DIN EN 16270-2015 Automotive fuels - Determination of high-boiling components including fatty acid methyl esters in petrol and ethanol (E85) automotive fuel - Gas chromatographic m.pdf

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1、August 2015 Translation by DIN-Sprachendienst.English price group 10No 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

2、 75.160.20!%E5“2342918www.din.deDDIN EN 16270Automotive fuels Determination of high-boiling components including fatty acid methylesters in petrol and ethanol (E85) automotive fuel Gas chromatographic method;English version EN 16270:2015,English translation of DIN EN 16270:2015-08Kraftstoffe fr Kraf

3、tfahrzeuge Bestimmung von hochsiedenden Komponenten inklusive Fettsure-Methylester inOttokraftstoff und Ethanol (E85)-Kraftstoff fr Fahrzeuge Gaschromatographisches Verfahren;Englische Fassung EN 16270:2015,Englische bersetzung von DIN EN 16270:2015-08Carburants pour automobiles Dtermination des com

4、poss haut point dbullition dont les esters mthyliques dacidesgras dans lessence et dans le carburant thanol pour automobiles (E85) Mthode par chromatographie en phase gazeuse;Version anglaise EN 16270:2015,Traduction anglaise de DIN EN 16270:2015-08SupersedesDIN EN 16270:2012-12www.beuth.deIn case o

5、f doubt, the German-language original shall be considered authoritative.Document comprises 17 pages 07.15 DIN EN 16270:2015-08 2 A comma is used as the decimal marker. National foreword This document (EN 16270:2015) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubric

6、ants and related products of petroleum, synthetic and biological origin” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-06-14 AA Chromatographisc

7、he Analyse of the Fachausschuss Minerall- und Brennstoffnormung (FAM). NOTE The scope of this document has been confined to the determination of fatty acid methyl esters consisting of C18 FAME compounds. Shorter chain FAME, in particular lauric types such as palm kernel and coconut methyl esters are

8、 not covered in this standard due to their low boiling point. Amendments This standard differs from DIN EN 16270:2012-12 as follows: a) the scope has been extended to include ethanol (E85) fuels; b) precision data have been updated; c) in Clause 3 “Terms and definitions”, “3.1 high boiling fraction”

9、 has been added; d) Clause 5 “Reagents and materials” now includes further information on solvents (5.5). Previous editions DIN EN 16270: 2012-12 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16270 June 2015 ICS 75.160.20 Supersedes EN 16270:2012English Version Automotive fuels - Determinatio

10、n of high-boiling components including fatty acid methyl esters in petrol and ethanol (E85) automotive fuel - Gas chromatographic method Carburants pour automobiles - Dtermination des composs haut point dbullition dont les esters mthyliques dacides gras dans lessence et dans le carburant thanol pour

11、 automobiles (E85) - Mthode par chromatographie en phase gazeuse Kraftstoffe fr Kraftfahrzeuge - Bestimmung von hochsiedenden Komponenten inklusive Fettsure-Methylester in Ottokraftstoff und Ethanol (E85)-Kraftstoff fr Fahrzeuge - Gaschromatographisches Verfahren This European Standard was approved

12、by CEN on 30 April 2015. 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 stand

13、ards 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 no

14、tified 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary,

15、Iceland, Ireland, Italy, 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 M

16、anagement Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16270:2015 EEN 16270:2015 (E) 2 Contents Page Foreword 3 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Princ

17、iple 7 5 Reagents and materials 7 6 Apparatus .8 7 Sampling .9 8 Preparation of the apparatus . 10 9 Calibration . 10 10 Procedure 10 11 Visual inspection of the chromatograms . 11 12 Calculation . 12 12.1 General . 12 12.2 Total high boiling fraction 12 12.3 FAME fraction 13 13 Expression of result

