intense negative attribute by direct 
olfactory means, in which case they shall record this exceptional circumstance in the profile sheet. 

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COI/T.20/Doc. No15/Rev. 10 11 
page 11 

10.4.  Classification of the oil 

The oil is graded as follows in line with the median of the defects and the median for the 
fruity attribute. The median of the defects is defined as the median of the defect perceived with 
the  greatest  intensity.  The  median  of  the  defects  and  the  median  of  the  fruity  attribute  are 
expressed to one decimal place. 

The oil is graded by comparing the median value of the defects and the median for the 
fruity attribute with the reference ranges given below. The error of the method has been taken 
into account when establishing the limits of these ranges, which are therefore considered to be 
absolute. The software packages allow the grading to  be  displayed as  a  table of statistics or a 
graph. 

(a) 

(b) 

(c) 

Extra virgin olive oil: the median of the defects is 0.0 and the median of the fruity 
attribute is above 0.0; 

Virgin olive oil: the median of the defects is above 0.0 but not more than 3.5 and 
the median of the fruity attribute is above 0.0; 

Ordinary virgin olive oil: the median of the defects is above 3.5 but not more than 
6.0, or the median of the defects is not more than 3.5 and the median of the fruity 
attribute is 0.0; 

(d) 

Lampante virgin olive oil: the median of the defects is above 6.0. 

Note 1: 

When  the  median  of  the  bitter  and/or  pungent  attribute  is  more  than  5.9,  the 
oanel elader shall state so on the test certificate. Upon request, and depending 
on the positive median of the attributes median of the oils which that have been 
assessed,  the  panel  leader  may  certify  those  attributes  according  to  the 
expressions described in point 4.4 of this document. 

For assessments intended to monitor compliance, one test shall be carried out. In the case of 
counter assessments, the analysis must be carried out in duplicate in different tasting sessions. 
The results of the duplicate analysis must be statistically homogenous. (See section 10.5). If 
not,  the  sample  must  be  reanalysed  twice  again.  The  final  value  of  the  median  of  the 
classification attributes will be calculated using the average of both medians. 

10.5  Criteria for the acceptance and rejection of duplicates 

The normalised error, defined below, shall be used to determine whether the two results of a 
duplicate analysis are homogenous or statistically acceptable: 

where x1 and x2 are the two values of the duplicate and U1 and U2 are the expanded 
uncertainties obtained for the two values, calculated as follows as specified in Annex I: 

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COI/T.20/Doc. No15/Rev. 10 11 
page 12 

For the expanded uncertainty, c = 1.96; hence: 

where CVr is the robust coefficient of variation and Me1 is the median of the first analysis. 

For it to be stated that the two values obtained are not statistically different, En must be equal 
to or less than 1.0. 

10.6  Verification of the declared category 

The organoleptic characteristics of an oil shall be deemed consistent with the declared category if 
a panel recognized by the IOC or approved by the competent authorities at national level confirms 
it. 
Should the panel not confirm the declared category as regards the organoleptic characteristics, the 
interested party may request the national authorities or their representatives to have carried out 
without any delay two independent counter-assessments by two other panels recognised by the 
IOC  or approved by the competent authorities at national level. The characteristics concerned 
shall be deemed consistent with the characteristics declared if both counter- assessments confirm 
the declared category. If that is not the case, the interested party shall be responsible for the cost 
of the two  counter-assessments. 

EN 

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page 13 

Figure 1 

PROFILE SHEET FOR VIRGIN OLIVE OIL INTENSITY OF 

PERCEPTION OF DEFECTS 

Fusty/muddy sediment 

Musty/humid/earthy 

Winey/vinegary 
acid/sour 
Frostbitten olives 
(wet wood) 

Rancid 

Other negative 
attributes: 

Metallic 

  Dry hay 

Grubby 

Rough 

Descriptor: 

Brine 

Heated or burnt 

Vegetable water 

Esparto 

Cucumber 

Greasy 

INTENSITY OF PERCEPTION OF POSITIVE ATTRIBUTES 

Fruity 

Bitter 

Pungent 

Name of taster: 

Sample code: 

Date: 

Comments: 

Green 

Ripe 

Taster code: 

Signature: 

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COI/T.20/Doc. No15/Rev. 10 11 
page 14 

Annex 1 

METHOD FOR CALCULATING THE MEDIAN AND THE CONFIDENCE INTERVALS 

Median 

Me = [p (X < x m) < ½  p (X < x m) > ½] 

The median is defined as the real number xm characterised  by the fact that the probability 
(p) that the distribution values (X) are below this number (xm), is less than and equal to 0.5 and 
that simultaneously the probability (p) that the distribution values (X) are below or equal to xm is 
greater than and equal to 0.5. A more practical definition is that the median is the 50th percentile 
of a distribution of numbers arranged in increasing order. In simpler terms, it is the midpoint of 
an ordered set of odd numbers, or the mean of two midpoints of an ordered set of even numbers. 

Robust standard deviation 

In order to arrive at a reliable estimate of the variability around the mean it is necessary 
to refer to the robust standard deviation as estimated according to Stuart and Kendall (4). The 
formula gives the asymptotic robust standard deviation, i.e. the robust estimate of the variability 
of the data considered where N is the number of observations and IQR is the interquartile range 
which encompasses exactly 50% of the cases of a given probability distribution: 

1.25 x IQR 

s* =  ───── 
1.35 x N 

The interquartile range is calculated by calculating the magnitude of the difference between the 
75th and 25th percentile. 

IQR = 75th percentile - 25th percentile 

Where the percentile is  the  value xpc characterised by the  fact that the probability (p) that the 
distribution  values  are  less  than  xpc  is  less  than  and  equal  to  a  specific  hundredth  and  that 
simultaneously the probability (p) that the distribution values are less than or equal to xpc is greater 
than and equal to that specific hundredth. The hundredth indicates the distribution fractile chosen. 
In the case of the median, it is equal to 50/100. 

n 

n 

percentile = [p (X < xpc) < ──  p (X < xpc) > ── ] 

100 

100 

For practical purposes, the percentile is the distribution value corresponding to a specific 
area subtended from the distribution or density curve. To give an example, the 25th percentile 
represents the distribution value corresponding to an area equal to 0.25 or 25/100. 

In this method percentiles are computed on the basis of the real values which appear in 

the data matrix (percentiles computing procedure). 

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COI/T.20/Doc. No15/Rev. 10 11 
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Robust coefficient of variation (%) 

The CVr% represents a pure number which indicates the percentage variability of the set 
of numbers analysed. For this reason, it is very useful for checking the reliability of the panel 
assessors. 

s* 

CVr = ─── 100 

Me 

Confidence intervals of the median at 95% 

The confidence intervals at 95% (value of the error of the first kind equal to 0.05 or 5%) 
represent the interval within which the value of the median could vary if it were possible to repeat 
an experiment an infinite number of times. In practice, it indicates the interval of variability of 
the  test in  the  operating conditions adopted starting from the  assumption that it  is  possible to 
repeat it many times. As with the CVr%, the interval helps to assess the reliability of the test. 

C.I. upper = Me + (c x s*) 

C.I. lower = Me - (c x s*) 

where C = 1.96 for the confidence interval at the 95% level. 

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COI/T.20/Doc. No15/Rev. 10 11 
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Explanation on the type of algorithm to compute the 25th and 75th percentiles 

IOC uses a unique algorithm (xxx-algorithm), presented below, for the computation of the 25th 
and 75th percentiles. 

It is possible to calculate the statistics either manually or through any data acquisition system 
but the algorithm MUST BE the following. 

The IOC provides an MS Excel worksheet in which the algorithm is applied successfully and 
monitors panel performance. 

Percentiles computing procedure 

There  are  several  ways  of  calculating  a  percentile  but  let’s  describe  and  use  the  following 
algorithm,  also  implemented  in  a  function  {PERCENTILE*(array;k)  k:0.25  and  0.75  or 
QUARTILE(array;q) q:1 and 3} in MS-Excel. 

[*in French version of MS-Excel CENTILE(array;k) or QUARTIL(array;q)] 

Step 1 - Sort the list of numbers into ascending order and score these numbers from 1 to n 

Step 2 - Use the following formula to calculate the corresponding ranking (split into an 

integer and a decimal). 

