Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contents

The purpose of this document is to describe a procedure for the determination of the ester content in fatty acid methyl esters (FAME) intended for incorporation into diesel oil. It also allows determining the linolenic acid methyl ester content. It allows verifying that the ester content of FAME is greater than 90 % (m/m) and that the linolenic acid content is between 1 % (m/m) and 15 % (m/m).
This method is suitable for FAME which contains methyl esters between C6 and C24.
NOTE 1   For the purposes of this document, the terms "% (m/m)" and "% (v/v)" are used to represent respectively the mass and volume fractions.
NOTE 2   This method was elaborated for FAME samples from usual raw material. For FAME sample from unidentified raw material, a solution of the test sample should be prepared without any internal standard addition, in order to verify the absence of natural nonadecanoic acid methyl ester.
NOTE 3   The distribution off fatty acid methyl esters is given in Annex C.
WARNING - The use of this method may involve hazardous equipment, materials and operations. This method does not purport to address to all of the safety problems associated with its use, but it is the responsibility of the user to search and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Ester-Gehaltes und des Gehaltes an Linolensäure-Methylester

Dieses Dokument legt ein Prüfverfahren für die Bestimmung des Estergehaltes in Fettsäure¬methylester (FAME) fest, die als Blendkomponente für Dieselkraftstoff Verwendung finden. Darüber hinaus ermöglicht das Verfahren auch, den Gehalt an Linolensäuremethylester zu bestimmen. Mit diesem Verfahren lässt sich sicherstellen, dass der Estergehalt in Fettsäuremethylester größer als 90 % (m/m) ist und der Gehalt an Linolensäure zwischen 1 % (m/m) und 15 % (m/m) ist.
Dieses Prüfverfahren ist für Methylester mit einer Kettenlänge von C6 bis C24 anwendbar.
ANMERKUNG 1   Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils einer Substanz der Ausdruck "% (m/m)" und für den Volumenanteil einer Substanz der Ausdruck "% (V/V)" verwendet.
ANMERKUNG 2   Dieses Verfahren wurde für FAME-Proben aus üblichen Rohstoffen ausgearbeitet. Bei FAME-Proben aus einem nicht identifizierten Rohstoff wird eine Lösung der Untersuchungsprobe ohne Zugabe eines internen Standards hergestellt, um das Nichtvorhandensein von natürlichem Methyl-Nonadecanoat nachzuweisen.
ANMERKUNG 3   Die Verteilung von Fettsäuremethylestern ist in Anhang C angeführt.
WARNUNG - Die Anwendung dieses Verfahrens kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Dieses Verfahren beansprucht nicht, alle mit seiner Anwendung verbundenen Sicherheitsprobleme zu behandeln, es liegt jedoch in der Verantwortung des Anwenders vor der Anwendung angemessene Maßnahmen hinsichtlich Sicherheit und Gesundheit zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln.

Produits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) - Détermination de la teneur en ester et en ester méthylique de l'acide linolénique

Le présent document a pour objet de décrire un mode opératoire de détermination de la teneur en ester des esters méthyliques d’acides gras (EMAG) destinés à être incorporés dans des carburants diesel. Il permet également la détermination de la teneur en ester méthylique de l’acide linolénique. Il permet de vérifier que la teneur en ester des EMAG est supérieure à 90 % (m/m) et que la teneur en ester méthylique de l’acide linolénique est comprise entre 1 % (m/m) et 15 % (m/m).
Cette méthode est applicable aux EMAG dont les esters méthyliques sont compris entre C6 et C24.
NOTE 1   Pour les besoins du présent document, les termes « % (m/m) » et « % (v/v) » sont utilisés pour représenter respectivement les fractions massiques et volumiques.
NOTE 2   Cette méthode a été élaborée pour les échantillons d’EMAG préparés à partir des matières premières courantes. Pour un échantillon d’EMAG issu de matières premières non identifiées, une solution de l’échantillon pour essai est préparée sans ajout d’aucun étalon interne, afin de vérifier l’absence de nonadécanoate de méthyle naturel.
NOTE 3   La distribution des esters méthyliques d’acides gras est donnée à l’Annexe C.
AVERTISSEMENT - La présente méthode peut impliquer l’utilisation de produits et la mise en oeuvre de modes opératoires et d’appareillages à caractère dangereux. La présente méthode n’a pas pour but d’aborder tous les problèmes de sécurité liés à son utilisation, mais il incombe à l’utilisateur de rechercher et d’établir, avant de l’utiliser, des pratiques d’hygiène et de sécurité appropriées et de déterminer l’applicabilité des restrictions réglementaires.

