Automotive fuels - Determination of high-boiling components including fatty acid methyl esters in petrol and ethanol (E85) automotive fuel - Gas chromatography method

This European Standard specifies a determination method of high boiling components in petrol and in ethanol (E85) automotive fuel. The method is based on capilary gas chromatography using flame ionisation detection. High boiling components, such as diesel or fatty acid methyl esters (FAME), are defined by those having a boiling point greater than or equal to 1-methyl-naphthalene.
This European Standard is applicable to materials having a vapour pressure low enough to permit sampling at ambient temperature and a boiling range of at least 100 °C. This method pays special attention to fatty acid methyl esters.

Kraftstoffe für Kraftfahrzeuge - Bestimmung von hochsiedenden Komponenten in Ottokraftstoff und Ethanol (E85)-Autokraftstoff - Gaschromatographisches Verfahren

Diese Europäische Norm legt ein Verfahren zur Bestimmung hochsiedender Komponenten in Ottokraftstoff nach EN 228 [1] und in Ethanol (E85)-Autokraftstoff nach CEN/TS 15293 [2] mittels Kapillar-Gaschromatographie mit Flammenionisationsdetektor fest. Dieses Verfahren ist anwendbar auf hochsiedende Substanzen wie Fettsäure-Methylester (FAME) oder Dieselkraftstoff, die einen Siedepunkt größer oder gleich 1-Methylnaphthalin besitzen.
Diese Norm ist anwendbar auf Stoffe mit einem Dampfdruck, der niedrig genug zur Probenahme bei Umgebungstemperatur ist, sowie einem Siedebereich von mindestens 100 °C. Dieses Verfahren berücksichtigt speziell Fettsäuremethylester.
Der Messbereich für den hochsiedenden Anteil ist in Ottokraftstoff von etwa 0,7 % (m/m) bis etwa 2,5 % (m/m). Für FAME ist der Bereich von etwa 0,2 % (m/m) bis etwa 2 % (m/m).
Der Messbereich für den hochsiedenden Anteil ist in Ethanol (E85) Autokraftstoff von etwa 0,2 % (m/m) bis etwa 2,2 % (m/m). Für FAME ist der Bereich von etwa 0,05 % (m/m) bis etwa 1,5 % (m/m).
ANMERKUNG 1   Für Berechnung des FAME Anteils werden im Rahmen dieses Verfahrens nur die C18-Isomere berücksichtigt.
ANMERKUNG 2   Für die Zwecke dieser Europäischen Norm wird zur Angabe des Massenanteils einer Substanz der Ausdruck „% (m/m)“ und für den Volumenanteil einer Substanz der Ausdruck „% (V/V)“ verwendet.
WARNUNG — Die Anwendung dieser Norm kann den Einsatz gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Europäische Norm gibt nicht vor, alle mit ihrer Anwendung verbundenen Sicherheitsprobleme anzusprechen. Der Anwender dieser Norm ist dafür verantwortlich, vorher angemessene Maßnahmen in Hinblick auf Sicherheit und Gesundheit zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln.

Carburants pour automobiles - Détermination des components haute-bouillantes dans l'essence et dans carburant automobile Ethanol (E85) - Méthode par chromatographie en phase gazeuse

Goriva za motorna vozila - Določevanje komponent z visokim vreliščem, vključno z metilnimi estri maščobnih kislin, v gorivih za motorna vozila, motornem bencinu in etanolu (E85) - Metoda plinske kromatografije

Ta evropski standard opredeljuje metodo določanja komponent z visokim vreliščem v motornem bencinu in etanolu (E85). Metoda temelji na metodi plinske kromatografije z uporabo z zaznavanjem plamenske ionizacije. Komponente z visokim vreliščem, kot so dizelsko gorivo ali metilni estri maščobnih kislin (FAME), so določeni s tistimi, ki imajo vrelišče višje ali enako kot 1-metil-naftalen. Ta evropski standard se uporablja za materiale, ki imajo dovolj nizek parni tlak, da je mogoče izvajati vzorčenje pri temperaturi okolice, in območje vrelišča najmanj 100 °C. Ta metoda posveča posebno pozornost metilnim estrom maščobnih kislin.