R=1+(P(n-1)/100)=I+D 

{ranks computation} 

where: 

P: percentile wanted 
n: total number of values 
I:  integer  part  of  ranking 
D: decimal part of ranking 

Step 3 - Use the following formula to interpolate between the necessary two numbers. 

p=YI+D(YI+1-YI) 

{interpolation} 

Example (EVEN NUMBER OF TASTERS) 

Computation of percentiles 

Raw data 

1.3 
2.1 
1.5 
1.2 
1.6 
2.4 
2.3 
1.9 

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COI/T.20/Doc. No15/Rev. 10 11 
page 17 

Ordered data 

1.2 
1.3 
1.5 
1.6 
1.9 
2.1 
2.3 
2.4 

Median=1.8 

Computing ranking 

r=1+(P(n-1)/100) 

{ranks computation} 

P: percentile (25 or 75) 
n: number of cases 
I: integer part of ranking 
D: decimal part of ranking 

1+((25*(8-1))/100)=2.75 

I=2 (integer) 
D=0.75 (decimal) 

1+((75*(8-1))/100)=6.25 

I=6 (integer) 
D=0.25 (decimal) 

Interpolating 

p=YI + D(YI+1 – YI) 

{interpolation} 

1.3+0.75*(1.5-1.3)=1.45 (25th percentile) 

2.1+0.25*(2.3-2.1)=2.15 (75th percentile) 

From excel {PERCENTILE(A2:A9;0.25 or 0.75)} 

25th percentile=1.45 
75th percentile=2.15 

Computation of IQR 

IQR= 75th percentile – 25th percentile 

IQR=2.15-1.45=0.7 

Computations of s* 

s*= Coefficient * IQR / Square root (Number of Judges) 

s*=0.925*0.7/2.828=0.23 

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COI/T.20/Doc. No15/Rev. 10 11 
page 18 

CVr% = (s* / Median) * 100 

CVr%=(0.23/1.75)=13.1% 

The classification is reliable 

Example (ODD NUMBER OF TASTERS) 

Computation of percentiles 

Raw data 

1.3 
2.1 
1.5 
1.2 
1.6 
2.4 
2.3 
1.9 
1.6 
1.8 
2.7 

Ordered data 

1.2 
1.3 
1.5 
1.6 
1.6 
1.8 
1.9 
2.1 
2.3 
2.4 
2.7 

Median=1.8 

Computing ranking 

r=1+(P(n-1)/100) 

P: percentile (25 or 75) 
n: number of cases 
I: integer part of ranking 
D: decimal part of ranking 

1+((25*(11-1))/100)=3.5 

I=3 (integer) 
D=0.5 (decimal) 

1+((75*(11-1))/100)=8.5 

I=8 (integer) 
D=0.5 (decimal) 

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COI/T.20/Doc. No15/Rev. 10 11 
page 19 

Interpolating 

p=YI + D(YI+1 – YI) 

1.5+0.5*(1.6-1.5)=1.55 (25th percentile) 

2.1+0.5*(2.3-2.1)=2.20 (75th percentile) 

From Excel {PERCENTILE(A2:A9;0.25 or 0.75)} 

25th percentile=1.55 
75th percentile=2.20 

Computation of IQR 

IQR= 75th percentile – 25th percentile 

IQR=2.20-1.55=0.65 

Computations of s* 

s*= Coefficient * IQR / Square root (Number of Judges) 

s*=0.925*0.65/3.317=0.18 

CVr% = (s* / Median) * 100 

CVr%=(0.18/1.80)=10.0% 

The classification is reliable 

Function PERCENTILE in different languages 

Language 

Function 
“PERCENTILE” 

FRAKTIL 
PROSENTTIPISTE 
CENTILE 
PERSENTIL 
PERCENTIEL 
PERCENTYL 
PERCENTIL 

Czechoslovak  PERCENTIL 
Danish 
Finnish 
French 
Norwegian 
Dutch 
Polish 
Portuguese 
Russian 
Spanish 
Swedish 
German 
Turkish 
Hungarian 

PERCENTIL 
PERCENTIL 
QUANTIL 
YÜZDEBIRLIK 
PERCENTILIS 

EN 

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Bibliography 

(1) Wilkinson, L. 1990. Systat: The system for statistics. Evanston, 

IL.SYSTAT Inc. 

(2) Cicchitelli, G. 1984. Probabilità e Statistica. Maggioli Editore, Rimini. 

(3)  Massart, D.L.; Vandeginste, B.G.M.; Deming, Y.; Michotte, L. 
1988. Chemometrics. A textbook. Elsevier. Amsterdam. 

(4)  Kendall,  M.G.;  Stuart,  A.  1967.  The  advanced  theory  of 
statistics. Vol. 1. Hafner Publishing Co. 

(5)  McGill, R.; Tukey, J.W.; Larsen, W.A. 1978. Variation of Box 
Plots. The American Statistician, 32, (2), 12-16. 

(6) COI/T.28/Doc.  No  1  September  2007  “Guidelines  for  the 
accreditation  of  sensory  testing  laboratories  with  particular 
reference  to  virgin  olive  oil  according  to  standard  ISO/IEC 
17025:2005” 

(7) COI/T.20/Doc. No 14/Rev. 3 November 2011 currently under 
revision 

(8) ISO/IEC 17025:05 currently under revision 

EN 

  EN 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
DRAFT DECISION No DEC III.X/118-VI/ 2023 

CONCERNING THE METHOD FOR THE DETERMINATION OF  
THE CONTENT OF WAXES, FATTY ACID ETHYL ESTERS BY 
CAPILLARY GAS CHROMATOGRAPHY 

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DRAFT DECISION Nº DEC-III.X/118-VI/2023 

CONCERNING THE METHOD FOR THE DETERMINATION OF THE CONTENT OF 
WAXES, FATTY ACID ETHYL ESTERS BY CAPILLARY GAS CHROMATOGRAPHY 

THE COUNCIL OF MEMBERS OF THE INTERNATIONAL OLIVE COUNCIL, 

Having  regard  to  the  International Agreement  on  Olive  Oil  and Table  Olives,  2015,  in 
particular Article 1 “Objectives of the Agreement” concerning standardisation and research, 
as  regards  achieving  uniformity  in  national  and  international  legislation,  and  the 
harmonisation of physico-chemical and organoleptic analysis, to improve knowledge of the 
composition  and  quality  characteristics  of  olive  products,  and  in  particular  Chapter  VI 
“Standardisation provisions”; 

Having  regard  to  the  recommendation  made  by  the  Chemistry  and  Standardisation 
Committee at its 13th meeting during the 118th session of the Council of Members; 

Considering the ring tests carried out by the chemists on waxes and ethyl esters; 

Considering the unanimous position of the chemistry experts appointed by Members at 
their  meeting  on  5  and  6  October  2023,  and  the  recommendation  to  incorporate  the 
modification  into  document  COI/T.20/Doc.  No  28/Rev.  3  and  subsequently  issue  a 
corrigendum for the latter; 

DECIDES 

To adopt the corrigendum for revision 3 of the document COI/T.20/Doc. No 28/Rev. 3 Corr. 
1 on the method of analysis for the determination of the content of waxes and fatty acid 
ethyl esters by capillary gas chromatography. 

Both  methods A  and  B  can  be  used  for  official  control.  Method A  (15  g  of  silica)  is  the 
reference method for counter-assessment. 

Document  COI/T.20/Doc.  No.  28/Rev.  3  Corr.  1  November  2023  replaces  and  repeals 
document COI/T.20/Doc. No 28/Rev. 3 November 2022. 

Madrid (Spain), 23 November 2023 

Mr Kaled Musa Al Henefat 

Chair of the International Olive Council 

EN 

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INTERNATIONAL  

COI/T.20/Doc. No 28/Rev. 3 Corr 1 
November 2023  

OLIVE 

COUNCIL 

ENGLISH 
Original: ENGLISH 

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

METHOD OF ANALYSIS 

DETERMINATION OF THE CONTENT OF WAXES AND FATTY ACID ETHYL 

ESTERS BY CAPILLARY GAS CHROMATOGRAPHY 

METHOD A (15 g of silica) 

1. 

PURPOSE 
This method is for the determination of the content of waxes and fatty acid ethyl esters in 

olive oils. The individual waxes and alkyl esters are separated according to the number of 

carbon atoms. The method is recommended as a tool for distinguishing between olive oil 

and olive-pomace oil, and as a quality parameter for extra virgin oils, as it  facilitates the 

identification of false blends of extra virgin olive oils and low-quality oils and determines 

whether they are virgin, lampante or deodorized oils. This document presents two methods 

that can be used for official control. Method A (15 g of silica) is the reference method for 

counter-assessment. 

2. 

PRINCIPLE 
Addition  of suitable  internal  standards  to  the oil  and  fractionation  by  chromatography  on 

hydrated silica gel column. Recovery of the fraction eluted under the test conditions (with a 

lower  polarity  than  that  of  the  triacylglycerols)  and  direct  analysis  by  capillary  gas 

chromatography. 

3. 

APPARATUS 

3.1.  Test tube, 10 ml. 
3.2.  Glass column for liquid chromatography, internal diameter 15 mm, length 40 cm, fitted 

with a suitable stopcock. 

