DIN EN 15751-2014 Automotive fuels - Fatty acid methyl ester (FAME) fuel and blends with diesel fuel - Determination of oxidation stability by accelerated oxidation method German v.pdf

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1、June 2014 Translation by DIN-Sprachendienst.English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 7

2、5.160.20!%2cEnglish version EN 15751:2014,English translation of DIN EN 15751:2014-06Kraftstoffe fr Kraftfahrzeuge Kraftstoff Fettsuremethylester (FAME) und Mischungen mit Dieselkraftstoff Bestimmung der Oxidationsstabilitt (beschleunigtes Oxidationsverfahren);Englische Fassung EN 15751:2014,Englisc

3、he bersetzung von DIN EN 15751:2014-06Carburants pour automobiles Esters mthyliques dacides gras (EMAG) et mlanges avec du gazole Dtermination de la stabilit loxydation par mthode doxydation acclre;Version anglaise EN 15751:2014,Traduction anglaise de DIN EN 15751:2014-06SupersedesDIN EN 15751:2009-

4、10www.beuth.deDocument comprises 19 pagesIn case of doubt, the German-language original shall be considered authoritative.05.14 DIN EN 15751:2014-06 2 A comma is used as the decimal marker. National foreword This document (EN 15751:2014) has been prepared by Technical Committee CEN/TC 19 “Gaseous an

5、d liquid fuels, lubricants and related products of petroleum, synthetic and biological origin” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-06-32-01 UA

6、 Prfung von FAME. Symbols By way of derogation from the English reference version, the following symbols are used in the German version of this document: Reference version German version Denotation blockT BT die Temperatur des Heizblocks (the temperature of the heating block) sensorT FT die im Reakt

7、ionsgef gemessene Temperatur (the measured temperature in the reaction vessel) targetT SollT die vorgesehene Messtemperatur (the intended measurement temperature) Amendments This standard differs from DIN EN 15751:2009-10 as follows: a) the scope of the method has been limited to a maximum induction

8、 period of 48 h, reflecting the precision range of the method; b) a potential alteration of the induction period in the presence of cetane enhancers has been indicated; c) the results of a short applicability check on non-petroleum based (such as Fischer-Tropsch synthesis or hydrotreatment process o

9、riginated) diesel types of fuels (see Introduction) has been included; d) the standard has been editorially revised in order to clarify the test procedure. Previous editions DIN 51627-2: 2008-08 DIN EN 15751: 2009-10 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15751 March 2014 ICS 75.160.20

10、 Supersedes EN 15751:2009English Version Automotive fuels - Fatty acid methyl ester (FAME) fuel and blends with diesel fuel - Determination of oxidation stability by accelerated oxidation method Carburants pour automobiles - Esters mthyliques dacides gras (EMAG) et mlanges avec du gazole - Dterminat

11、ion de la stabilit loxydation par mthode doxydation acclre Kraftstoffe fr Kraftfahrzeuge - Kraftstoff Fettsuremethylester (FAME) und Mischungen mit Dieselkraftstoff - Bestimmung der Oxidationsstabilitt (beschleunigtes Oxidationsverfahren) This European Standard was approved by CEN on 20 December 201

12、3. 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 o

13、n 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-CENE

14、LEC 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, Ital

15、y, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Aven

16、ue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15751:2014 EEN 15751:2014 (E) 2 Contents Page Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Principle 5

17、 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 8 9 Measurement . 10 10 Calculation and evaluation 13 10.1 Automatic evaluation . 13 10.2 Manual evaluation . 14 11 Expression of results . 14 12 Prec

18、ision 14 12.1 General . 14 12.2 Repeatability, r 14 12.3 Reproducibility, R . 14 13 Test report . 15 Annex A (informative) Background of the method . 16 Bibliography . 17 DIN EN 15751:2014-06 EN 15751:2014 (E) 3 Foreword This document (EN 15751:2014) has been prepared by Technical Committee CEN/TC 1

