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-Methylestern (FAME) fest, die als Blendkomponente für Dieselkraftstoff Verwendung finden. Darüber hinaus ermöglicht das Verfahren, den Gehalt an Linolensäure-Methylester zu bestimmen. Mit diesem Verfahren lässt sich sicherstellen, dass der Estergehalt in Fettsäure-Methylester größer als 90 % (m/m) ist und der Gehalt an Linolensäure-Methylester zwischen 1 % (m/m) und 15 % (m/m) ist.
Die Präzision wurde nur mit FAME mit einem Estergehalt von 95 % (m/m) und 100 % (m/m) ermittelt, wodurch der Bereich des Grenzwertes abgedeckt ist. Das Verfahren ist auch außerhalb dieses Bereichs geeignet, die Präzision für niedrigere Konzentrationen ist jedoch Gegenstand weiterführender Arbeiten.
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)“ verwendet.
Dieses Verfahren wurde für FAME-Proben aus gängigen Rohstoffen ausgearbeitet. Bei FAME-Proben aus einem nicht identifizierten Rohstoff wird eine Lösung der zu untersuchenden Probe ohne Zugabe eines internen Standards hergestellt, um die Abwesenheit natürlichen Methyl-Nonadecanoats oder anderer, unbekannter Substanzen, die zusammen mit dem IS eluieren, nachzuweisen.
ANMERKUNG 2 Das Verfahren zur Berechnung des Musters von Fettsäure-Methylestern 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
Overview
EN 14103:2020 (CEN) defines a gas‑chromatographic procedure for determining the ester content and linolenic acid methyl ester (C18:3) content in Fatty Acid Methyl Esters (FAME) intended for incorporation into diesel fuel. The method verifies that FAME ester content is greater than 90 % (m/m) and that linolenic acid methyl ester content lies between 1 % (m/m) and 15 % (m/m). It is applicable to FAME containing methyl esters in the carbon range C6–C24 and uses an internal standard (nonadecanoic acid methyl ester, C19:0) with gas chromatography and flame ionization detection (GC‑FID).
Key topics and requirements
- Scope: Quantitative determination of total methyl ester content and linolenic acid methyl ester in FAME for diesel blending. Precision established around ester contents of 95 % and 100 %.
- Analytical principle: Internal calibration by GC‑FID using nonadecanoic acid methyl ester (FAME C19:0) as internal standard.
- Internal standard purity: C19:0 GC purity must be checked each new lot (minimum 99.0 % (m/m)); water content monitored.
- Sample preparation: Example procedure includes weighing approximately 250 mg of homogenized FAME and 100 mg internal standard, diluting to 10 mL with toluene prior to GC analysis.
- Chromatography: Uses a capillary column with a polyethylene glycol (Carbowax) stationary phase (example: 30 m × 0.25 mm × 0.25 µm). Carrier gas can be hydrogen or helium. GC conditions (oven program, injector/detector temperatures, split ratio) are adjusted to resolve C6:0 through C24:1.
- Identification and integration: Integrate peaks from C6:0 up to nervonic acid methyl ester (C24:1), taking all peaks into account (including odd‑chain or branched FAME from ruminant fats or unknowns from used cooking oil).
- Safety note: Users must observe laboratory safety and regulatory requirements; hazardous materials and operations are involved.
- Reference: Sampling guidance is available (EN ISO 5555 recommended).
Applications and users
- Biodiesel producers performing quality control on FAME raw materials and finished blends.
- Fuel testing laboratories verifying compliance before diesel blending.
- Regulatory bodies and enforcement labs ensuring fuel specifications and safety limits for linolenic content.
- Refineries and formulators assessing feedstock suitability and blend stability.
- R&D groups analyzing FAME composition for process optimization and raw material selection.
Related standards
- EN 14103:2020 is part of CEN/TC 307’s methods for oils and fats analysis. For sampling and broader biodiesel standards, users should consult the relevant EN/ISO standards (EN ISO 5555 is cited for sampling guidance).
Keywords: EN 14103:2020, FAME, fatty acid methyl esters, ester content, linolenic acid methyl ester, GC‑FID, nonadecanoic acid methyl ester, biodiesel testing, diesel blending, C6–C24.