Derivati maščob in olj - Metilni estri maščobnih kislin (FAME) - Določevanje estra in metilnega estra linolenske kisline

Namen tega dokumenta je opisati postopek določevanja vsebnosti estra v metilnih estrih maščobnih kislin (FAME) za vključitev v dizelsko gorivo. Omogoča tudi določevanje vsebnosti metilnega estra linolenske kisline. Z dokumentom je mogoče preveriti, ali je vsebnost metilnega estra maščobne kisline večja od 90 % (m/m) in ali je vsebnost linolenske kisline od 1 do 15 % (m/m). Ta metoda je primerna za metilne estre maščobnih kislin, ki vsebujejo metilne estre v območju od C6 do C24.
OPOMBA 1: V tem dokumentu sta uporabljeni oznaki % (m/m) in % (v/v), ki predstavljata masni oziroma prostorninski delež.
OPOMBA 2: Ta metoda je bila izdelana za vzorce metilnih estrov maščobnih kislin iz običajnih surovin. Za vzorce metilnih estrov maščobnih kislin iz neznanih surovin naj se pripravi raztopina preskusnega vzorca brez dodajanja internega standarda, da se preveri odsotnost metilnega estra naravne nonadekanojske kisline.
OPOMBA 3: Porazdelitev metilnih estrov maščobnih kislin je podana v dodatku C.
OPOZORILO: Pri uporabi te metode so lahko prisotni nevarna oprema, materiali in postopki. Ta metoda ne obravnava vseh varnostnih težav, ki se navezujejo na njeno uporabo, vendar pa je za iskanje in vzpostavitev ustreznih varnostnih in zdravstvenih praks ter za določitev uporabnosti regulativnih omejitev pred uporabo odgovoren uporabnik.

General Information

Status
Published
Public Enquiry End Date
24-Nov-2018
Publication Date
09-Feb-2020
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
04-Feb-2020
Due Date
10-Apr-2020
Completion Date
10-Feb-2020

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SLOVENSKI STANDARD
SIST EN 14103:2020
01-marec-2020
Nadomešča:
SIST EN 14103:2011

Derivati maščob in olj - Metilni estri maščobnih kislin (FAME) - Določevanje estra

in metilnega estra linolenske kisline

Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and

linolenic acid methyl ester contents

Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester

(FAME) - Bestimmung des Ester-Gehaltes und des Gehaltes an Linolensäure-
Methylester
Produits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) -

Détermination de la teneur en ester et en ester méthylique de l'acide linolénique

Ta slovenski standard je istoveten z: EN 14103:2020
ICS:
67.200.10 Rastlinske in živalske Animal and vegetable fats
maščobe in olja and oils
SIST EN 14103:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN 14103:2020
---------------------- Page: 2 ----------------------
SIST EN 14103:2020
EN 14103
EUROPEAN STANDARD
NORME EUROPÉENNE
January 2020
EUROPÄISCHE NORM
ICS 67.200.10 Supersedes EN 14103:2011
English Version
Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) -
Determination of ester and linolenic acid methyl ester
contents

Produits dérivés des corps gras - Esters méthyliques Erzeugnisse aus pflanzlichen und tierischen Fetten und

d'acides gras (EMAG) - Détermination de la teneur en Ölen - Fettsäure-Methylester (FAME) - Bestimmung

ester et en ester méthylique de l'acide linolénique des Ester-Gehaltes und des Gehaltes an Linolensäure-