19、9 “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 b

20、y September 2014 and conflicting national standards shall be withdrawn at the latest by September 2014. 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 su

21、ch patent rights. This document supersedes EN 15751:2009. Significant changes between this document and EN 15751:2009 are: a) the limitation of the scope of the method to a maximum induction period of 48 h, reflecting the precision range of the method, b) indication of a potential alteration of the

22、induction period in the presence of cetane enhancers, c) inclusion of the results of a short applicability check on non-petroleum based (such as Fischer-Tropsch synthesis or hydrotreatment process originated) diesel type of fuels (see Introduction), d) editorial changes in order to clarify the test

23、procedure. 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, Former Yugoslav Republic of Macedonia,

24、France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 15751:2014-06 EN 15751:2014 (E) 4 Introduction This document is based

25、 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 r

26、emained 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, di

27、esel/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

28、blends falls out the scope of CEN/TC 307. While developing the fuels specification for paraffinic diesel fuel, three labs executed a small test on neat fuel and on 7 % (V/V) FAME blend based on product originating from both Fischer-Tropsch synthesis and hydrotreatment process. No indications towards

29、 a different interaction with the methodology of this document were found, so it was concluded that the stability of these paraffinic diesel fuels can be determined with the test method described in this document. The stability of these products usually is that high that the results do not match the

30、 scope of this European Standard. 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. DIN EN 15751:2014-06 EN 15751:2014 (E) 5 1 Scope This European

31、Standard specifies a test method for the determination of the oxidation stability of fuels for diesel engines, 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 componen

32、t for diesel fuels, and to blends of FAME with diesel fuel containing 2 % (V/V) of FAME at minimum. NOTE 1 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). NOTE 2 For induction periods

33、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 st

34、udies 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 European Standard, the term “% (V/V)” is used to represent the volume fraction () of a material. 2 Normative r

35、eferences The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applie

36、s. 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. 3.1 induction period time which passes between the moment when

37、the measurement is started and the moment when the formation of oxidation products begins to increase rapidly 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

38、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 demineralised or distilled water, equipped with a conductivity

39、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

40、background of the method, see Annex A. DIN EN 15751:2014-06 EN 15751:2014 (E) 6 5 Reagents and materials Use only reagents of analytical grade and distilled or demineralised water 3. 5.1 Ternary solvent mixture, consisting of methanol/toluene/acetone 1:1:1 (by volume) 5.2 Alkaline laboratory glass c

41、leaning solution 5.3 2-Propanol 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 Figures 1 and 2). NOTE An instrument for determining the oxidation stability is commercially

42、 available under the trade name Rancimat, (model 743 or higher, from Metrohm AG, Herisau, Switzerland) or OSIInstrument (from Omnion Inc., Rockland, Massachusetts, USA)1). 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 t

43、he suction end of a pump. 6.1.2 Gas membrane pump, with an adjustable flow rate of (10 1,0) l/h. 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 exceed the depth of the oven by at least 130 mm,

44、in order to reduce evaporation losses to a minimum by condensing, volatile fuel components at the cold vessel walls outside the oven. 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 in

45、let and outlet tube. A few centimetres below the top, the vessel shall preferably have a slightly reduced inner diameter 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 capaci

46、ty, with a gas inlet tube extending to the bottom inside of the vessel. The cell shall have ventilation holes at the top. 6.1.5 Electrodes, for measuring conductivity within a range of 0 S/cm to 300 S/cm aligned with the dimensions of the measurement cell (6.1.4). 6.1.6 Measuring and recording appar

47、atus, comprising: a) an amplifier, and b) a recorder registering the signal of each of the electrodes (6.1.5). 1) These are examples of suitable equipment which are given for the convenience of users of this European Standard. They do not constitute an endorsement by CEN of these products. DIN EN 15

48、751:2014-06 EN 15751:2014 (E) 7 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. 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 u