3.3.  Gas chromatograph suitable for use with a capillary column, equipped with a system for 

direct, on-column injection comprising: 

3.3.1.  Thermostat-controlled oven with temperature programming. 

3.3.2.  Cold injector for direct on-column injection 

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COI/T.20/Doc. No 28 
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3.3.3.  Flame ionisation detector and converter-amplifier. 

3.3.4.  Recorder-integrator  (Note 1) for use with  the converter-amplifier  (3.3.3), with  a 

response time of not more than 1 s and a variable paper speed. 

3.3.5.  Capillary column, fused silica (for analysis of the waxes and methyl and ethyl 

esters), length 8-12 m, internal diameter 0.25-0.32 mm, internally coated with liquid 

phase (Note 2) to a uniform thickness of 0.10-0.25 m. 

3.4.  Microsyringe, 10 l, with hardened needle, for direct on-column injection. 

3.5.  Electric shaker. 

3.6.  Rotary evaporator. 

3.7.  Muffle oven. 

3.8.  Analytical balance for weighing to an accuracy of ± 0.1 mg. 

3.9.  Usual laboratory glassware. 

4.1. 

4.2. 

 REAGENTS 

4. 
Silica gel, 60-200 m mesh. Place the silica gel in the muffle oven at 500 °C for at 
least 4 hours. Allow to cool and then add 2% water in relation to the quantity of silica 
gel used. Shake well to homogenise slurry and keep in the desiccator for at least 12 
hours prior to use. If the silica gel is ultra-pure grade, the muffle oven treatment will 
not be necessary. 
n-Hexane,  chromatography  (or  residue)  grade  –  the  purity  must  be  checked  as 
follows: 100 ml of n-hexane are evaporated to dryness, residue is re-dissolved in 100 
µl n-heptane, and analysed applying the same gas chromatographic conditions. There 
must  be  no  peak  in  the  elution  alkyl  esters  area.  (Hexane  can  be  replaced  by 
Isooctane) Hexane – Chromosolv Pestanal is available from Honeywell-Riedel-de 
Haen (code 34484). 
This reference is an example of suitable products, which are available commercially. 
This information is given for the convenience of users of this Standard and does not 
constitute an endorsement of these products. 

WARNING – Fumes may ignite. Keep away from sources of heat, sparks or naked flames. 
Make sure the bottles are always properly closed. Ensure proper ventilation during usage. 
Avoid  build-up  of  fumes  and  remove  any  possible  fire  risk,  such  as  heaters  or  electric 
apparatus not manufactured from non- 

Note 1.  Computerised systems may also be used where the gas chromatography data are entered   
through a PC. 

Note 2.  Suitable commercial liquid phases are available for this purpose such as SE52, SE54 (methyl 
silicon with 5% phenyl), etc. or other phase with similar or lower polarity. 

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COI/T.20/Doc. No 28 
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and remove any possible fire risk, such as heaters or electric apparatus not manufactured from non-
inflammable material. Harmful if inhaled because it may cause nerve cell damage. Avoid breathing 
in the fumes. Use a suitable respiratory apparatus if necessary. Avoid contact with eyes and skin. 
Ethyl ether, chromatography grade.  
WARNING – Highly inflammable and moderately toxic. Irritates the skin. Harmful if inhaled. May 
cause damage to eyes. Effects may be delayed. It can form explosive peroxides. Fumes may ignite. 
Keep away from sources of heat, sparks or naked flames. Make sure the bottles are always properly 
closed. Ensure proper ventilation during usage. Avoid build-up of fumes and remove any possible 
fire risk, such as heaters or electric apparatus not manufactured from non-inflammable material. Do 
not evaporate to dryness or near dryness. The addition of water or an appropriate reducing agent 
can reduce peroxide formation. Do not drink. Avoid breathing in the fumes. Avoid prolonged or 
repeated contact with skin. 
n-heptane, chromatography grade, or iso-octane 
WARNING – Inflammable. Harmful if inhaled. Keep away from sources of heat, sparks or naked 
flames. Make sure the bottles are always properly closed. Ensure proper ventilation during usage. 
Avoid breathing in the fumes. Avoid prolonged or repeated contact with skin. 
Standard solution of lauryl arachidate (Note 3) at 0.02% (m/V) in heptane (internal standard for 
waxes). 
Standard solution of methyl heptadecanoate at 0.005% (m/V) in heptane (internal standard for 
methyl and ethyl esters). 
Sudan  1  (1-phenylazo-2-naphthol)  optional  (attention:  azo-compounds  have  mutagenic  and 
carcinogenic properties) 

4.3. 

4.4. 

4.5. 

4.6. 

4.7. 

4.8.  Carrier gas: hydrogen or helium, pure, gas chromatography grade. 

WARNING 
Hydrogen.  Highly  inflammable,  under  pressure.  Keep  away  from  sources  of  heat,  sparks,  naked 
flames or electric apparatus not manufactured from non-inflammable material. Make sure the bottle 
valve is shut when not in use. Always use with a pressure reducer. Release the tension of the reducer 
spring before opening the bottle valve. Do not stand in front of the bottle outlet when opening the 
valve. Ensure proper ventilation during usage. Do not transfer hydrogen from one bottle to another. 
Do not mix gas in the bottle. Make sure the bottles cannot be knocked over. Keep them away from 
sunlight  and  sources  of  heat.  Store  in  a  corrosive-free  environment.  Do  not  use  damaged  or 
unlabelled bottles. 
Helium. Compressed gas at high pressure. It reduces the amount of oxygen available for breathing. 
Keep the bottle shut. Ensure proper ventilation during usage. Do not enter storage areas unless they 
are properly ventilated. Always use with a pressure reducer. Release the tension of the reducer spring 
before opening the bottle valve. Do not transfer gas from one bottle to another. Make sure the bottles 
cannot be knocked over. Do not stand in front of the bottle outlet when opening the valve. Keep them 
away from sunlight and  

Note 3. Palmityl palmitate, myristyl stearate or arachidyl laureate may also be used. 

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COI/T.20/Doc. No 28 
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sources of heat. Store in a corrosive-free environment. Do not use damaged or unlabelled bottles. Do 

not inhale. Use solely for technical purposes. 

4.9. Auxiliary gases: 

-  Hydrogen, pure, gas chromatography grade.  

-  Air, pure, gas chromatography grade. 

WARNING 

Air. Compressed gas at high pressure. Use with caution in the presence of combustible substances 

as the self-ignition temperature of most of the organic compounds in the air is considerably lower 

under high pressure. Make sure the bottle valve is shut when not in use. Always use a pressure 

reducer. Release the tension of the reducer spring before opening the bottle valve. Do not stand 

in front of the bottle outlet when opening the valve. Do not transfer gas from one bottle to another. 

Do not mix gas in the bottle. Make sure the bottles cannot be knocked over. Keep them away 

from sunlight and sources of heat. Store in a corrosive-free environment. Do not use damaged or 

unlabelled bottles. Air intended for technical purposes must not be used for inhaling or respiratory 

apparatus.  

PROCEDURE 

5. 
Preparation of the chromatography column 

5.1. 

Suspend 15 g of silica gel (4.1) in n-hexane (4.2) and introduce into the column (3.2). Allow to 

settle  spontaneously.  Complete  settling  with  the  aid  of  an  electric  shaker  (3.5)  to  make  the 

chromatographic bed more homogeneous. Percolate 20 ml of n-hexane to remove any impurities. 

Weigh exactly 500 mg of the sample into the 10-ml test tube (3.1), using the analytical balance 

(3.8),  and  add  a  suitable  amount  of  internal  standard  (4.5)  depending  on  the  assumed  wax 

content, e.g. add 0.10 mg of lauryl arachidate in the case of extra virgin olive oil, virgin olive 

oil, refined olive oil and olive oil, 0.25-0.50 mg in the case of olive-pomace oil and 0.05 mg of 

methyl  heptadecanoate  for  extra  virgin  olive  oils  (4.6).  Transfer  the  prepared  sample  to  the 

chromatography column with the aid of two 2-ml portions of n-hexane (4.2). Allow the solvent 

to flow to 1 mm above the upper level of the absorbent. Percolate a 50 ml n-hexane/ethyl ether 

(99:1)  to  further  remove  hydrocarbons  (alkanes  and  sterenes)  of  n-hexane/ethyl  ether  (99:1) 

(Note 4) and collect 150 ml at a flow of about 15 drops every 10 seconds. 

(This fraction contains ethyl esters and waxes) (Note 5). 