General Information

Status
Published
Public Enquiry End Date
09-Apr-2014
Publication Date
26-Jul-2015
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Jul-2015
Due Date
05-Sep-2015
Completion Date
27-Jul-2015

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kraftstoffe für Kraftfahrzeuge - Bestimmung von hochsiedenden Komponenten in Ottokraftstoff und Ethanol (E85)-Autokraftstoff - Gaschromatographisches VerfahrenCarburants pour automobiles - Détermination des components haute-bouillantes dans l'essence et dans carburant automobile Ethanol (E85) - Méthode par chromatographie en phase gazeuseAutomotive fuels - Determination of high-boiling components including fatty acid methyl esters in petrol and ethanol (E85) automotive fuel - Gas chromatography method75.160.20Liquid fuelsICS:Ta slovenski standard je istoveten z:EN 16270:2015SIST EN 16270:2015en,fr,de01-september-2015SIST EN 16270:2015SLOVENSKI
STANDARDSIST EN 16270:20121DGRPHãþD



SIST EN 16270:2015



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16270
June 2015 ICS 75.160.20 Supersedes EN 16270:2012English Version
Automotive fuels - Determination of high-boiling components including fatty acid methyl esters in petrol and ethanol (E85) automotive fuel - Gas chromatographic method
Carburants pour automobiles - Détermination des composés à haut point d'ébullition dont les esters méthyliques d'acides gras dans l'essence et dans le carburant éthanol pour automobiles (E85) - Méthode par chromatographie en phase gazeuse
Kraftstoffe für Kraftfahrzeuge - Bestimmung von hochsiedenden Komponenten inklusive Fettsäure-Methylester in Ottokraftstoff und Ethanol (E85)-Kraftstoff für Fahrzeuge - Gaschromatographisches Verfahren This European Standard was approved 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 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, 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
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management 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 ESIST EN 16270:2015



EN 16270:2015 (E) 2 Contents Page Foreword .3 1 Scope .4 2 Normative references .4 3 Terms and definitions .4 4 Principle .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 results . 13 14 Precision . 13 14.1 General . 13 14.2 Repeatability . 13 14.3 Reproducibility . 13 15 Test report . 14 Bibliography . 15
SIST EN 16270:2015



EN 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 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 2015, and conflicting national standards 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 16270:2012. 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 this 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16270:2015



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] 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 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 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 calculating 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 involve 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 regulatory 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 referenced 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 - Automatic 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 high 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 SIST EN 16270:2015



EN 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) Y FID signal Figure 1a — Chromatogram explaining high boiling fraction SIST EN 16270:2015



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 boiling 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 SIST EN 16270:2015



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-FAME 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 quantification. 3.5 total high boiling area for a calibration mixture Atc sum of the areas of 1-methylnaphthalene and dotriacontane Note 1 to entry: See Figure 2. 3.6 total FAME area for a calibration mixture Afc cumulative area from the start of the FAME C18-fraction until the end of the FAME C18-fraction for a calibration mixture Note 1 to entry: See Figure 2. 3.7 total high boiling area for a sample As cumulative area from the start of the high boiling fraction until the end of high boiling
...

SLOVENSKI STANDARD
oSIST prEN 16270:2014
01-marec-2014
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Automotive fuels - Determination of high-boiling components including fatty acid methyl
esters in petrol and ethanol (E85) automotive fuel - Gas chromatography method
Kraftstoffe für Kraftfahrzeuge - Bestimmung von hochsiedenden Komponenten in
Ottokraftstoff und Ethanol (E85)-Autokraftstoff - Gaschromatographisches Verfahren
Carburants pour automobiles - Détermination des components haute-bouillantes dans
l'essence et dans carburant automobile Ethanol (E85) - Méthode par chromatographie
en phase gazeuse
Ta slovenski standard je istoveten z: prEN 16270
ICS:
75.160.20 7HNRþDJRULYD Liquid fuels
oSIST prEN 16270:2014 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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oSIST prEN 16270:2014

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oSIST prEN 16270:2014

EUROPEAN STANDARD
DRAFT
prEN 16270
NORME EUROPÉENNE

EUROPÄISCHE NORM

February 2014
ICS 75.160.20 Will supersede EN 16270:2012
English Version
Automotive fuels - Determination of high-boiling components
including fatty acid methyl esters in petrol and ethanol (E85)
automotive fuel - Gas chromatography method
Carburants pour automobiles - Détermination des Kraftstoffe für Kraftfahrzeuge - Bestimmung von
components haute-bouillantes dans l'essence et dans hochsiedenden Komponenten in Ottokraftstoff und Ethanol
carburant automobile Ethanol (E85) - Méthode par (E85)-Autokraftstoff - Gaschromatographisches Verfahren
chromatographie en phase gazeuse
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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey 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: Avenue Marnix 17, B-1000 Brussels
© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 16270:2014 E
worldwide for CEN national Members.