Frequently Asked Questions
EN 14103:2020 is a standard published by the European Committee for Standardization (CEN). Its full title is "Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contents". This standard covers: 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.
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.
EN 14103:2020 is classified under the following ICS (International Classification for Standards) categories: 67.200.10 - Animal and vegetable fats and oils. The ICS classification helps identify the subject area and facilitates finding related standards.
EN 14103:2020 has the following relationships with other standards: It is inter standard links to EN 14103:2011. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
You can purchase EN 14103:2020 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of CEN standards.
Standards Content (Sample)
SLOVENSKI STANDARD
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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.
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
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.
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).
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).
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
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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
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© 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.
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
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.
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).
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).
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
...
기사 제목: EN 14103:2020 - 지방 및 오일 유도체 - 지방산 메틸 에스터 (FAME) - 에스터 및 리놀렌산 메틸 에스터 함량의 결정 기사 내용: 이 문서의 목적은 디젤 오일에 투입될 지방산 메틸 에스터 (FAME)의 에스터 함량을 결정하는 절차를 설명하는 것입니다. 또한 리놀렌산 메틸 에스터 함량을 결정할 수 있습니다. 이 방법은 FAME의 에스터 함량이 90 % (m/m) 이상이고 리놀렌산 함량이 1 % (m/m)에서 15 % (m/m) 사이임을 확인하는 데 사용할 수 있습니다. 이 방법은 C6에서 C24까지의 메틸 에스터를 포함하는 FAME에 적합합니다. 참고 1: 이 문서에서 "% (m/m)" 및 "% (v/v)"라는 용어는 각각 질량 및 체적 분율을 나타내기 위해 사용됩니다. 참고 2: 이 방법은 일반적인 원료에서 얻은 FAME 샘플에 대해 개발되었습니다. 식별되지 않은 원료에서 얻은 FAME 샘플의 경우 내부 표준 무첨가로 시험 샘플의 용액을 준비하여 천연 비니데카노산 메틸 에스터의 부재를 확인해야 합니다. 참고 3: 지방산 메틸 에스터의 분포는 부록 C에 제시되어 있습니다. 경고 - 이 방법의 사용은 위험한 장비, 재료 및 작업을 수반할 수 있습니다. 이 방법은 사용과 관련된 모든 안전 문제를 다루지는 않지만 사용자는 적절한 안전 및 보건 절차를 탐색하고 수립하고 사용 전에 규정 제한의 적용 가능성을 결정하는 것이 사용자의 책임입니다.
The article discusses the EN 14103:2020 standard, which outlines a procedure for determining the ester content in fatty acid methyl esters (FAME) used in diesel oil. It also allows for the determination of the linolenic acid methyl ester content. The standard ensures that the ester content of FAME is greater than 90% and the linolenic acid content is between 1% and 15%. This method is suitable for FAME containing methyl esters between C6 and C24. The article provides notes on the use of mass and volume fractions, testing samples from unidentified raw materials, and the distribution of fatty acid methyl esters. It also warns users about the potential hazards involved in using this method and emphasizes the need to establish appropriate safety practices and determine regulatory limitations.
기사 제목: EN 14103:2020 - 지방 및 오일 유도체 - 지방산 메틸 에스터 (FAME) - 에스터 및 리놀레닉 산 메틸 에스터 함량의 결정 기사 내용: 이 문서의 목적은 디젤 오일에 포함되는 지방산 메틸 에스터 (FAME)의 에스터 함량을 결정하기 위한 절차를 설명하는 것이다. 또한 리놀레닉 산 메틸 에스터 함량을 결정할 수 있다. 이 방법은 FAME의 에스터 함량이 90% (m/m) 이상이고 리놀레닉 산 함량이 1% (m/m)에서 15% (m/m) 사이임을 확인할 수 있게 해준다. 이 방법은 C6부터 C24까지의 메틸 에스터를 포함하는 FAME에 적합하다. 참고 1 - 이 문서에서 "% (m/m)"와 "% (v/v)"라는 용어는 각각 질량과 부피 분수를 나타내기 위해 사용된다. 참고 2 - 이 방법은 평범한 원료에서 얻은 FAME 샘플에 대해 개발되었다. 모르는 원료에서 얻은 FAME 샘플의 경우, 자연적인 논아데카노산 메틸 에스터의 부재를 확인하기 위해 내부 표준물질 첨가 없이 시험 샘플의 용액을 준비해야 한다. 참고 3 - 지방산 메틸 에스터의 분포는 부록 C에 나와 있다. 경고 - 이 방법의 사용은 위험한 장비, 재료 및 작업을 수반할 수 있다. 이 방법은 사용과 관련된 모든 안전 문제를 해결해 주지는 않지만, 사용자는 적절한 안전 및 보건 관행을 찾고 확립하고 사용 전에 규정적인 제한 사항의 적용 가능성을 결정하는 것이 사용자의 책임이다.