Note 4. The n-hexane/ethyl ether (99:1) mixture should be freshly prepared every day, n-hexane 
can be replaced with the same amount of iso octane 
Note 5 . 100 l of Sudan I dye at 1% in the elution mixture can be added to the sample solution to 
check visually that the waxes are eluted properly. The retention time of the dye lies in between that 
of the waxes and triacylglycerols. Hence, when the dye reaches the bottom of the chromatography 

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COI/T.20/Doc. No 28 
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Evaporate the resultant fractions in a rotary evaporator (3.6) until the solvent is almost removed. Remove 

the last 2 ml under a weak current of nitrogen. Collect the fraction containing the ethyl esters and waxes 

diluted with 1-2 ml of n-heptane or iso-octane. 

5.2.  Gas chromatography analysis 
5.2.1.  Preliminary procedure 

Fit the column to the gas chromatograph (3.3), connecting the inlet port to the on-column system and 

the  outlet  port  to  the  detector.  Check  the  gas  chromatography  apparatus  (operation  of  gas  loops, 

efficiency of detector and recorder system, etc.). 

If the column is being used for the first time, it is advisable to condition it. Run a light flow of gas through 

the column, then switch on the gas chromatography apparatus. Gradually heat to 350 °C (approximately 

4 hours). 

Maintain this temperature for at least 2 hours, then regulate the apparatus to the operating conditions 

(regulate  gas  flow,  light  flame,  connect  to  electronic  recorder  (3.3.4),  regulate  oven  temperature  for 

column, regulate detector, etc.). Record the signal at a sensitivity at least twice as high as required for 

the analysis. The base line should be linear, with no peaks of any kind, and must not have any drift. 

Negative  straight-line  drift  indicates  that  the  column  connections  are  not  correct  while  positive  drift 

indicates that the column has not been properly conditioned. 

5.2.2. 

Choice of operating conditions for waxes and ethyl esters (Note 6) 

The operating conditions are generally as follows: 

-   Column temperature: 

                       20 °C/min         5 °C/min          

80 °C at first (1’)        140 °C         335 °C (20’) for ethyl esters and waxes 

                             20 °C/min               5°C/min                 20 °C/min              

80 °C at first (1’)           240 °C              325 °C (6’)            340 ºC (10’) for waxes only 

-   Detector temperature: 350 °C. 

-  Amount injected: 1 µl of n-heptane solution (1-2ml). 
-  Carrier gas: helium or hydrogen at the optimal linear speed for the gas chosen (see Annex A). 
-  Instrument sensitivity: suitable for fulfilling the above conditions. 

These conditions may be modified to suit the characteristics of the column and the gas chromatograph 

in order to separate all the waxes and fatty acid ethyl esters and to obtain satisfactory peak separation 

(see Figures1-2) and a retention time of 18  3 minutes for the lauryl arachidate internal standard. The 

most representative peak of the waxes must be over 60% of the full-scale value in the case of refined 

olive oil, olive oil, olive pomace oils, while it should be between 60% and full scale in the case of extra 

virgin olive oil and virgin olive oil. The methyl heptadecanoate internal standard for the ethyl esters must 

fit the full-scale value. 

column, elution must be suspended because all the waxes have been eluted. Verify the correct elution 
by checking the presence on the chromatogram at the same time of squalene and epoxy squalene. 

Note 6 . Due to the high final temperature, positive drift is allowed but may not exceed more than 
10% of the full-scale value. 

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COI/T.20/Doc. No 28 
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- 

- 

Carrier gas: helium or hydrogen at the optimal linear speed for the gas chosen (see 

Annex A). 

Instrument sensitivity: suitable for fulfilling the above conditions. 

5.3. 

 Performance of the analysis 

Take up 1-2 µl of the solution with the aid of the 10 µl micro-syringe, drawing back 

the plunger until the needle is empty. Introduce the needle into the injection system 

and inject quickly after 1–2 s. After about 5 s, gently extract the needle.  

Perform the recording until the waxes (C40-C46) are completely eluted, depending 

on the fraction being analysed.  

The base line must always meet the required conditions. 

5.4.  Peak identification 

Identify  the  peaks  from  the  retention  times  by  comparing  them  with  mixtures  of 

waxes with known retention times, analysed under the same conditions. The alkyl 

esters are identified from mixtures of methyl and ethyl esters of the main fatty acids 

in olive oils (palmitic and oleic).  

Figure 1. Shows a chromatogram of the FAEE and waxes in an extra virgin olive oil using 

the  

method A (15 g). 

Figure 2. Shows a chromatogram of the FAEE and waxes in a lampante olive oil using the 

method A (15 g). 

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5.5.  Quantitative analysis of the waxes 

Determine the area of the peaks corresponding to the lauryl arachidate internal standard and 

the aliphatic esters from C42 to C46 in the case of extra virgin olive oil and virgin olive oil and 

form C40 to C46 in the case of other oils, with the aid of the integrator. 

COI/T.20/Doc. No 28 
page 7 

Determine the content of each individual wax, in mg/kg of fat, as follows: 

𝑊𝑎𝑥𝑒𝑠, 𝑚𝑔/𝑘𝑔 =

𝐴𝑥 ∗ 𝑚𝑠 ∗ 1000
𝐴𝑠 ∗ 𝑚

where: 

Ax = 

area  corresponding  to  the  peak  for  the  individual  ester,  in  computer 

counts (peak no. 11-13, 14-15, 16-17-18 in fig. 2) 

As    = 

area  corresponding  to  the  peak  for  the  lauryl  arachidate  internal 

standard, in computer counts 

ms  = 

mass of the lauryl arachidate internal standard added, in milligrams 

m   = 

mass of the sample taken for determination, in grams 

5.6.  Quantitative analysis of the ethyl esters 

Using  the  integrator,  determine  the  areas  of  the  peaks  corresponding  to  the  methyl 

heptadecanoate internal standard, the ethyl esters of the C16 and C18 fatty acids. 

Determine the content of ethyl ester, in mg/kg of fat, as follows: 

𝐸𝑠𝑡𝑒𝑟, 𝑚𝑔/𝑘𝑔 =

𝐴𝑥 ∗ 𝑚𝑠 ∗ 1000
𝐴𝑠 ∗ 𝑚

where: 

Ax = 

area corresponding to the peak for the individual C16 and C18 ethyl ester, 

in computer counts 

As    = 

area corresponding to the peak for the methyl heptadecanoate internal 

standard, in computer counts 

ms  = 

mass  of  the  methyl  heptadecanoate 

internal  standard  added, 

in 

milligrams; 

m   = 

mass of the sample taken for determination, in grams.  

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COI/T.20/Doc. No 28 
page 8 

6. 

EXPRESSION OF RESULTS 

Report the sum of the contents of the different waxes from C42 to C46 in the case of extra 

virgin and virgin  olive oils  and from  C40 to  C46 in  the case of other oils (Note  7) in 

milligrams per kilograms of fat (ppm). 

Report the sum of the contents of the ethyl esters from C16 to C18 and the total of the 

two. 

Results should be expressed to one decimal place. 

-Results should be expressed to the nearest mg/kg. 

Note 7 . The components for quantification refer to the peaks with even carbon numbers amongst 
the C40-C46 esters, according to the specimen chromatogram of the waxes in olive oil provided in 
the attached figure. 

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COI/T.20/Doc. No 28 
page 9 

METHOD B (3 g OF SILICA) 

1. 

PURPOSE 

This method is for the determination of the content of waxes and fatty acid ethyl esters in 

olive oils. The individual waxes and alkyl esters are separated according to the number of 

carbon atoms. The method is recommended as a tool for distinguishing between olive oil and 

olive-pomace  oil  and  as  a  quality  parameter  for  extra  virgin  oils,  as  it  facilitates  the 

identification of false blends of extra virgin olive oils and low-quality oils and determines 

whether they are virgin, lampante or deodorized oils. 

2. 

PRINCIPLE 

Addition of suitable internal standards to the oil and fractionation by chromatography on a 

hydrated silica gel column. Recovery of the fraction eluted under the test conditions (with a 

lower  polarity  than  that  of  the  triacylglycerols)  and  direct  analysis  by  capillary  gas 

chromatography. 

3. 

APPARATUS 

3.1.  Test tube, 10 ml. 

3.2.  Glass  column  for  liquid  chromatography,  internal  diameter  10  mm,  length  40  cm, 

fitted with a suitable stopcock. 

3.3.  Gas chromatograph suitable for use with a capillary column, equipped with a system 

for direct, on-column injection comprising: 

3.3.1.  Thermostat-controlled oven with temperature programming. 

3.3.2.  Cold injector for direct on-column injection 

3.3.3.   Flame ionisation detector and converter-amplifier 

3.3.4.  Recorder-integrator (Note 1) for use with the converter-amplifier (3.3.3), with a response 

time of not more than 1 s and a variable paper speed. 

Note 1 . Computerised systems may also be used where the gas chromatography data are entered 
through a PC. 

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COI/T.20/Doc. No 28 
page 10 

3.3.5. Capillary column, fused silica (for analysis of the waxes and methyl and ethyl esters), length 8-12 
m,  internal  diameter  0.25-0.32  mm,  internally  coated  with  liquid  phase  (Note  2)  to  a  uniform 
thickness of 0.10-0.25 µm. 

