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

This European Standard specifies a test method for determining the oxidation stability of diesel fuels and of fatty acid esters fuels (usually FAME and FAEE) intended for use as pure biofuel or as a blending component for diesel fuels. The use is primarily intended for automotive purposes.
This European Standard specifies a test method for determining the oxidation stability of fuels for diesel engines. The method is applicable to fatty acid methyl esters (FAME) intended for use as pure biofuel or as a blending component for diesel fuels, and to blends of FAME and petroleum-based diesel containing 2 volume percentage of FAME at minimum. NOTE EN 14112 [1] describes a similar test method for oxidation stability determination of pure fatty acid methyl esters (see the Introduction to this European Standard). EN ISO 12205 [3] describes a test method that is applicable to pure petroleum-based diesel.

Kraftstoffe für Kraftfahrzeuge - Kraftstoff Fettsäuremethylester (FAME) und Mischungen mit Dieselkraftstoff - Bestimmung der Oxidationsstabilität (beschleunigtes Oxidationsverfahren)

Diese Europäische Norm legt ein Prüfverfahren zur Bestimmung der Oxidationsstabilität von Kraftstoff für Dieselmotoren fest. Dieses Verfahren ist anwendbar auf Fettsäure¬methylester (FAME), welche zur Anwendung als reine Biokraftstoffe oder als Blendkomponente für Dieselkraftstoffe gedacht sind, und für Mischungen von FAME mit aus Erdöl hergestellten Dieselkraftstoff.
ANMERKUNG   EN 14112 [1] beschreibt ein ähnliches Prüfverfahren zur Bestimmung der Oxidationsstabilität von Fettsäuremethylester, welche nicht als Kraftstoff verwendet werden (siehe Einleitung zu dieser Europäischen Norm). EN 12205 [3] beschreibt ein Prüfverfahren welches auf reinen aus Erdöl hergestellten Diesel anwendbar ist.

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

Cette Norme européenne spécifie une méthode d’essai pour déterminer la stabilité à l’oxydation des
carburants pour les moteurs diesel. 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 et de gazole d'origine pétrolière contenant au minimum 2 %, en volume, d’EMAG.
NOTE L’EN 14112 [1] décrit une méthode d’essai similaire pour déterminer la stabilité à l’oxydation des EMAG, purs,
(voir l’Introduction à cette Norme européenne). L’EN ISO 12205 [3] décrit une méthode d’essai qui est applicable au
gazole purement d'origine pétrolière.

Goriva za motorna vozila - Metilni estri maščobne kisline (FAME) goriv in mešanice z dizelskim gorivom - Določevanje oksidativne stabilnosti z metodo s pospešeno oksidacijo

General Information

Status
Withdrawn
Public Enquiry End Date
09-Apr-2008
Publication Date
16-Aug-2009
Withdrawal Date
16-Apr-2014
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
17-Apr-2014
Due Date
10-May-2014
Completion Date
17-Apr-2014

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.RNVLGDFLMRKraftstoffe 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 gazole - Détermination de la stabilité à l'oxydation par méthode d'oxydation accéléréeAutomotive fuels - Fatty acid methyl ester (FAME) fuel and blends with diesel fuel - Determination of oxidation stability by accelerated oxidation method75.160.20Liquid fuelsICS:Ta slovenski standard je istoveten z:EN 15751:2009SIST EN 15751:2009en,fr,de01-september-2009SIST EN 15751:2009SLOVENSKI
STANDARD



SIST EN 15751:2009



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15751June 2009ICS 75.160.20 English VersionAutomotive fuels - Fatty acid methyl ester (FAME) fuel andblends with diesel fuel - Determination of oxidation stability byaccelerated oxidation methodCarburants pour automobiles - Esters méthyliques d'acidesgras (EMAG) et mélanges avec gazole - Détermination dela stabilité à l'oxydation par méthode d'oxydation accéléréeKraftstoffe für Kraftfahrzeuge - KraftstoffFettsäuremethylester (FAME) und Mischungen mitDieselkraftstoff - Bestimmung der Oxidationsstabilität(beschleunigtes Oxidationsverfahren)This European Standard was approved by CEN on 23 May 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, 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 STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre:
Avenue Marnix 17,
B-1000 Brussels© 2009 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15751:2009: ESIST EN 15751:2009



EN 15751:2009 (E) 2 Contents Page Foreword .3 Introduction .4 1 Scope .5 2 Normative references .5 3 Terms and definitions .5 4 Principle .5 5 Reagents and materials .6 6 Apparatus .6 7 Sampling .7 8 Preparation of measurement .8 8.1 Preparation of test sample .8 8.2 Preparation of apparatus .9 9 Procedure . 10 10 Calculation and evaluation . 11 10.1 Automatic evaluation . 11 10.2 Manual evaluation . 12 11 Expression of results . 12 12 Precision . 14 12.1 General . 14 12.2 Repeatability, r . 14 12.3 Reproducibility, R . 14 13 Test report . 14 Annex A (informative)
Background of the method . 15 Bibliography . 16
SIST EN 15751:2009



EN 15751:2009 (E) 3 Foreword This document (EN 15751:2009) 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 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 December 2009, and conflicting national standards shall be withdrawn at the latest by December 2009. 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. 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, 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 the United Kingdom. SIST EN 15751:2009