Methylester
This European Standard was approved by CEN on 18 November 2019.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14103:2020 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 14103:2020
EN 14103:2020 (E)
Contents Page

European foreword ...................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 4

5 Reagents ............................................................................................................................................................. 5

6 Apparatus .......................................................................................................................................................... 5

7 Sampling ............................................................................................................................................................. 5

8 Procedure .......................................................................................................................................................... 5

8.1 Operating conditions ..................................................................................................................................... 5

8.2 Internal standard GC purity determination .......................................................................................... 6

8.3 FAME sample preparation and analysis ................................................................................................. 6

8.4 Identification .................................................................................................................................................... 7

9 Calculation ......................................................................................................................................................... 7

9.1 Determination of ester content ................................................................................................................. 7

9.2 Determination of linolenic acid methyl ester ..................................................................................... 10

9.3 Expression of results ................................................................................................................................... 10

10 Precision .......................................................................................................................................................... 10

10.1 General.............................................................................................................................................................. 10

10.2 Repeatability .................................................................................................................................................. 10

10.3 Reproducibility .............................................................................................................................................. 11

11 Test report ....................................................................................................................................................... 11

Annex A (informative) Chromatograms of FAME samples - Determination of ester content

and linolenic acid methyl ester content – Summary of the analytical conditions ................. 12

Annex B (informative) Results of an interlaboratory trial ......................................................................... 16

Annex C (informative) Calculation of the pattern of fatty acid methyl esters...................................... 18

Bibliography ................................................................................................................................................................. 19

---------------------- Page: 4 ----------------------
SIST EN 14103:2020
EN 14103:2020 (E)
European foreword

This document (EN 14103:2020) has been prepared by Technical Committee CEN/TC 307 “Oilseeds,

vegetable and animal fats and oils and their by-products — Methods of sampling and analysis”, the

secretariat of which is held by AFNOR.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by July 2020, and conflicting national standards shall be

withdrawn at the latest by July 2020.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN 14103:2011.

In comparison with the previous edition, the following technical modifications have been made:

a) note on natural nonadecanoic acid methyl ester added in the scope;

b) new procedure to check nonadecanoic acid methyl ester purity, with new GC conditions, and

reduction of the minimum GC purity (99,5 to 99,0 % (m/m));

c) calculation of results revised by incorporation of theoretical flame ionization detector correction

factor (TCF), this gives a better accuracy of the calculated contents in case of presence of methyl

esters with short chains;
d) new inter-laboratories study (ILS) conducted and precision adopted;
e) new sample chromatograms recorded and added;

f) calculation of the pattern of fatty acid methyl esters incorporated as informative Annex C;

g) modification of the way of integration in 8.4 by taking all the peaks into consideration whereas in

the previous edition all the peaks identified as fatty acid methyl esters were taken into

consideration;

h) increase of the FAME sample test portion in 8.3 to 250 mg whereas in the previous edition the

sample test portion was 100 mg;
i) document revised editorially.

According to the CEN-CENELEC Internal Regulations, the national standards organisations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
---------------------- Page: 5 ----------------------
SIST EN 14103:2020
EN 14103:2020 (E)
1 Scope

The purpose of this document is to describe a procedure for the determination of the ester content in

fatty acid methyl esters (FAME) intended for incorporation into diesel oil. It also allows determining the

linolenic acid methyl ester content. It allows verifying that the ester content of FAME is greater

than 90 % (m/m) and that the linolenic acid methyl ester content is between 1 % (m/m)

and 15 % (m/m).

The precision was established using FAMEs with an ester content of 95 % (m/m) and 100 % (m/m)

only, thus covering the range of the limit value. The method is also suitable outside of this range;

however, precision for lower concentrations is subject to further work.

This method is suitable for FAME which contains methyl esters between C6 and C24.

NOTE 1 For the purposes of this document, the term “% (m/m)” is used to represent the mass fractions.

This method was elaborated for FAME samples from usual raw material. For FAME sample from

unidentified raw material, a solution of the test sample is prepared without any internal standard

addition, in order to verify the absence of natural nonadecanoic acid methyl ester or other unknown

substances co-eluting with the IS.