記事のタイトル: EN 14103:2020 - 脂肪および油の誘導体 - 脂肪酸メチルエステル（FAME） - エステルおよびリノレン酸メチルエステル含有量の測定 記事の内容: この文書の目的は、ディーゼルオイルに組み込むための脂肪酸メチルエステル（FAME）のエステル含有量を測定する手順を説明することです。また、リノレン酸メチルエステル含有量も測定できます。この方法は、FAMEのエステル含有量が90 %（m/m）以上であり、リノレン酸含有量が1 %（m/m）から15 %（m/m）の間であることを確認するのに使用できます。 この方法は、C6からC24までのメチルエステルを含むFAMEに適しています。 注1: この文書では、"%（m/m）"および"%（v/v）"という用語は、それぞれ質量および体積の割合を表すために使用されます。 注2: この方法は、通常の原料から得られるFAMEサンプルに対して作成されました。特定の原料から得られるFAMEサンプルの場合、内部標準物質の添加は行わず、テストサンプルの溶液を準備して自然なノナデカン酸メチルエステルの欠如を確認する必要があります。 注3: 脂肪酸メチルエステルの分布は付属書Cに記載されています。 警告 - この方法の使用には、危険な装置、材料、および操作が関連している場合があります。この方法はその使用に関連するすべての安全上の問題に対処するものではありませんが、使用者は適切な安全および健康の手順を調査・確立し、使用前に規制の制限の適用可能性を判断する責任があります。
記事のタイトル：EN 14103：2020 - 脂肪とオイルの誘導体 - 脂肪酸メチルエステル（FAME）- エステルおよびリノレン酸メチルエステルの含有量の測定 記事内容：この文書の目的は、ディーゼル燃料に組み込まれる脂肪酸メチルエステル（FAME）のエステル含有量を測定する手順を説明することです。また、リノレン酸メチルエステルの含有量も測定できます。この方法により、FAMEのエステル含有量が90％以上（m / m）であり、リノレン酸含有量が1％（m / m）から15％（m / m）の間であることを確認することができます。 この方法は、C6からC24のメチルエステルを含むFAMEに適しています。 注意 1- この文書では、「％（m/m）」および「％（v/v）」の用語は、それぞれ質量および体積の割合を表すために使用されます。 注意 2- この方法は通常の原料から得られたFAMEサンプルに対して作成されました。特定の原料から得られたFAMEサンプルの場合、内部標準物質の添加を行わずにテストサンプルの溶液を調製し、自然のノナデカン酸メチルエステルの存在を確認する必要があります。 注意 3- 脂肪酸メチルエステルの分布については、付録Cに記載されています。 警告- この方法の使用には、危険な機器、材料、および操作が関与する場合があります。この方法は使用に関連するすべての安全上の問題を解決するものではありませんが、使用者は適切な安全および衛生の手順を確立し、使用前に規制上の制限の適用可能性を判断するための探索と確立の責任があります。
The article discusses EN 14103:2020, a document that describes a procedure for determining the ester content in fatty acid methyl esters (FAME) used in diesel oil. It also allows for the determination of the linolenic acid methyl ester content. The method is applicable to FAME that contains methyl esters ranging from C6 to C24. The document emphasizes the use of mass and volume fractions to represent percentages. Additionally, it provides a warning about potential hazards associated with using the method and advises users to establish appropriate safety practices and consider regulatory limitations.
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