3.4.  Microsyringe, 10 µl, with hardened needle, for direct on-column injection. 
3.5.  Electric shaker. 
3.6.  Rotary evaporator. 
3.7.  Muffle oven. 
3.8.  Analytical balance for weighing to an accuracy of ± 0.1 mg. 
3.9.  Usual laboratory glassware. 

REAGENTS 

4. 
4.1.  Silica gel, 60-200 µm mesh. Place the silica gel in the muffle oven at 500 °C for at least 4 hours. 
Allow to cool and then add 2% water in relation to the quantity of silica gel used. Shake well to 
homogenise slurry and keep in the desiccator for at least 12 hours prior to use.  If the silica gel is 
ultra-pure grade, the muffle oven treatment will not be necessary. 

4.2.  n-Hexane, chromatography or residue grade the purity must be checked as follows 200 ml of n-
hexane are evaporated to dryness, residue is redissolved in 100 µl n-heptane and analysed applying 
the same gas chromatographic conditions. There must be no peak in the elution alkyl esters area. 
(Hexane can be replaced by Isoctane) Hexane – Chromosolv Pestanal is available from Honeyell-
Riedel-de Haen (code 34484). 

This reference is an example of suitable products which are available commercially. This information is 

given for the convenience of users of this Standard and does not constitute an endorsement of 

these products.  

WARNING – Fumes may ignite. Keep away from sources of heat, sparks or naked flames. Make sure the 

bottles are always properly closed. Ensure proper ventilation during usage. Avoid build-up of fumes 

and remove any possible fire risk, such as heaters or electric apparatus not manufactured from non-

inflammable material. Harmful if inhaled because it may cause nerve cell damage. Avoid breathing 

in the fumes. Use a suitable respiratory apparatus if necessary. Avoid contact with eyes and skin. 

4.3.  Ethyl ether, chromatography grade. 

WARNING – Highly inflammable and moderately toxic. Irritates the skin. Harmful if inhaled. May 

cause damage to eyes. Effects may be delayed. It can form explosive peroxides. Fumes may ignite. 

Keep away  

Note 2. Suitable commercial liquid phases are available for this purpose such as SE52, SE54 (methyl 

silicon with 5% phenyl), etc. or other phase with similar or lower polarity. 

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COI/T.20/Doc. No 28 
page 11 

from  sources  of  heat,  sparks  or  naked  flames.  Make sure  the  bottles  are  always  properly  closed. 
Ensure proper ventilation during usage. Avoid build-up of fumes and remove any possible fire risk, 
such  as  heaters  or  electric  apparatus  not  manufactured  from  non-inflammable  material.  Do  not 
evaporate to dryness or near dryness. The addition of water or an appropriate reducing agent can 
reduce peroxide formation. Do not drink. Avoid breathing in the fumes. Avoid prolonged or repeated 
contact with skin. 

4.4. 

n-heptane, chromatography grade, or iso-octane. 

WARNING  –  Inflammable.  Harmful  if  inhaled.  Keep  away  from  sources  of  heat,  sparks  or  naked 

flames. Make sure the bottles are always properly closed. Ensure proper ventilation during usage. 

Avoid breathing in the fumes. Avoid prolonged or repeated contact with skin. 

4.5. 

4.6. 

4.7. 
4.8. 

Standard solution of lauryl arachidate (Note 3), at 0.01% (m/V) in heptane (internal standard 
for waxes). 
Solution of methyl heptadecanoate, at 0.002% (m/V) in heptane (internal standard for methyl 
and ethyl esters). 
Sudan 1 (1-phenylazo-2-naphthol) 
Carrier gas: hydrogen or helium, pure, gas chromatography grade.  

WARNING 

Hydrogen. Highly  inflammable under pressure. Keep away from sources of heat,  sparks, naked 

flames or electric apparatus not manufactured from non-inflammable material. Make  sure the 

bottle valve is shut when not in use. Always use with a pressure reducer. Release the tension of 

the reducer spring before opening the bottle valve. Do not stand in front of the bottle outlet when 

opening the valve. Ensure proper ventilation during usage. Do not transfer hydrogen from one 

bottle to another. Do not mix gas in the bottle. Make sure the bottles cannot be knocked over. 

Keep them away from sunlight and sources of heat. Store in a corrosive-free environment. Do not 

use damaged or unlabelled bottles. 

Helium. Compressed gas at high pressure. It reduces the amount of oxygen available for breathing. 

Keep the bottle shut. Ensure proper ventilation during usage. Do not enter storage areas unless they 

are properly ventilated. Always use with a pressure reducer. Release the tension of the reducer spring 

before opening the bottle valve. Do not transfer gas from one bottle to another. Make sure the bottles 

cannot be knocked over. Do not stand in front of the bottle outlet when opening the valve. Keep them 

away from sunlight and sources of heat. Store in a corrosive-free environment. Do not use damaged 

or unlabelled bottles. Do not inhale. Use solely for technical purpose. 

4.9. 

Auxiliary gases: 
-  Hydrogen, pure, gas chromatography grade.  
-  Air, pure, gas chromatography grade. 

Note 3. Palmityl palmitate, myristyl stearate or arachidyl laureate may also be used.  

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COI/T.20/Doc. No 28 
page 12 

WARNING 

Air. Compressed gas at high pressure. Use with caution in the presence of combustible substances as 

the self-ignition temperature of most of the organic compounds in the air is considerably lower under 

high pressure. Make sure the bottle valve is shut when not in use. Always use a pressure reducer. 

Release the tension of the reducer spring before opening the bottle valve. Do not stand in front of 

the bottle outlet when opening the valve. Do not transfer gas from one bottle to another. Do not mix 

gas in the bottle. Make sure the bottles cannot be knocked over. Keep them away from sunlight and 

sources of heat. Store in a corrosive-free environment. Do not use damaged or unlabelled bottles. Air 

intended for technical purposes must not be used for inhaling or respiratory apparatus. 

5. 
5.1. 

PROCEDURE 
Preparation of the chromatography column 
Suspend 3 g of silica gel (4.1) in n-hexane (4.2) and introduce into the column (3.2). Allow 

to settle spontaneously. Complete settling with the aid of an electric shaker (3.5) to make 

the chromatographic bed more homogeneous. Percolate 10 ml of n-hexane to remove any 

impurities. Weigh exactly 100 mg of the sample into the 10-ml test tube (3.1), using the 

analytical balance (3.8), and add a suitable amount of internal standard (4.5) depending on 

the assumed wax content, e.g. add 0.01 mg of lauryl arachidate in the case of extra virgin 

olive oil, virgin olive oil, refined olive oil and olive oil, 0.025-0.10 mg in the case of olive-

pomace oil and 0.002 mg of methyl heptadecanoate for extra virgin olive oil and olive oil 

(4.6). Transfer the prepared sample to the chromatography column with the aid of two 2-

ml portions of n-hexane (4.2). 

Allow the solvent to flow to 1 mm above the upper level of the absorbent. Percolate a 12-

15  ml  n-Hexane  (*)  to  further  remove  hydrocarbons  (alkanes  and  sterenes)  of  n-
hexane/ethyl ether (99:1) (Note 4) and collect 40-45 ml at a flow of about 15 drops every 10 
seconds.  
This fraction contains the ethyl esters and waxes (Note 5). 
(*) Not necessary for the determination of waxes only. 

Note 4. The n-hexane/ethyl ether (99:1) mixture should be freshly prepared every day, n-hexane can 
be replaced with the same amount of iso octane. 
Note 5. 100 µl of Sudan I dye at 1% in the elution mixture can be added to the sample solution to 
check visually that the waxes are eluted properly. The retention time of the dye lies in between that 
of the waxes and triacylglycerols. Hence, when the dye reaches the bottom of the chromatography 
column, elution must be suspended because all the waxes have been eluted. 

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COI/T.20/Doc. No 28 
page 13 

Evaporate  the  resultant  fractions  in  a  rotary  evaporator  (3.6)  until  the  solvent  is  almost 

removed.  Remove  the  last  2  ml  under  a  weak  current  of  nitrogen.  Collect  the  fraction 

containing the methyl and ethyl esters diluted with 0.5-1 ml of n-heptane or iso-octane. 

5.2.  Gas chromatography analysis 

5.2.1.  Preliminary procedure 

Fit the column to the gas chromatograph (3.3), connecting the inlet port to the on-column 

system  and  the  outlet  port  to  the  detector.  Check  the  gas  chromatography  apparatus 

(operation of gas loops, efficiency of detector and recorder system, etc.). 