NOTE 2 The calculation method of the pattern of fatty acid methyl esters is given in Annex C.

WARNING — The use of this method may involve hazardous equipment, materials and operations. This

method does not purport to address to all of the safety problems associated with its use, but it is the

responsibility of the user to search and establish appropriate safety and health practices and determine

the applicability of regulatory limitations prior to use.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle

Determination of the mass percentage of total methyl esters of fatty acids and the mass percentage of

linolenic acid methyl ester present in the sample, by gas chromatography according to a procedure

using internal calibration (nonadecanoic acid methyl ester).
---------------------- Page: 6 ----------------------
SIST EN 14103:2020
EN 14103:2020 (E)
5 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.

5.1 Toluene, analytical grade, no impurities of toluene eluting after methyl ester C6:0.

5.2 Nonadecanoic acid methyl ester (FAME C19:0), GC purity, min. 99,0 % (m/m).

GC Purity of nonadecanoic acid methyl ester shall be checked for every new lot according to the

procedure described in 8.2.

Standard shall be kept at room temperature in a dry storage (e.g. desiccator) in order to limit its water

absorption. Its water content shall be below 0,2 % (m/m) and verified by Karl Fischer determination

when a new lot of standard is opened.
If the purity is lower than 99,0 % (m/m) do not use it for this determination.

5.3 Carrier gas, hydrogen or helium, 99,999 5 % pure or better, gas chromatography quality, dried,

oxygen removed by suitable filters (<0,1 mg/kg), free from organic impurities.

5.4 Auxiliary gases, hydrogen and air, gas chromatography quality, free from organic impurities.

6 Apparatus
Usual laboratory apparatus and, in particular, the following.

6.1 Gas chromatograph, equipped with a variable split flow injector or equivalent device, a

temperature programmable oven and a flame ionization detector.

6.2 Capillary column, coated with polyethylene glycol (Carbowax 20M) stationary phase, the

following characteristics have been found suitable: length: 30 m, internal diameter: 0,25 mm, film

thickness: 0,25 μm.

Stationary phase other than polyethylene glycol should be tested first before being selected as co-

elution between the internal standard (FAME C19:0) and other fatty acid methyl esters may exist.

NOTE Indeed, there is a co-elution between FAME C19:0 and linoleic acid methyl ester (FAME C18:2) when

using a column with a stationary phase such as 70 % cyanopropyl-polysilphenylene-siloxane (BPX70).

6.3 Glass mono-use tubes, equipped with plastic mono-use stopper, 10 ml capacity.

6.4 Pipette, 10 ml capacity.
6.5 Analytical balance, accuracy ± 0,1 mg.
7 Sampling

Sampling is not part of the method specified in this European Standard. A recommended sampling

method is given in EN ISO 5555 [1].
8 Procedure
8.1 Operating conditions

The chromatographic analysis conditions will be chosen taking into account the characteristics of the

column being used and the type of carrier gas (hydrogen or helium).
---------------------- Page: 7 ----------------------
SIST EN 14103:2020
EN 14103:2020 (E)
By way of indication, an example of analysis conditions is described below:

• column temperature: 60 °C hold for 2 min, programmed at 10 °C/min up to 200 °C, programmed

at 5 °C/min up to 240 °C, final temperature hold for 7 min;
• injector temperature and detector temperature: 250 °C;

• carrier gas flow rate 1-2 ml/min, a minimum flow rate of 1 ml/min shall be warranted when

operating at the maximum temperature;
• injected volume: 1 μl;
• carrier gas (hydrogen) pressure: 70 kPa;
• split flow: 100 ml/min.
8.2 Internal standard GC purity determination

In order to verify the absence of heavy impurities in the IS, the GC conditions were chosen according to

EN 14105.

Prepare a solution of nonadecanoic acid methyl ester in toluene approx. at 1 mg/ml. Analyse 1 μl of this

solution by gas chromatography on a capillary column of 15 m length and capable of being programmed

up to 400 °C (“high temperature” type) with thin film thickness, with an on-column injector or

equivalent device and flame ionization detection, according to the conditions described below. Analyse

using the same conditions 1 µl of toluene to verify that the impurities do not come from the solvent.

