Automotive fuels - Fatty acid methyl ester (FAME) fuel and blends with diesel fuel - Determination of oxidation stability by accelerated oxidation method at 110 °C

This document specifies a test method for the determination of the oxidation stability of fuels for diesel engines at 110 °C, by means of measuring the induction period of the fuel up to 48 h. The method is applicable to fatty acid methyl esters (FAME) intended for the use as pure biofuel or as a blending component for diesel fuels, and to blends of FAME with diesel fuel containing 2 % (V/V) of FAME at minimum.
The precision of the test method has been developed for conventional diesel. This test method is applicable for paraffinic diesel fuels as specified in EN 15940, however, a separate precision statement for paraffinic diesel is not available.
NOTE 1   EN 14112 [1] describes a similar test method for the determination of the oxidation stability of pure fatty acid methyl esters (see the Introduction to this document). Additionally, EN 16568 [4] describes a similar test method for the determination of the oxidation stability of fuels for diesel engines at 120 °C, by means of measuring the induction period of the fuel up to 20 h. EN 16568 is applicable to blends of FAME with diesel fuel containing 2 % (V/V) of FAME at minimum. Other alternative test methods for the determination of the oxidation stability of distillate fuels are described in CEN/TR 17225 [5].
NOTE 2   For induction periods higher than 48 h the precision is not covered by the precision statement of this method. The limit values of the relevant fuel standards are well within the scope of this test method.
NOTE 3   The presence of cetane improver can reduce the oxidation stability determined by this test method. Limited studies with EHN (2-ethyl hexyl nitrate) indicated, however, that the stability is reduced to an extent which is within the reproducibility of the test method.
NOTE 4   For the purposes of this document, the term “% (V/V)” is used to represent the volume fraction (φ) of a material.

Kraftstoffe für Kraftfahrzeuge - Fettsäuremethylester (FAME) Kraftstoff und Mischungen mit Dieselkraftstoff - Bestimmung der Oxidationsstabilität mit beschleunigtem Oxidationstest bei 110 °C

Dieses Dokument legt ein Prüfverfahren zur Bestimmung der Oxidationsstabilität von Kraftstoffen für Dieselmotoren bei 110 °C mittels Messung der Induktionszeit des Kraftstoffs bis zu 48 h fest. Dieses Verfahren gilt für Fettsäuremethylester (FAME), die zur Verwendung als reine Biokraftstoffe oder als Blendkomponente für Dieselkraftstoffe vorgesehen sind, und für Mischungen von FAME mit Dieselkraftstoff, die mindestens 2 % (V/V) FAME enthalten.
Die Präzision des Prüfverfahrens wurde für konventionellen Dieselkraftstoff ermittelt. Dieses Prüfverfahren ist anwendbar auf paraffinische Dieselkraftstoffe, wie in EN 15940 festgelegt; eine gesonderte Angabe zur Präzision für paraffinischen Dieselkraftstoff ist jedoch nicht verfügbar.
ANMERKUNG 1   EN 14112 [1] beschreibt ein ähnliches Prüfverfahren zur Bestimmung der Oxidationsstabilität reiner Fettsäuremethylester (siehe Einleitung dieses Dokumentes). Darüber hinaus beschreibt EN 16568 [3] ein ähnliches Prüfverfahren zur Bestimmung der Oxidationsstabilität von Kraftstoffen für Dieselmotoren bei 120 °C mittels Messung der Induktionszeit des Kraftstoffs bis zu 20 h. Dieses Verfahren gilt für Mischungen von FAME mit Dieselkraftstoff, die mindestens 2 % (V/V) FAME enthalten. Weitere alternative Prüfverfahren zur Bestimmung der Oxidationsstabilität von Destillatkraftstoffen sind in CEN/TR 17225 [4] beschrieben.
ANMERKUNG 2   Für Induktionszeiten über 48 h wird die Präzision nicht durch die angegebene Präzision dieses Verfahrens abgedeckt. Die Grenzwerte der relevanten Kraftstoffnormen liegen innerhalb des Anwendungsbereiches dieses Verfahrens.
ANMERKUNG 3   Die Gegenwart von Zündwilligkeitsverbesserern kann die Oxidationsstabilität, die mithilfe dieses Verfahrens bestimmt wurde, verringern. Begrenzte Untersuchungen mit EHN (2 Ethylhexylnitrat) wiesen jedoch darauf hin, dass sich die Stabilität in einem Umfang verringert, der innerhalb der Vergleichbarkeit dieses Prüfverfahrens liegt.
ANMERKUNG 4   Für die Zwecke dieses Dokumentes wird zur Angabe des Volumenanteils einer Substanz (φ) der Ausdruck „% (V/V)“ verwendet.