If the column is being used for the first time, it is advisable to condition it. Run a light flow 

of gas through the column, then switch on the gas chromatography apparatus. Gradually 

heat to 350 °C (approximately 4 hours). 

Maintain this temperature for at least 2 hours, then regulate the apparatus to the operating 

conditions (regulate gas flow, light flame, connect to electronic recorder (3.3.4), regulate 

oven temperature for column, regulate detector, etc.). Record the signal at a sensitivity at 

least twice as high as that required for the analysis. The base line should be linear, with no 

peaks of any kind, and must not have any drift. Negative straight-line drift indicates that the 

column connections are not correct while positive drift indicates that the column has not 

been properly conditioned. 

5.2.2.  Choice of operating conditions for waxes and ethyl esters (Note 6) 

The operating conditions are generally as follows: 

-  

Column temperature: 

                              20 °C/min 

  5 °C/min          

  80 °C at first (1’)         140 °C          335 °C (20’) for ethyl esters and waxes 

         20 °C/min 

         5 °C/min          

  80 °C at first (1’)              200 °C          335 °C (20’) for waxes only 

-   Detector temperature: 350 °C. 

- 

Amount injected: 1 µl of n-heptane solution (0.5-1ml). 

Note 6. Due to the high final temperature, positive drift is allowed but may not exceed more than 
10% of the full-scale value. 

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COI/T.20/Doc. No 28 
page 14 

- 

- 

Carrier gas: helium or hydrogen at the optimal linear speed for the gas chosen (see 

Annex A). 

Instrument sensitivity: suitable for fulfilling the above conditions. 

These conditions may be modified to suit the characteristics of the column and the gas 

chromatograph in order to separate all the waxes and fatty acid ethyl esters and to obtain 

satisfactory peak separation (see Figures1-2) and a retention time of 18  3 minutes for 

the lauryl arachidate internal standard. 

The most representative peak of the waxes must be over 60% of the full-scale value in the 

case of refined olive oil, olive oil, olive pomace oils, while it should be between 60% and 

full  scale  in  the  case  of  extra  virgin  olive  oil  and  virgin  olive  oil.  The  methyl 

heptadecanoate internal standard for the ethyl esters must fit the full-scale value. 

- 

- 

Carrier gas: helium or hydrogen at the optimal linear speed for the gas chosen (see 

Annex A). 

Instrument sensitivity: suitable for fulfilling the above conditions. 

5.3.  Performance of the analysis 

Take up 1-2 µl of the solution with the aid of the 10 µl micro-syringe, drawing back 

the plunger until the needle is empty. Introduce the needle into the injection system 

and inject quickly after 1–2 s. After about 5 s, gently extract the needle. 

Perform  the  recording  until  the  waxes  are  completely  eluted,  depending  on  the 

fraction being analysed. 

The base line must always meet the required conditions. 

5.4.  Peak identification 

Identify  the  peaks  from  the  retention  times  by  comparing  them  with  mixtures  of 

waxes with known retention times, analysed under the same conditions. The alkyl 

esters are identified from mixtures of methyl and ethyl esters of the chief fatty acids 

in olive oils (palmitic and oleic).  

Annex A reports some examples of chromatograms of ethyl esters and waxes suitable 

to identify related peaks. 

Figure 3. Shows a chromatogram of the FAEE and waxes in an extra virgin olive oil 

using the method B (3 g). 

Figure 4. Shows the chromatograms of FAEE and waxes in a virgin olive oil using 

the method B (3 g). 

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COI/T.20/Doc. No 28 
page 15 

5.5.  Quantitative analysis of the waxes 

Determine  the  area  of  the  peaks  corresponding  to  the  lauryl  arachidate  internal 

standard  and  the  aliphatic  esters  from  C42  to  C46  in  the  case  of  extra  virgin  and 

virgin olive oils and from C40 to C46 for other oils with the aid of the integrator. 

     Determine the content of each individual wax, in mg/kg of fat, as follows: 

𝑊𝑎𝑥𝑒𝑠, 𝑚𝑔/𝑘𝑔 =

𝐴𝑥 ∗ 𝑚𝑠 ∗ 1000
𝐴𝑠 ∗ 𝑚

  where: 

Ax = 

area  corresponding  to  the  peak  for  the  individual  ester,  in  computer 

counts (peak n° 11- 13, 14-15,16-17-18 in fig.2) 

As    = 

area corresponding to the peak for the lauryl arachidate internal standard, 

in computer counts 

ms   = 

mass of the lauryl arachidate internal standard added, in milligrams 

            m =  mass of the sample taken for determination, in grams. 

5.6.  Quantitative analysis of the ethyl esters 

With the aid of the integrator, determine the areas of the peaks corresponding to the 

methyl heptadecanoate internal standard, the ethyl esters of the C16 and C18 fatty 

acids. Determine the content of ethyl ester, in mg/kg of fat, as follows: 

𝐸𝑠𝑡𝑒𝑟, 𝑚𝑔/𝑘𝑔 =

𝐴𝑥 ∗ 𝑚𝑠 ∗ 1000
𝐴𝑠 ∗ 𝑚

where: 

Ax = 

area corresponding to the peak for the individual C16 and C18 ethyl ester, 

in computer counts 

As    = 

area corresponding to the peak for the methyl heptadecanoate internal 

standard, in computer counts 

ms  = 

mass  of  the  methyl  heptadecanoate 

internal  standard  added, 

in 

milligrams; 

m   = 

mass of the sample taken for determination, in grams.  

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COI/T.20/Doc. No 28 
page 16 

6. 

EXPRESSION OF RESULTS 

Report the sum of the contents of the different waxes from C42 to C46 in the case of extra 

virgin olive oil and virgin olive oil and from C40 to C46 in the case of other oils (Note 7) in 

milligrams per kilograms of fat. 

Report the sum of the contents of the ethyl esters from C16 to C18 and the total of the two. 

Results  should  be  expressed  to  one  decimal  place.  Results  should  be  expressed  to  two 

decimal places, up to 1 mg/kg above this with one decimal place. 

Results should be expressed to the nearest mg/kg. 

Note 7. The components for quantification refer to the peaks with even carbon numbers amongst the 
C40-C46 esters, according to the specimen chromatogram of the waxes in olive oil provided in the 
attached figure. 

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COI/T.20/Doc. No 28 
page 17 

ANNEX A 

Examples of chromatograms: 

The following chromatograms are reported as an aid to identify peaks as well as to give information 

about the separation to be obtained. 

Figure 1: Chromatogram of FAEE and waxes of EVOO using method A (15 g). 

Figure 2: Chromatogram of FAEE and waxes of Lampante olive oil using method A (15 
g). 

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COI/T.20/Doc. No 28 
page 18 

Figure 3: Chromatogram of FAEE and waxes of EVOO using method B (3 g). 

Figure 4: Chromatogram of FAEE and waxes of VOO using method B (3 g). 

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COI/T.20/Doc. No 28 
page 19 

ANNEX B 

Determination of linear gas speed 

Inject 1:3  μl of  methane  (or  propane)  into  the gas chromatograph  after adjusting  it to  the normal 

operating conditions. Measure the time the gas takes to run through the column from the moment it 

is injected until the peak emerges (tM). 

The linear speed in cm/s is given by L/tM where L is the length of the column, in cm, and tM is the time 

measured in s. 

ANNEX C 

Precision values of the ethyl esters and wax method  

Analysis of the collaborative test results  

The  results  of  the  collaborative  test  organised  by  the  IOC  Executive  Secretariat  were  statistically 

processed according to the rules laid down in the international standards ISO 5725.  

Accuracy (trueness and precision) of measurement methods and results. Outliers were examined 

by applying Cochran’s and Grubbs’s test to the laboratory results for each determination (replicates a 

and b). 

The precision values of the method are given in the table overleaf. 

The table lists: 

n 

number of participating laboratories 

outliers number of laboratories with outlying values  

mean 

mean of the accepted results 

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 may be expected to lie with a probability of 95%  

Sr 

repeatability standard deviation. 

RSDr (%) 

repeatability coefficient of variation (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 different operators using different equipment may be expected to lie with a 

probability of 95%. 