EN 15751:2009 (E) 4 Introduction This document is based on EN 14112:2003 [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. The modifications required a new validation covering pure FAME, diesel/FAME blends and pure diesel fuels, which resulted in the fact that the method is not suitable for pure petroleum-based diesel fuels. SIST EN 15751:2009



EN 15751:2009 (E) 5 1 Scope This European Standard specifies a test method for determining the oxidation stability of fuels for diesel engines. The method is applicable to fatty acid methyl esters (FAME) intended for use as pure biofuel or as a blending component for diesel fuels, and to blends of FAME and petroleum-based diesel containing 2 volume percentage of FAME at minimum. NOTE EN 14112 [1] describes a similar test method for oxidation stability determination of pure fatty acid methyl esters (see the Introduction to this European Standard). EN ISO 12205 [3] describes a test method that is applicable to pure petroleum-based diesel. 2 Normative references The following referenced documents are indispensable for the application 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 3170:2004) EN ISO 3171, Petroleum liquids – Automatic pipeline sampling (ISO 3171:1988) 3 Terms and definitions For the purposes of this European Standard, the following terms and definitions apply. 3.1 induction period time which passes between the moment when the measurement is started and the moment when the formation of oxidation products rapidly begins to increase 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 brought to a specified temperature. The vapours released during the oxidation process, together with the air, are passed into a flask containing water which has been demineralised or distilled and contains an electrode for measuring the conductivity. The electrode is connected to a measuring and recording device. It indicates the end of the induction period when the conductivity begins to increase rapidly. This accelerated increase is caused by 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 Annex A. SIST EN 15751:2009



EN 15751:2009 (E) 6 5 Reagents and materials Use only reagents of recognised analytical grade, and distilled or demineralised water [4]. 5.1 Ternary solvent mixture, consisting of methanol/toluene/acetone 1:1:1 (by volume) 5.2 Alkaline laboratory glass cleaning solution 5.3 2-Propanol 6 Apparatus Usual laboratory equipment and glassware, together with the following: 6.1 Appliance for the determination of oxidation stability, consisting of the following (see Figures 1 and 2 for diagrammatic representations): NOTE An apparatus for determining oxidation stability can be obtained commercially under the trade name Rancimat®, (model 743 or higher, from Metrohm AG, Herisau, Switzerland) or OSI® Instrument (from Omnion Inc., Rockland, Massachusetts, USA). These are examples of suitable equipment and are given for the convenience of users of this document. It does not constitute an endorsement by CEN of this equipment. 6.1.1 Air filter, comprising a tube fitted with filter paper at the ends and filled with a molecular sieve (6.6), connected to the suction end of a pump. 6.1.2 Gas diaphragm pump, with an adjustable flow rate of 10 l/h in combination with an apparatus to control the flow rate manually or automatically with a maximum deviation of ± 1,0 l/h from the set value. 6.1.3 Reaction vessels of borosilicate glass, provided with a sealing cap. The length of the reaction vessel depends on the measuring equipment and shall stick out of the oven at least for 130 mm. Condensing volatile fuel components at the cold vessel walls outside the oven reduces evaporation losses to a minimum. EXAMPLE Total length of the test tube for the Metrohm Rancimat 743 L = 250 mm, for the Omnion OSI Instrument L = 300 mm. The sealing cap shall be fitted with a gas inlet and outlet tube. The cylindrical part of the vessel shall preferably be narrower a few centimetres below the top in order to break any emerging foam. An artificial foam blocker (e.g. glass ring) may also be used for this purpose. 6.1.4 Closed measurement cells, of approximately 150 ml capacity, with a gas inlet tube extending to the bottom inside of the vessel. The cell shall be provided at the top with ventilation holes. 6.1.5 Electrodes, for measuring conductivity with a measuring range of 0 µS/cm to 300 µS/cm aligned with the dimensions of the measurement cell (6.1.4). 6.1.6 Measuring and recording apparatus, comprising of: a) an amplifier, and b) a recorder for registering the measuring signal of each of the electrodes (6.1.5). 6.1.7 Thyristor and contact thermometer graduated in 0,1 °C or Pt 100 element to measure the block temperature, with attachments for relay connection and an adjustable heating element; temperature scale 0 °C to 150 °C. SIST EN 15751:2009



EN 15751:2009 (E) 7 6.1.8 Heating block, made of cast aluminium, adjustable to a temperature up to (150 ± 0,1) °C. The block shall be provided with holes for the reaction vessels (6.1.3), and an aperture for the contact thermometer (6.1.7). Alternatively, a heating bath may be used, filled with oil suitable for temperatures up to 150 °C and adjustable to the nearest 0,1 °C. 6.2 Certified and calibrated thermometer or Pt100 element, with a temperature range up to 150 °C, graduated in 0,1 °C.
Key 1 Air filter (6.1.1) 5 Electrode (6.1.5) 2 Gas diaphragm pump with flow rate control (6.1.2) 6 Measuring and recording apparatus (6.1.6) 3 Reaction vessel (6.1.3) 7 Thyristor and contact thermometer (6.1.7) 4 Measurement cell (6.1.4) 8 Heating block (6.1.8) Figure 1 — Diagrammatic representation of the apparatus 6.3 Measuring pipettes and/or measuring cylinders
6.4 Oven, capable of being maintained up to (150 ± 3) °C. 6.5 Connecting hoses, flexible and made of inert material [polytetrafluoroethylene (PTFE) or silicone]. 6.6 Molecular sieve, with moisture indicato
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