18、s . 13 14 Precision 13 14.1 General . 13 14.2 Repeatability 13 14.3 Reproducibility 13 15 Test report . 14 Bibliography . 15 DINEN 16270:2015-08EN 16270:2015(E)3 Foreword This document (EN 16270:2015) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and relate

19、d 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 2015, and conflicting national standard

20、s shall be withdrawn at the latest by December 2015. 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 16270

21、:2012. Its scope has been extended to ethanol (E85) automotive fuel, the precision data have been updated and further technical improvements have been included. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement t

22、his European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slova

23、kia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16270:2015-08 EN 16270:2015 (E) 4 1 Scope This European Standard specifies a determination method of high boiling components in petrol according to EN 228 1 and ethanol (E85) automotive fuels according to CEN/TS 15293 2

24、 by capillary gas chromatography using flame ionization detection. This method is applicable to high boiling material, such as fatty acid methyl ester (FAME) or diesel fuel, having a boiling point greater than or equal to 1-methyl-naphthalene. This European Standard is applicable to materials having

25、 a vapour pressure low enough to permit sampling at ambient temperature and covers a boiling range of at least 100 C. This method pays special attention to fatty acid methyl esters. In petrol the measurement range for the high boiling fraction is from about 0,7 % (m/m) to about 2,5 % (m/m). For the

26、FAME fraction the range is from about 0,2 % (m/m) to about 2 % (m/m). In ethanol (E85) automotive fuel the measurement range for the high boiling fraction is from about 0,2 % (m/m) to about 2,2 % (m/m), for the FAME fraction the range is from about 0,05 % (m/m) to about 1,5 % (m/m) NOTE 1 When calcu

27、lating the FAME fraction, this method only takes the C18 FAME compounds into account. NOTE 2 For the purposes of this European Standard, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass fraction and the volume fraction. WARNING The use of this European Standard may invol

28、ve hazardous materials, operations and equipment. This European Standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and to determine the applicability of re

29、gulatory limitations prior to use. 2 Normative references 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 refer

30、enced document (including any amendments) applies. EN 14214, Liquid petroleum products - Fatty acid methyl esters (FAME) for use in diesel engines and heating applications - Requirements and test methods EN ISO 3170, Petroleum liquids - Manual sampling (ISO 3170) EN ISO 3171, Petroleum liquids - Aut

31、omatic pipeline sampling (ISO 3171) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. NOTE Figure 1a, 1b and 2 give some visual explanation of the definitions on the basis of an exemplary chromatogram. 3.1 high boiling fraction total fraction of hi

32、gh boiling material starting from 1-methylnaphthalene until and including dotriacontane and therefore includes all FAME peaks that may be present in this area 3.2 start of high boiling fraction 1-methyl-naphthalene is the first peak to be included in the high boiling fraction DIN EN 16270:2015-08 EN

33、 16270:2015 (E) 5 3.3 end of high boiling fraction dotriacontane (n-C32) is the last peak to be included in the high boiling fraction Key 1 1-Methyl-naphthalene 4 Start of high boiling fraction 2 Total high boiling area 5 Baseline for high boiling fraction 3 End of high boiling fraction X time (min)

34、 Y FID signal Figure 1a Chromatogram explaining high boiling fraction DIN EN 16270:2015-08 EN 16270:2015 (E) 6 Key 1 C18 FAME peak area 2 Manual baseline for FAME fraction calculation X time (min) Y FID signal Figure 1b Chromatogram explaining FAME fraction Key 1 1-Methyl-naphthalene start of high b

35、oiling fraction 3 Dotriacontane end of high boiling fraction 2 C18-FAME X time (min) Y FID signal Figure 2 Example of a calibration mixture chromatogram DIN EN 16270:2015-08 EN 16270:2015 (E) 7 3.4 Fatty acid methyl esters fraction FAME fraction combined area of the C18:0, C18:1, C18:2 and C18:3-FAM