Sr 

reproducibility standard deviation  

RSDr (%) 

reproducibility coefficient of variation (Sr x 100 / mean) 

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COI/T.20/Doc. No 28 
page 20 

Ethyl esters (mg/kg) – Method A 15 g of silica  

Sample 

Mean 

n 

outliers 

Sr 

RSDr (%) 

r 

SR 

RSDR (%) 

R 

Sample 

Mean 

n 

outliers 

Sr 

RSDr (%) 

r 

SR 

RSDR (%) 

R 

Sample 

Mean 

n 

Outliers 

Sr 

RSDr (%) 

r 

SR 

RSDR (%) 

R 

M1 

10 

16 

3 

0.574 

5.74 

1.61 

0.759 

7.59 

2.12 

M2 

8.21 

16 

2 

0.330 

4.02 

0.92 

0.915 

11.15 

2.56 

M3 

36.97 

16 

0 

1.316 

3.56 

3.68 

3.720 

10.06 

10.42 

M4 

50.83 

16 

0 

1.934 

3.80 

5.41 

6.736 

13.25 

18.86 

Waxes  (mg/kg) Method A 15 g of silica 

M1 

93.00 

16 

4 

0.610 

0.66 

1.71 

8.053 

8.66 

22.55 

M2 

45.17 

16 

1 

1.406 

3.11 

3.94 

4.879 

10.80 

13.66 

M3 

38.54 

16 

2 

1.315 

3.41 

3.68 

5.590 

14.51 

15.65 

M4 

M5 

323.17 

2350.72 

16 

1 

4.346 

1.34 

12.17 

16 

0 

35.728 

1.52 

100.04 

23.649 

247.180 

7.32 

66.22 

10.52 

692.10 

Ethyl esters (mg/kg) -Method B  (3 g of silica) 

M1 

10.00 

15 

4 

M2 

8.15 

15 

4 

M3 

39.22 

15 

0 

0.570 

0.225 

1.234 

5.90 

1.65 

1.681 

14.00 

3.92 

2.76 

0.63 

0.991 

12.16 

2.77 

3.15 

3.46 

4.450 

11.34 

12.46 

M4 

52.46 

15 

0 

1.903 

3.63 

5.33 

4.691 

8.94 

13.13 

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Waxes (mg/kg) Method B (3 g of silica) 

M1 

M2 

M3 

M4 

M5 

90.45 

45.53 

38.81 

325.47 

2354.21 

15 

2 

15 

1 

15 

2 

15 

0 

15 

0 

1.770 

2.306 

1.745 

7.758 

50.548 

1.96 

4.96 

15.287 

16.90 

42.80 

5.06 

6.46 

7.066 

15.52 

19.79 

4.50 

4.89 

8.236 

21.22 

23.06 

2.38 

2.15 

21.72 

141.54 

23.614 

213.990 

7.26 

9.09 

66.12 

599.17 

Sample 

Mean 

n 

Outliers 

Sr 

RSDr (%) 

r 

SR 

RSDR (%) 

R 

ANNEX D  

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 
– Part 6: Use in practice of accuracy values 

Accuracy (trueness and precision) of measurement methods and results 

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DECISION Nº. xxx/2024 

REVISING THE TRADING  STANDARD  FOR  OLIVE  OIL AND  OLIVE-
POMACE OIL 

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INTERNATIONAL 

OLIVE  

COUNCIL 

COI/T.15/NC No 3/Rev. 19 20 
June 2024 

ENGLISH 
Original: FRENCH 

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  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: 

(i) Extra virgin olive oil: virgin olive oil which has a 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. 

EN 

  EN 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 2 

(ii) Virgin olive oil: virgin olive oil which has a 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. 

(iii) Ordinary virgin olive oil: virgin olive oil which has a 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 a 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: olive oil obtained from virgin olive oils by refining methods which 
do not lead to alterations in the initial glyceridic structure. It has a 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: oil consisting of a blend 
of refined olive oil and virgin olive oils fit for consumption as they are. It has a 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 oil3/ 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: 

2.2.1.  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. 

____________ 
1/  This product may only be sold direct to the consumer if permitted in the country of retail 
sale.  If  not  permitted,  the  designation  of  this  product  shall  comply  with  the  legal 
provisions of the country concerned. 

2/  This product may only be sold direct to the consumer if permitted in the country of retail 

sale. 

3/  Olive pomace oil cannot be sold with the designation or definition “olive oil”. 

EN 

  EN 

 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 3 

2.2.2.  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 a 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.1/ 

2.2.3.  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 a 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.2/ 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): 

-  Myristic acid 
-  Palmitic acid 
-  Palmitoleic acid 
-  Heptadecanoic acid 
-  Heptadecenoic acid 
-  Stearic acid 
-  Oleic acid 
-  Linoleic acid 
-  Linolenic acid 
-  Arachidic acid 
-  Gadoleic acid (eicosenoic) 
-  Behenic acid 
-  Lignoceric acid 

< 0.03 
7.00 - 20.00 
0.30 - 3.50 
< 0.40 
< 0.60 
0.50 - 5.00 
55.00 - 85.00 
2.50 - 21.00 
< 1.003/ 
< 0.60 
< 0.50 
< 0.20* 
< 0.20 

__________ 

1/  This product may only be sold direct to the consumer if permitted in the country of retail 

sale. 

2/  The country of retail sale may require a more specific designation. 
3/  When  an  edible  virgin  olive  oil  exhibits  1.00<linolenic  acid%≤1.40,  then  this  oil  is 
authentic, provided that App. β-sito/Campe content ≥ 24 and all other purity criteria lie 
within the official limit 

*  Limit raised to < 0.30 for olive pomace oils. 

EN 

  EN 

 
 
 
 
 
 
 
 
 
 
3.2. 

Trans fatty acid content (% trans fatty acids) 

COI/T.15/NC No 3/Rev. 19 20 
page 4 

C18:1  T 
% 

C18:2 T + 
C18:3 T % 

< 0.05 
< 0.10 
< 0.20 
< 0.20 
< 0.20 
< 0.40 
< 0.40 

< 0.05 
< 0.10 
< 0.30 
< 0.30 
< 0.10 
< 0.35 
≤ 0.35 

-  Edible virgin olive oils 
-  Lampante virgin olive oil 
-  Refined olive oil 
-  Olive oil (ROO+VOOs)1 
-  Crude olive pomace oil 
-  Refined olive pomace oil 
-  Olive pomace oil (ROPO+VOOs)2 

3.3. 

Sterol and triterpene dialcohol composition 

3.3.1.  Desmethylsterol composition (% total sterols) 

-  Cholesterol 
-  Brassicasterol 
-  Campesterol 
-  Stigmasterol 
-  Delta 7 stigmastenol 
-  Apparent beta sitosterol: 

beta-sitosterol + delta-5-avenasterol 
+ delta-5-23-stigmastadienol +clerosterol 
+ sitostanol + delta 5-24-stigmastadienol 

< 0.5 
< 0.1* 
< 4.0** 
< campesterol in edible oils 
< 0.5*** 
> 93.0 

__________ 
1 Blend of refined olive oil and virgin olive oils 
2 Blend of refined olive pomace oil and virgin olive oils 

*  Limit raised to < 0.2 for olive pomace oils. 

**  An  extra  virgin  or  virgin  olive  oil  that  exhibits  4.0<  campesterol  %  ≤4.5  is  authentic 
provided  that  stigmasterol  ≤1.4%,  Δ7-stigmastenol  ≤0.3%  and  all  other  parameters  lie 
within the limits fixed in this standard. 

*** An olive oil or olive-pomace oil that exhibits 0.5< Δ7-stigmastenol % ≤0.8 is authentic 

provided that: 

a) app. β-sitosterol/campesterol≥28, ΔECN42 ≤│0.10│ (for extra virgin or virgin olive 

oil) 

b) app.  β-sitosterol/campesterol≥28,  ΔECN42  ≤│0.15│,  stigmastadiene≤0.30  (for 

lampante virgin olive oil) 

c) app. β-sitosterol/campesterol≥28, ΔECN42≤│0.15│ (for refined olive oil or olive oil 

(ROO+VOOs)) 

d) stigmasterol ≤1.4%, ΔECN42 ≤│0.40│ (crude olive-pomace oil, refined olive-pomace 

oil or olive pomace oil (ROPO+VOOs)) 

In all the above cases, all other parameters lie within the limits fixed in this standard. 

EN 

  EN 

 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 5 

3.3.2.  Total sterol content 

(mg/kg) 

-  Virgin olive oils 
-  Refined olive oil 
-  Olive oil (ROO+VOOs) 
-  Crude olive pomace oil 
-  Refined olive pomace oil 
-  Olive pomace oil (ROPO+VOOs) 

3.3.3.  Erythrodiol and uvaol content 

(% total sterols) 

-  Edible virgin olive oils 
-  Lampante virgin olive oil 
-  Refined olive oil 
-  Olive oil (ROO+VOOs) 
-  Crude olive pomace oil 
-  Refined olive pomace oil 
-  Olive pomace oil (ROPO+VOOs) 

3.4.  Wax content 

(mg/kg) 

C42 + C44 + C46 (mg/kg) 
- 

Extra virgin olive oil and virgin olive oil 

C40 + C42 + C44 + C46 (mg/kg) 
-  Ordinary virgin olive oil 
Lampante virgin olive oil 
- 
- 
Refined olive oil 
-  Olive oil (ROO+VOOs) 
Crude olive pomace oil 
- 
- 
Refined olive pomace oil 
-  Olive pomace oil (ROPO+VOOs) 

> 1000 

> 2500 
> 1800 
> 1600 

< 4.5 
< 4.51/ 
< 4.52/ 
< 4.5 
> 4.53/ 
> 4.5 
> 4.5 

< 150 

< 250 
< 3001/ 
< 350 
< 350 
> 3502/ 
> 350 
> 350 

__________ 

1/  When the oil has a wax content between 300 mg/kg and 350 mg/kg it is considered a 
lampante  virgin  olive  oil  if  the  total  aliphatic  alcohol  content  is  <  350  mg/kg  or  the 
erythrodiol + uvaol content is < 3.5%. 

