SIST EN 14103:2020
(Main)Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contents
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
Relations
Buy Standard
Standards Content (Sample)
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.
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SIST EN 14103:2020
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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.
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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
2
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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.
3
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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).
4
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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).
5
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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
...
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
2
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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.
3
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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).
4
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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).
5
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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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oSIST prEN 14103:2018
01-november-2018
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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: prEN 14103
ICS:
67.200.10 5DVWOLQVNHLQåLYDOVNH Animal and vegetable fats
PDãþREHLQROMD and oils
oSIST prEN 14103:2018 en,fr,de
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---------------------- Page: 1 ----------------------
oSIST prEN 14103:2018
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oSIST prEN 14103:2018
DRAFT
EUROPEAN STANDARD
prEN 14103
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2018
ICS 67.200.10 Will supersede 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 draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 307.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 14103:2018 E
worldwide for CEN national Members.
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oSIST prEN 14103:2018
prEN 14103:2018 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus . 5
7 Sampling . 5
8 Procedure . 5
8.1 Operating conditions . 5
8.2 Internal standard purity determination . 6
8.3 FAME sample preparation and analysis . 6
8.4 Identification . 6
9 Expression of results . 7
9.1 Determination of ester content . 7
9.2 Determination of linolenic acid methyl ester . 9
9.3 Expression of results . 9
10 Precision . 9
10.1 Interlaboratory test . 9
10.2 Repeatability . 9
10.3 Reproducibility . 10
11 Test report . 10
Annex A (informative) Chromatograms of a FAME samples — Determination of ester
content — Summary of the analysis conditions . 11
Annex B (informative) Results of an interlaboratory trial . 15
Annex C (informative) Calculation of the pattern of fatty acid methyl esters. 17
Bibliography . 18
2
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prEN 14103:2018 (E)
European foreword
This document (prEN 14103:2018) 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 document is currently submitted to the CEN Enquiry.
This document will supersede 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) check for nonadecanoic acid methyl ester purity added;
c) GC conditions for internal standard determination added;
d) calculation of results revised by incorporation of theoretical flame ionization detector correction
factor (TCF);
e) new ILS conducted and precision adopted;
f) new sample chromatograms recorded and added;
g) calculation of the pattern of fatty acid methyl esters incorporated as informative Annex C;
h) document revised editorially.
3
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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 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 is 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.
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 percentage of total methyl esters of fatty acids and the percentage of linolenic acid
methyl ester present in the sample, by gas chromatography according to a procedure using internal
calibration (nonadecanoic acid methyl ester).
5 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.
5.1 Toluene, analytical grade.
5.2 Nonadecanoic acid methyl ester (FAME C19), GC purity, min. 99,0 % (m/m).
Purity of nonadecanoic acid methyl ester shall be checked for every new lot according to the procedure
described in 6.2.
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 verified by Karl-Fischer when a new lot of standard is open.
4
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prEN 14103:2018 (E)
5.3 Carrier gas, hydrogen or helium.
5.4 Auxiliary gases:
• air;
• hydrogen.
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) and other fatty acid methyl esters may exist.
NOTE Indeed, there is a co-elution between FAME C19 and linoleic acid methyl ester (FAME C18:2) when
using a column with a stationary phase such as 70 % cyanopropyl-polysilphenyl-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).
By way of indication, an example of analysis conditions is described below:
-1
• column temperature: 60 °C hold for 2 min, programmed at 10 °C.min up to 200 °C, programmed
-1
at 5 °C.min up to 240 °C, final temperature hold for 7 min;
• injector temperature and detector temperature: 250 °C;
-1 -1
• 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;
• hydrogen pressure = 70 KPa;
-1
• split flow = 100 ml.min .
5
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prEN 14103:2018 (E)
8.2 Internal standard purity determination
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 short capillary column 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 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 FAME content (see 9.1).
GC conditions for internal standard determination:
• 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
Accurately weigh approximately 250 mg (accuracy ± 0,1 mg) of homogenized sample in a 10 ml tube
(6.3), and approximately 100 mg (accuracy ± 0,1 mg) of nonadecanoic acid methyl ester (5.2), and
dilute with 10 ml of toluene (5.1).
Standard and samples should be let at ambient temperature, in their container closed, at least 3 h prior
being weighed, in order to limit the water absorption during weighting.
For FAME sample
...
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