Calculate the purity P of the nonadecanoic acid methyl ester taking into account all the peaks eluted in

the chromatogram, excluding the solvent peak.

The purity of nonadecanoic acid methyl ester should be taken into consideration for the calculation of

the ester content (see 9.1) and the linolenic acid methyl ester content (see 9.2)..

By way of indication, an example of analysis conditions is described below:

• capillary column, capable of being programmed up to 400 °C (“high temperature” type) for which

the following characteristics are advised: 100 % dimethylpolysiloxane or 95 % dimethyl -

5 % diphenyl-polysiloxane stationary phase; length 15 m; internal diameter 0,32 mm; film

thickness 0,1 µm;

• column temperature: 50 °C hold for 1 min, programmed at 15 °C/min up to 180 °C, programmed

at 7 °C/min up to 230 °C, programmed at 10 °C/min up to 370 °C, final temperature hold

for 15 min;
• detector temperature: 380 °C;
• carrier gas pressure (hydrogen): 80 kPa;
• volume injected: 1 µl.
8.3 FAME sample preparation and analysis
Standard and FAME samples should be let at ambient temperature, in their cont
...

SLOVENSKI STANDARD
SIST EN 14103:2020
01-marec-2020
Nadomešča:
SIST EN 14103:2011

Derivati maščob in olj - Metilni estri maščobnih kislin (FAME) - Določevanje estra

in metilnega estra linolenske kisline

Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and

linolenic acid methyl ester contents

Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester

(FAME) - Bestimmung des Ester-Gehaltes und des Gehaltes an Linolensäure-
Methylester
Produits dérivés des corps gras - Esters méthyliques d'acides gras (EMAG) -

Détermination de la teneur en ester et en ester méthylique de l'acide linolénique

Ta slovenski standard je istoveten z: EN 14103:2020
ICS:
67.200.10 Rastlinske in živalske Animal and vegetable fats
maščobe in olja and oils
SIST EN 14103:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN 14103:2020
---------------------- Page: 2 ----------------------
SIST EN 14103:2020
EN 14103
EUROPEAN STANDARD
NORME EUROPÉENNE
January 2020
EUROPÄISCHE NORM
ICS 67.200.10 Supersedes EN 14103:2011
English Version
Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) -
Determination of ester and linolenic acid methyl ester
contents

Produits dérivés des corps gras - Esters méthyliques Erzeugnisse aus pflanzlichen und tierischen Fetten und

d'acides gras (EMAG) - Détermination de la teneur en Ölen - Fettsäure-Methylester (FAME) - Bestimmung

ester et en ester méthylique de l'acide linolénique des Ester-Gehaltes und des Gehaltes an Linolensäure-

Methylester
This European Standard was approved by CEN on 18 November 2019.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14103:2020 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 14103:2020
EN 14103:2020 (E)
Contents Page

European foreword ...................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 4

5 Reagents ............................................................................................................................................................. 5

6 Apparatus .......................................................................................................................................................... 5

7 Sampling ............................................................................................................................................................. 5

8 Procedure .......................................................................................................................................................... 5

8.1 Operating conditions ..................................................................................................................................... 5

8.2 Internal standard GC purity determination .......................................................................................... 6

8.3 FAME sample preparation and analysis ................................................................................................. 6

8.4 Identification .................................................................................................................................................... 7

9 Calculation ......................................................................................................................................................... 7

9.1 Determination of ester content ................................................................................................................. 7

9.2 Determination of linolenic acid methyl ester ..................................................................................... 10

9.3 Expression of results ................................................................................................................................... 10

10 Precision .......................................................................................................................................................... 10

10.1 General.............................................................................................................................................................. 10

10.2 Repeatability .................................................................................................................................................. 10

10.3 Reproducibility .............................................................................................................................................. 11

11 Test report ....................................................................................................................................................... 11

Annex A (informative) Chromatograms of FAME samples - Determination of ester content

and linolenic acid methyl ester content – Summary of the analytical conditions ................. 12