2/  When the oil has an erythrodiol + uvaol content of between 4.5 and 6 %, the erythrodiol 

content must be < 75 mg/kg. 

3/  When the oil has a wax content between 300 mg/kg and 350 mg/kg it is considered a 
crude  olive  pomace  oil  if  the  total  aliphatic  alcohol  content  is  >  350  mg/kg  and  the 
erythrodiol + uvaol content is > 3.5%. 

EN 

  EN 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
3.5.  Maximum  difference  between  the  actual  and  theoretical  ECN  42  triacylglycerol 

content (%) 

COI/T.15/NC No 3/Rev. 19 20 
page 6 

-  Edible virgin olive oils 
-  Lampante virgin olive oil 
-  Refined olive oil 
-  Olive oil (ROO+VOOs) 
-  Crude olive pomace oil 
-  Refined olive pomace oil 
-  Olive pomace oil (ROPO+VOOs) 

3.6. 

  Stigmastadiene content 

(mg/kg) 

-  Extra virgin olive oil and virgin olive oil 
-  Ordinary virgin olive oil 
-  Lampante virgin olive oil 

3.7.  Content of 2-glyceryl monopalmitate 

(%) 

≤ |0.20| 
≤ |0.30| 
≤ |0.30| 
≤ |0.30| 
≤ |0.60| 
≤ |0.50| 
≤ |0.50| 

< 0.05 
< 0.10 
< 0.50 

-  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) 
-  Crude and refined olive pomace oils  

< 1.2% 
< 1.4% 

3.8.  Unsaponifiable matter 

(g/kg) 

-  Olive oils 
-  Olive pomace oils 

< 15 
< 30 

EN 

  EN 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
4.  QUALITY CRITERIA 

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

COI/T.15/NC No 3/Rev. 19 20 
page 7 

Extra 
virgin 
olive 
oil 

Virgin 
olive 
oil 

Ordinary 
virgin 
olive 
oil 

Lampante 
virgin 
olive 
oil* 

Refined 
olive 
oil 

Olive 
Oil 
(ROO+VO
Os) 

Crude 
olive 
pomace 
oil 

Refined 
olive  
pomace 
oil 

Olive 
pomace 
oil 
(ROPO+VO
Os) 

4.1 Organoleptic 
characteristics 

- odour and taste 

- median of defect 
- median of the fruity 
attribute 

- colour 

- aspect at 20oC for 
24 hours 

Me = 0.0 
Me > 0.0 

0.0 < Me < 3.5 
Me > 0.0 

3.5 <Me < 6.0** 

Me > 6.0 

acceptable 

good 

acceptable 

good 

Light yellow 

Light 
yellow to 
green 

Light yellow 
to brownish 
yellow 

Light yellow 
to green 

limpid 

limpid 

limpid 

limpid 

4.2. Free acidity 

< 0.80 

< 2.0 

< 3.3 

> 3.3 

< 0.30 

< 1.00 

no limit 

< 0.30 

< 1.00 

% m/m expressed in 
oleic acid 

4.3. Peroxide value 

< 20.0 

< 20.0 

< 20.0 

no limit 

< 5.0 

< 15.0 

no limit 

< 5.0 

< 15.0 

in milleq. peroxide 
oxygen per kg/oil 

* ..... 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. 

EN 

  EN 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 8 

4.  QUALITY CRITERIA (contd.) 

Extra 
virgin 
olive 
oil 

Virgin 
olive 
oil 

Ordinary 
virgin 
olive 
oil 

Lampante 
virgin 
olive 
oil 

Refined 
olive 
oil 

Olive 
Oil 
(ROO+VOOs) 

Crude 
olive 
pomace 
oil 

Refined 
olive 
pomace 
oil 

Olive 
pomace 
oil 
(ROPO+VOOs) 

4.4. Absorbency in ultra-violet 

- 270 nm (cyclohexane) / 
  268 nm (iso-octane) 
- K 
- 232 nm* 

< 0.22 

< 0.25 

< 0.01 
< 2.50** 

< 0.01 
< 2.60** 

< 0.30 

< 0.01 

< 1.25 

< 0.16 

< 1.15 

< 0.15 

< 2.00 

< 0.20 

< 1.70 

< 0.18 

4.5. Moisture and volatile matter 

< 0.2 

< 0.2 

< 0.2 

< 0.3 

< 0.1 

< 0.1 

< 1.5 

< 0.1 

< 0.1 

(% m/m) 

4.6. Insoluble impurities in light 

< 0.10 

< 0.10 

< 0.10 

< 0.20 

< 0.05 

< 0.05 

< 0.05 

< 0.05 

petroleum 
(% m/m) 

4.7. Flash point 

4.8. Trace metals 
(mg/kg) 
Iron 
Copper 

< 3.0 
< 0.1 

< 3.0 
< 0.1 

< 3.0 
< 0.1 

< 3.0 
< 0.1 

< 3.0 
< 0.1 

< 3.0 
< 0.1 

< 3.0 
< 0.1 

< 3.0 
< 0.1 

> 120oC 

4.9. Fatty acid ethyl esters 

≤ 35 mg/kg 

(FAEEs) 

4.10. Phenols content 

See section 11.21 

* ..... 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. 

EN 

  EN 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 9 

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. 

6.3. 

Halogenated solvents 

-  Maximum content of each halogenated solvent 
-  Maximum content of the sum of all halogenated solvents 

0.1 mg/kg 
0.2 mg/kg 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 10 

7. 

HYGIENE 

7.1. 

7.2. 

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. 

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; 

8.2. 

8.3. 

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

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. 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 11 

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 oil1/ 
- Refined olive oil1/ 
- Olive oil (ROO+VOOs)2/ 

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. 

________________ 
1/ 

This product may only be sold direct to the consumer if permitted in the country of retail sale. 

2/ 

The country of retail sale may require a more specific designation. 

 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 12 

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, the country in which such processing is carried out shall be considered as the country of 
origin for 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. 

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. 

 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 13 

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.  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. 

10.3.2.  Net contents 

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

10.3.3.  Name and address 

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

10.3.4.  Country of origin 

The name of the exporting country shall be declared. 

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. 

11.1. 

Sampling 

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

11.2. 

Preparation of the test sample 

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

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 14 

11.3. 

Determination of the fatty acid composition and trans fatty acid content 

According to COI/T.20/Doc. No 33/Rev.2, “Determination of the fatty acid composition in olive and olive-
pomace oils by gas chromatography” 

11.4.  Determination 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”. 

11.5.  Determination 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. 

11.6.  Determination 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. 

11.7.  Determination 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. 

11.8.  Determination 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. 

11.9.  Determination of the organoleptic characteristics 

According to COI/T.20/Doc. No 15/Rev. 10 11, "Organoleptic assessment of virgin olive oil". 

11.10.  Determination of the free acidity 

According to COI/T.20/Doc. No 34/Rev.1, “Determination of free fatty acids, cold method”. 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 15 

11.11.  Determination of the peroxide value 

According 
ISO 3960, or AOCS Cd 8b-90. 

to  COI/T.20/Doc.  No  35/Rev.1, 

“Determination  of 

the  peroxide  value”, 

11.12.  Determination 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. 

11.13.  Determination of the moisture and volatile matter 

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

11.14.  Determination of the insoluble impurities in light petroleum 

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

11.15.  Determination of the flash point 

According to the FOSFA International method. 

11.16.  Detection of trace metals 

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

11.17.  Determination of the alpha-tocopherol 

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

11.18.  Determination 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. 

11.19.  Detection of traces of halogenated solvents 

According  to  COI/T.20/Doc.  No  8,  “Determination  of  tetrachloroethylene  in  olive  oils  by  gas-liquid 
chromatography”. 

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
COI/T.15/NC No 3/Rev. 19 20 
page 16 

11.20.  Determination of the content of waxes and alkyl esters 

[According to COI/T.20/Doc. No 28/Rev.3 Corr 1, “Determination of the content of waxes, fatty acid methyl 
esters and fatty acid ethyl esters by capillary gas chromatography“. 

11.21.  Determination of biophenols 

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

11.22.  Determination 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”. 

11.23.  Determination 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”.