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oSIST prEN 16270:2014
prEN 16270:2014 (E)
Contents Page
Foreword .3
1 Scope .3
2 Normative references .3
3 Terms and definitions .3
4 Principle .6
5 Reagents and materials .6
6 Apparatus .7
7 Sampling .8
8 Preparation of the apparatus .8
9 Calibration .8
10 Procedure .9
11 Visual inspection of the chromatograms . 10
12 Calculation . 11
12.1 General . 11
12.2 Total high boiling fraction . 11
12.3 FAME fraction . 11
13 Expression of results . 11
14 Precision . 11
14.1 General . 11
14.2 Repeatability . 12
14.3 Reproducibility . 12
15 Test report . 12
Bibliography . 13

2

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oSIST prEN 16270:2014
prEN 16270:2014 (E)
Foreword
This document (prEN 16270:2014) 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 16270:2012. Its scope has been extended to ethanol (E85) automotive fuel,
the precision data have been updated and further technical improvements have been included.
1 Scope
This European Standard specifies a determination method of high boiling components in petrol according to
EN 228 [1] and ethanol automotive fuels according to CEN/TS 15293 [2] by capillary gas chromatography
using flame ionisation 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.
The standard is applicable to materials having a vapour pressure low enough to permit sampling at ambient
temperature and 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 FAME fraction the range is from about 0,2 % (m/m) to about 2 % (m/m).
In ethanol automotive fuel the measurement range 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 calculating the FAME fraction, this method only takes the C18-isomers 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 involve 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 regulatory limitations prior to use.
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 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 3170:2004)
EN ISO 3171, Petroleum liquids - Automatic pipeline sampling (ISO 3171:1988)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3

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oSIST prEN 16270:2014
prEN 16270:2014 (E)
NOTE Figure 1 gives some visual explanation of the definitions on the basis of an exemplary chromatogram.
3.1
start of high boiling fraction
1-methyl-naphthalene is the first peak to be included in the high boiling fraction
3.2
end of high boiling fraction
dotriacontane (n-C32) is the last peak to be included in the high boiling fraction
3.3
Fatty acid methyl esters fraction
FAME fraction
combined area of the C18:0, C18:1, C18:2 and C18:3-FAME peaks
Note 1 to entry: The area is defined as shown in Figure 1b
Note 2 to entry: This method only takes the C18-isomers into account as other isomers 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 quantification.


Key
1 Methyl-naphthalene 4 Start high boiling fraction
2 Total high boiling area 5 Baseline for high boiling fraction
3 Dotriacontane
x-axis time (min) y-axis FID signal
Figure 1a – Chromatogram explaining high boiling fraction
4

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oSIST prEN 16270:2014
prEN 16270:2014 (E)

Key
1 C18 FAME peak area 2 Manual baseline for FAME calculation
x-axis time (min) y-axis FID signal
Figure 1b – Chromatogram explaining FAME fraction

Key
1 1-Methyl-naphthalene – start of high boiling fraction 3 Dotriacontane – end of high boiling fraction
2 C18-FAME
x-axis time (min) y-axis FID signal
Figure 2 — Example of a calibration mixture chromatogram
3.4
total high boiling area for a calibration mixture
Atc
sum of the areas of 1-methylnaphthalene and dotriacontane
Note 1 to entry: See Figure 2.
5

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oSIST prEN 16270:2014
prEN 16270:2014 (E)
3.5
total FAME area for a calibration mixture
Afc
cumulative area from the start of the FAME C18-fraction until the end of the FAME C18-fraction for a
calibration mixture
Note 1 to entry: See Figure 2.
3.6
total high boiling area for a sample
As
cumulative 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.
3.7
total FAME fraction area for a sample
Af
cumulative area from 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 c
...

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