Carburants pour automobiles - Esters méthyliques d'acides gras (EMAG) et mélanges avec du gazole - Détermination de la stabilité à l'oxydation par méthode d'oxydation accélérée à 110 °C

Le présent document spécifie une méthode d’essai pour déterminer la stabilité à l’oxydation des carburants pour les moteurs diesel à 110 °C, par la mesure de la période d’induction du carburant jusqu’à 48 h. Cette méthode est applicable aux esters méthyliques d’acides gras (EMAG), utilisés comme biocarburant pur ou comme une base de mélange pour les gazoles, et aux mélanges d’EMAG avec du gazole contenant au minimum 2 % (V/V) d’EMAG.
La fidélité de la méthode d’essai a été développée pour des gazoles conventionnels. Cette méthode d’essai est applicable aux gazoles paraffiniques conformes à l’EN 15940, cependant la fidélité pour les gazoles paraffiniques n’est pas disponible.
NOTE 1   L’EN 14112 [1] spécifie une méthode d’essai similaire pour déterminer la stabilité à l’oxydation des EMAG purs (voir l’Introduction du présent document). En outre, la norme EN 16568 [3] spécifie une méthode d'essai similaire pour la détermination de la stabilité à l'oxydation des carburants pour moteurs diesel à 120 °C, par la mesure de la période d'induction du carburant jusqu'à 20 h. Cette méthode est applicable aux mélanges d'EMAG avec du carburant diesel contenant au moins 2 % (V/V) d'EMAG. D'autres méthodes d'essai pour la détermination de la stabilité à l'oxydation des distillats sont décrites dans le rapport technique CEN/TR 17225 [4].
NOTE 2   Pour des périodes d’induction supérieures à 48 h, les valeurs de fidélité établies dans cette méthode ne s’appliquent pas. Les valeurs limites des normes de carburants concernées sont bien comprises dans le domaine d’application de cette méthode d’essai.
NOTE 3   La présence de pro-cétane peut réduire la stabilité à l’oxydation déterminée au moyen de cette méthode. Des études limitées avec du EHN (nitrate de 2-éthyl hexyle) ont montré, cependant, que la stabilité est réduite dans une proportion qui est inférieure à la reproductibilité de la méthode d’essai.
NOTE 4   Pour les besoins du présent document, l’expression « % (V/V) » est utilisée pour représenter la fraction volumique (φ) du produit.

Goriva za motorna vozila - Metilni estri maščobnih kislin (FAME) goriv in mešanice z dizelskim gorivom - Ugotavljanje oksidativne stabilnosti z metodo pospešene oksidacije

General Information

Status
Not Published
Publication Date
30-Apr-2025
Current Stage
4599 - Dispatch of FV draft to CMC - Finalization for Vote
Start Date
20-Nov-2024
Due Date
02-Dec-2024
Completion Date
20-Nov-2024

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SLOVENSKI STANDARD
01-april-2024
Goriva za motorna vozila - Metilni estri maščobnih kislin (FAME) goriv in mešanice
z dizelskim gorivom - Ugotavljanje oksidativne stabilnosti z metodo pospešene
oksidacije
Automotive fuels - Fatty acid methyl ester (FAME) fuel and blends with diesel fuel -
Determination of oxidation stability by accelerated oxidation method
Kraftstoffe für Kraftfahrzeuge - Kraftstoff Fettsäuremethylester (FAME) und Mischungen
mit Dieselkraftstoff - Bestimmung der Oxidationsstabilität (beschleunigtes
Oxidationsverfahren)
Carburants pour automobiles - Esters méthyliques d'acides gras (EMAG) et mélanges
avec du gazole - Détermination de la stabilité à l'oxydation par méthode d'oxydation
accélérée
Ta slovenski standard je istoveten z: prEN 15751
ICS:
75.160.20 Tekoča goriva Liquid fuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
EUROPEAN STANDARD
prEN 15751
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2024
ICS 75.160.40 Will supersede EN 15751:2014
English Version
Automotive fuels - Fatty acid methyl ester (FAME) fuel and
blends with diesel fuel - Determination of oxidation
stability by accelerated oxidation method at 110 °C
Carburants automotives - Esters méthyliques d'acides Kraftstoffe für Kraftfahrzeuge - Fettsäuremethylester
gras (EMAG) et mélanges avec gazole - Détermination (FAME) Kraftstoff und Mischungen mit Dieselkraftstoff
de la stabilité à l'oxydation par méthode d'oxydation - Bestimmung der Oxidationsstabilität mit
accélérée à 110 °C beschleunigtem Oxidationstest bei 110 °C
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 19.
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, 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, Türkiye 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
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15751:2024 E
worldwide for CEN national Members.

prEN 15751:2024 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 6
5 Chemicals . 6
6 Apparatus . 6
7 Sampling . 8
8 Preparation of measurement . 8
8.1 Preparation of test sample . 8
8.2 Preparation of apparatus . 9
8.2.1 Cleaning procedure . 9
8.2.2 Temperature correction . 9
9 Measurement . 10
10 Calculation and evaluation . 13
10.1 Automatic evaluation . 13
10.2 Manual evaluation . 14
11 Expression of results . 15
12 Precision . 15
12.1 General. 15
12.2 Repeatability, r . 15
12.3 Reproducibility, R . 15
13 Test report . 15
Bibliography . 17

prEN 15751:2024 (E)
European foreword
This document (prEN 15751:2024) has been prepared by Technical Committee CEN/TC 19 “Gaseous
and liquid fuels, lubricants and related products of petroleum, synthetic and biological origin”, the
secretariat of which is held by NEN.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 15751:2014.
This document has been improved by editorial changes to clarify the test procedure.