Annex B (informative) Results of an interlaboratory trial ......................................................................... 16

Annex C (informative) Calculation of the pattern of fatty acid methyl esters...................................... 18

Bibliography ................................................................................................................................................................. 19

---------------------- Page: 4 ----------------------
SIST EN 14103:2020
EN 14103:2020 (E)
European foreword

This document (EN 14103:2020) has been prepared by Technical Committee CEN/TC 307 “Oilseeds,

vegetable and animal fats and oils and their by-products — Methods of sampling and analysis”, the

secretariat of which is held by AFNOR.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by July 2020, and conflicting national standards shall be

withdrawn at the latest by July 2020.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN 14103:2011.

In comparison with the previous edition, the following technical modifications have been made:

a) note on natural nonadecanoic acid methyl ester added in the scope;

b) new procedure to check nonadecanoic acid methyl ester purity, with new GC conditions, and

reduction of the minimum GC purity (99,5 to 99,0 % (m/m));

c) calculation of results revised by incorporation of theoretical flame ionization detector correction

factor (TCF), this gives a better accuracy of the calculated contents in case of presence of methyl

esters with short chains;
d) new inter-laboratories study (ILS) conducted and precision adopted;
e) new sample chromatograms recorded and added;

f) calculation of the pattern of fatty acid methyl esters incorporated as informative Annex C;

g) modification of the way of integration in 8.4 by taking all the peaks into consideration whereas in

the previous edition all the peaks identified as fatty acid methyl esters were taken into

consideration;

h) increase of the FAME sample test portion in 8.3 to 250 mg whereas in the previous edition the

sample test portion was 100 mg;
i) document revised editorially.

According to the CEN-CENELEC Internal Regulations, the national standards organisations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
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SIST EN 14103:2020
EN 14103:2020 (E)
1 Scope

The purpose of this document is to describe a procedure for the determination of the ester content in

fatty acid methyl esters (FAME) intended for incorporation into diesel oil. It also allows determining the

linolenic acid methyl ester content. It allows verifying that the ester content of FAME is greater

than 90 % (m/m) and that the linolenic acid methyl ester content is between 1 % (m/m)

and 15 % (m/m).

The precision was established using FAMEs with an ester content of 95 % (m/m) and 100 % (m/m)

only, thus covering the range of the limit value. The method is also suitable outside of this range;

however, precision for lower concentrations is subject to further work.

This method is suitable for FAME which contains methyl esters between C6 and C24.

NOTE 1 For the purposes of this document, the term “% (m/m)” is used to represent the mass fractions.

This method was elaborated for FAME samples from usual raw material. For FAME sample from

unidentified raw material, a solution of the test sample is prepared without any internal standard

addition, in order to verify the absence of natural nonadecanoic acid methyl ester or other unknown

substances co-eluting with the IS.

NOTE 2 The calculation method of the pattern of fatty acid methyl esters is given in Annex C.

WARNING — The use of this method may involve hazardous equipment, materials and operations. This

method does not purport to address to all of the safety problems associated with its use, but it is the

responsibility of the user to search and establish appropriate safety and health practices and determine

the applicability of regulatory limitations prior to use.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle

Determination of the mass percentage of total methyl esters of fatty acids and the mass percentage of

linolenic acid methyl ester present in the sample, by gas chromatography according to a procedure

using internal calibration (nonadecanoic acid methyl ester).
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SIST EN 14103:2020
EN 14103:2020 (E)
5 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.

5.1 Toluene, analytical grade, no impurities of toluene eluting after methyl ester C6:0.

5.2 Nonadecanoic acid methyl ester (FAME C19:0), GC purity, min. 99,0 % (m/m).

GC Purity of nonadecanoic acid methyl ester shall be checked for every new lot according to the

procedure described in 8.2.

Standard shall be kept at room temperature in a dry storage (e.g. desiccator) in order to limit its water

absorption. Its water content shall be below 0,2 % (m/m) and verified by Karl Fischer determination

when a new lot of standard is opened.
If the purity is lower than 99,0 % (m/m) do not use it for this determination.