36、E peaks Note 1 to entry: The area is defined as shown in Figure 1b Note 2 to entry: This method only takes the C18 FAME compounds into account as other compounds such as C16:0 can only be present in very limited amounts. In addition, C16:0 co-elutes with an n-paraffin which affects the quantificatio

37、n. 3.5 total high boiling area for a calibration mixture Atcsum of the areas of 1-methylnaphthalene and dotriacontane Note 1 to entry: See Figure 2. 3.6 total FAME area for a calibration mixture Afccumulative area from the start of the FAME C18-fraction until the end of the FAME C18-fraction for a c

38、alibration mixture Note 1 to entry: See Figure 2. 3.7 total high boiling area for a sample Ascumulative area from the start of the high boiling fraction until the end of high boiling fraction for a sample Note 1 to entry: See Figure 1a. 3.8 total FAME fraction area for a sample Afcumulative area fro

39、m the start of the FAME C18-fraction until the end of the FAME C18-fraction for a sample Note 1 to entry: See Figure 1b. 4 Principle A test portion is introduced into a gas chromatographic column, which separates hydrocarbons in the order of increasing boiling point. The column temperature is raised

40、 at a linear reproducible rate and the area under the chromatogram is recorded throughout the analysis. The beginning and the end of the fractions are determined with a calibration mixture. 5 Reagents and materials Unless otherwise stated, only chemicals of recognized analytical quality shall be use

41、d. 5.1 Carrier gases, helium, nitrogen or hydrogen, of at least 99,999 % (V/V) purity, any oxygen present should be removed, e.g. by a chemical resin filter. WARNING Follow the safety instructions from the filter supplier. 5.2 Hydrogen, grade suitable for flame ionization detectors. DINEN 16270:2015

42、-08.EN 16270:2015 (E) 8 5.3 Compressed air, regulated for flame ionization detectors. 5.4 Calibration components, 1-methyl-naphthalene (98 % (m/m), a fatty acid methyl ester (as specified in EN 14214) and dotriacontane (C32H66, 97 % (m/m). NOTE Fatty acid methyl esters that are mainly consisting of

43、C18 FAME compounds such as rapeseed or soy are suitable components. Other methyl esters, such as palm oil, with higher amounts of C16 compounds, are not suitable 5.5 Solvent, for preparing calibration mixture. A typical solvent to be used is n-heptane (99 % (m/m) purity). Other solvents or mixtures

44、of hydrocarbons can be used provided their boiling point is in the range of about 80C to about 160C to limit possible evaporation when preparing the mixture and overcome interference with the 1-methylnaphthalene peak. 5.6 Calibration mixture Prepare about 100 g of a calibration mixture by gravimetri

45、cally blending the components mentioned in 5.4. Typically a blend of 0,1 % (m/m) 1-methyl-naphthalene, 0,2 % (m/m) dotriacontane and 0,2 % (m/m) FAME in n-heptane is used. Record the masses to the nearest 0,1 mg when weighing the components. Calculate the % (m/m) of each calibration component in the

46、 mixture and round to the nearest 0,001 % (m/m). The boiling point range of the solvent shall not interfere with the calibration components. NOTE The calibration mixture may contain mixtures of different origin of FAMEs such as rapeseed or soy, as is most representative for a specific application. 6

47、 Apparatus 6.1 Gas chromatograph, with the following performance characteristics: 6.1.1 Flame ionization detector, the detector shall be capable of operating at a temperature at least equivalent to the maximum column temperature employed in the method. The capillary column should sit just below the

48、flame tip and it is recommended that the orifice of the jet should be 0,6 mm minimum to prevent frequent blocking with silicones. 6.1.2 Column temperature programmer, capable of linear programmed temperature operation over a range from ambient temperature to 350 C. 6.1.3 Sample inlet system, consisting of a programmable temperature vaporizer (PTV) or temperature programmable cool on-column (COC) injection port. The maximum temperature of the injection device shall be higher than the final ov