SIST EN 14103:2011

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

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

Dieses Dokument beschreibt ein Prüfverfahren für die Bestimmung des Estergehaltes in Fettsäure-
Methylester (FAME), die als Blendkomponente für Dieselkraftstoff Verwendung finden. Darüber hinaus
ermöglicht das Verfahren auch, den Gehalt an Linolensäure-Methylester zu bestimmen.
Dieses Prüfverfahren ist für Methylester mit einer Kettenlänge von C6 bis C24 anwendbar.
WARNUNG — Die Anwendung dieses Verfahrens kann den Einsatz gefährlicher Stoffe, Arbeitsgänge
und Geräte mit sich bringen. Diese Norm gibt nicht vor, alle mit ihrer Anwendung verbundenen
Sicherheitsprobleme anzusprechen. Der Anwender dieser Norm ist dafür verantwortlich, vorher
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 - 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. Elle permet
également la détermination de la teneur en ester méthylique de l’acide linolénique.
Cette méthode est applicable aux EMAG dont les esters méthyliques sont compris entre C6 et C24.
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 - Metil estri maščobnih kislin (FAME) - Določevanje estra in metil estra linolenske kisline

Namen tega dokumenta je opisati postopek za določevanje estra v metilestrih maščobnih kislin (FAME), ki so namenjeni za vključitev v dizelska olja. Prav tako omogoča določevanje metilestra linolenske kisline. Ta metoda je primerna za FAME, ki vsebuje metilestre med C6 in C24.

General Information

• Status: Withdrawn
• Publication Date: 31-May-2011
• Withdrawal Date: 09-Feb-2020
• ICS: 67.200.10 - Animal and vegetable fats and oils
• Technical Committee: KŽP - Agricultural food products
• Current Stage: 9900 - Withdrawal (Adopted Project)
• Start Date: 10-Feb-2020
• Due Date: 04-Mar-2020
• Completion Date: 10-Feb-2020
• Ref Project: EN 14103:2011 - Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contents

Relations

• Replaced By: SIST EN 14103:2020 - Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contents
• Effective Date: 01-Mar-2020
• Replaces: SIST EN 14103:2003 - Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contents
• Effective Date: 01-Jul-2011
• Replaces: SIST EN 14103:2003 - Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contents
• Effective Date: 08-Jun-2022

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Ester-Gehaltes und des Gehaltes an Linolensäure-MethylesterFat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of ester and linolenic acid methyl ester contents67.200.10Animal and vegetable fats and oilsICS:Ta slovenski standard je istoveten z:EN 14103:2011SIST EN 14103:2011en,fr,de01-julij-2011SIST EN 14103:2011SLOVENSKI
STANDARDSIST EN 14103:20031DGRPHãþD



SIST EN 14103:2011



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 14103
April 2011 ICS 67.200.10 Supersedes EN 14103:2003English 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 d'acides gras (EMAG) - Détermination de la teneur en ester et en ester méthylique de l'acide linolénique
Erzeugnisse aus pflanzlichen und tierischen Fetten und Ölen - Fettsäure-Methylester (FAME) - Bestimmung des Ester-Gehaltes und des Gehaltes an Linolensäure-Methylester This European Standard was approved by CEN on 10 March 2011.
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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 14103:2011: ESIST EN 14103:2011



EN 14103:2011 (E) 2 Contents Page Foreword . 31Scope . 42Principle . 43Reagents . 44Apparatus . 45Sampling . 56Procedure . 57Expression of results . 68Precision . 79Test report . 8Bibliography . 13 SIST EN 14103:2011



EN 14103:2011 (E) 3 Foreword This document (EN 14103:2011) 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 October 2011, and conflicting national standards shall be withdrawn at the latest by October 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 14103:2003. The main modifications of the standard are intended: - to enlarge the scope of the method to FAME from animal fat, by changing the internal standard (FAME C19 instead of FAME C17); - to verify the purity of the internal standard as it was proven that some lots may have a purity not good enough; - to improve the precision data by modifying the preparation of the test portion. According to the CEN/CENELEC Internal Regulations, the national standards organizations 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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. SIST EN 14103:2011



EN 14103:2011 (E) 4 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 For the purposes of this European Standard, the terms “% (m/m)” and “%(v/v)” are used to represent respectively the mass and volume fractions. 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 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). 3 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. 3.1 Toluene, analytical grade. 3.2 Nonadecanoic acid methyl ester (FAME C19), purity, min. 99,5 % (m/m)1). NOTE Standard should be kept in a dry storage in order to limit its water absorption. Its water content should be verified by Karl-Fischer when a new lot of standard is open. 3.3 Carrier gas, hydrogen or helium. 3.4 Auxiliary gases:  air;  hydrogen.
4 Apparatus Usual laboratory apparatus and, in particular, the following.
1) Nonadecanoic FAME with acceptable quality is available from Fluka - Ref: 74208 (www.sigmaaldrich.com) or from Nu Chek Prep - Ref: N-19-M (www.nu-chekprep.com) or Dr. Ehrenstorfer GmbH – ref 15 622 360 (www.analytical-standards.com). This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of these products. SIST EN 14103:2011



EN 14103:2011 (E) 5 4.1 Gas chromatograph, equipped with a variable split flow injector or equivalent device, a temperature programmable oven and a flame ionization detector. 4.2 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. NOTE 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. 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. 4.3 Glass mono-use tubes equipped with plastic mono-use stopper, 10 ml capacity. 4.4 Pipette, 10 ml capacity. 4.5 Analytical balance, accuracy ± 0,1 mg. 5 Sampling Sampling is not part of the method specified in this European Standard. A recommended sampling method is given in EN ISO 5555 [1]. 6 Procedure 6.1 Operating conditions The chromatographic ana
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