prEN 15751:2024 (E)
Introduction
This document is based on EN 14112 [1], which was specifically adapted for the determination of
oxidation stability of fatty acid methyl esters (FAME). This method had been developed under
CEN/TC 307 (Fats and oils). At the time of development the method was applicable for FAME fuel
according to EN 14214 [2], but questions remained on the accuracy towards blends of FAME and diesel
fuel.
The modifications to EN 14112 as given in this document, allow application of this test method for
oxidation stability for pure FAME and diesel/FAME blends at various levels.
The goal was to have one single test method for FAME fuel, diesel/FAME blends and pure diesel fuels.
Although the modifications cover FAME fuel and diesel/FAME blends, CEN/TC 307 decided that it was
better to retain EN 14112 for methyl esters and publish a separate standard for all automotive fuel and
heating oil applications, as the use of 'diesel and diesel blends' falls out the scope of CEN/TC 307.
EN 15751 was originally developed to describe the oxidation stability of blends consisting of
conventional diesel fuel and FAME. FAME blends with paraffinic diesel fuel were not included into the
fuel matrix used to acquire precision data.
While developing specification EN 15940 for paraffinic diesel fuel, three laboratories executed a small
test on neat paraffinic fuel and on 7 % (V/V) FAME blends based on products originating from both
Fischer-Tropsch synthesis and hydrotreatment processes. No indications were found that FAME blends
with paraffinic diesel fuel behave differently than blends consisting of conventional diesel fuel and
FAME.
The modifications required a new validation covering pure FAME, diesel/FAME blends and pure diesel
fuels which resulted in the fact that the method has a lower precision for pure petroleum-based diesel
fuels.
prEN 15751:2024 (E)
1 Scope
This document specifies a test method for the determination of the oxidation stability of fuels for diesel
engines at 110 °C, by means of measuring the induction period of the fuel up to 48 h. The method is
applicable to fatty acid methyl esters (FAME) intended for the use as pure biofuel or as a blending
component for diesel fuels, and to blends of FAME with diesel fuel containing 2 % (V/V) of FAME at
minimum.
The precision of the test method has been developed for conventional diesel. This test method is
applicable for paraffinic diesel fuels as specified in EN 15940, however a separate precision statement
for paraffinic diesel is not available.
NOTE 1 EN 14112 [1] describes a similar test method for the determination of the oxidation stability of pure
fatty acid methyl esters (see the Introduction to this document). Additionally, EN 16568 [3] describes a similar
test method for the determination of the oxidation stability of fuels for diesel engines at 120 °C, by means of
measuring the induction period of the fuel up to 20 h. This method is applicable to blends of FAME with diesel fuel
containing 2 % (V/V) of FAME at minimum. Other alternative test methods for the determination of the oxidation
stability of distillate fuels are described in CEN/TR 17225 [4].
NOTE 2 For induction periods higher than 48 h the precision is not covered by the precision statement of this
method. The limit values of the relevant fuel standards are well within the scope of this test method.
NOTE 3 The presence of cetane improver can reduce the oxidation stability determined by this test method.
Limited studies with EHN (2-ethyl hexyl nitrate) indicated, however, that the stability is reduced to an extent
which is within the reproducibility of the test method.
NOTE 4 For the purposes of this document, the term “% (V/V)” is used to represent the volume fraction (φ) of a
material.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170)
EN ISO 3171, Petroleum liquids — Automatic pipeline sampling (ISO 3171)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp/
— IEC Electropedia: available at https://www.electropedia.org/
3.1
induction period
time which passes between the moment when the measurement is started and the moment when the
formation of oxidation products begins to increase rapidly
prEN 15751:2024 (E)
3.2
oxidation stability
induction period determined according to the procedure specified in this European Standard, expressed
in hours
4 Principle
A stream of purified air is passed through the sample which has been heated to the target temperature
which is 110 °C in the usual application of the method. Volatile compounds are formed during the
oxidation process. They are passed together with the air into a flask containing demineralized or
distilled water and equipped with a conductivity electrode. The electrode is connected to a measuring
and recording device. It indicates the end of the induction period by rapid increase of the conductivity
due to the dissociation of volatile carboxylic acids produced during the oxidation process and absorbed
in the water. For more details on the background of the method, see CEN/TR 17225 [4].
5 Chemicals
5.1 Distilled or demineralized water according to EN ISO 3696 [7].
5.2 Alkaline laboratory glass cleaning solution.
5.3 Ternary solvent mixture 1: 1: 1 (by volume), consisting of methanol/toluene/acetone, each of
recognized analytical grade.
5.4 2-Propanol of recognized analytical grade.
5.5 Thermo-stable oil, e.g. silicon oil.
6 Apparatus
Usual laboratory equipment and glassware, together with the following:
6.1 Device for the determination of oxidation stability, comprising the following parts (see
Figure 1 and Figure 2).
6.1.1 Air filter, comprising a tube fitted with filter
...

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