5.3 Carrier gas, hydrogen or helium, 99,999 5 % pure or better, gas chromatography quality, dried,

oxygen removed by suitable filters (<0,1 mg/kg), free from organic impurities.

5.4 Auxiliary gases, hydrogen and air, gas chromatography quality, free from organic impurities.

6 Apparatus
Usual laboratory apparatus and, in particular, the following.

6.1 Gas chromatograph, equipped with a variable split flow injector or equivalent device, a

temperature programmable oven and a flame ionization detector.

6.2 Capillary column, coated with polyethylene glycol (Carbowax 20M) stationary phase, the

following characteristics have been found suitable: length: 30 m, internal diameter: 0,25 mm, film

thickness: 0,25 μm.

Stationary phase other than polyethylene glycol should be tested first before being selected as co-

elution between the internal standard (FAME C19:0) and other fatty acid methyl esters may exist.

NOTE Indeed, there is a co-elution between FAME C19:0 and linoleic acid methyl ester (FAME C18:2) when

using a column with a stationary phase such as 70 % cyanopropyl-polysilphenylene-siloxane (BPX70).

6.3 Glass mono-use tubes, equipped with plastic mono-use stopper, 10 ml capacity.

6.4 Pipette, 10 ml capacity.
6.5 Analytical balance, accuracy ± 0,1 mg.
7 Sampling

Sampling is not part of the method specified in this European Standard. A recommended sampling

method is given in EN ISO 5555 [1].
8 Procedure
8.1 Operating conditions

The chromatographic analysis conditions will be chosen taking into account the characteristics of the

column being used and the type of carrier gas (hydrogen or helium).
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SIST EN 14103:2020
EN 14103:2020 (E)
By way of indication, an example of analysis conditions is described below:

• column temperature: 60 °C hold for 2 min, programmed at 10 °C/min up to 200 °C, programmed

at 5 °C/min up to 240 °C, final temperature hold for 7 min;
• injector temperature and detector temperature: 250 °C;

• carrier gas flow rate 1-2 ml/min, a minimum flow rate of 1 ml/min shall be warranted when

operating at the maximum temperature;
• injected volume: 1 μl;
• carrier gas (hydrogen) pressure: 70 kPa;
• split flow: 100 ml/min.
8.2 Internal standard GC purity determination

In order to verify the absence of heavy impurities in the IS, the GC conditions were chosen according to

EN 14105.

Prepare a solution of nonadecanoic acid methyl ester in toluene approx. at 1 mg/ml. Analyse 1 μl of this

solution by gas chromatography on a capillary column of 15 m length and capable of being programmed

up to 400 °C (“high temperature” type) with thin film thickness, with an on-column injector or

equivalent device and flame ionization detection, according to the conditions described below. Analyse

using the same conditions 1 µl of toluene to verify that the impurities do not come from the solvent.

Calculate the purity P of the nonadecanoic acid methyl ester taking into account all the peaks eluted in

the chromatogram, excluding the solvent peak.

The purity of nonadecanoic acid methyl ester should be taken into consideration for the calculation of

the ester content (see 9.1) and the linolenic acid methyl ester content (see 9.2)..

By way of indication, an example of analysis conditions is described below:

• capillary column, capable of being programmed up to 400 °C (“high temperature” type) for which

the following characteristics are advised: 100 % dimethylpolysiloxane or 95 % dimethyl -

5 % diphenyl-polysiloxane stationary phase; length 15 m; internal diameter 0,32 mm; film

thickness 0,1 µm;

• column temperature: 50 °C hold for 1 min, programmed at 15 °C/min up to 180 °C, programmed

at 7 °C/min up to 230 °C, programmed at 10 °C/min up to 370 °C, final temperature hold

for 15 min;
• detector temperature: 380 °C;
• carrier gas pressure (hydrogen): 80 kPa;
• volume injected: 1 µl.
8.3 FAME sample preparation and analysis
Standard and FAME samples should be let at ambient temperature, in their cont
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