Automotive fuels - Determination of methanol in automotive ethanol (E85) fuel by gas chromatography - Part 2: Method using heart cut technique

This European Standard specifies a determination method of methanol in E85 automotive fuel by capillary gas chromatography using heart cutting and flame ionisation detection. The standard is applicable to fuels having a methanol content from about 0,5 to about 1,6 % (V/V). The method is applicable in a wider range, from about 0.1% to about 2.2 % (V/V), but precision was not established over this full range.

Kraftstoffe für Kraftfahrzeuge - Bestimmung von Methanol im automotive Ethanol (E85) als Kraftstoff durch Gaschromatographie - Teil 2: Methode mit Herz schnitt Technik

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Methanol in Ethanolkraftstoff (E85) (auch benannt als Ethanolkraftstoff (E85) oder kurz 'E85') durch Kapillarsäulengaschromatographie mittels Heart-Cut-Technik fest. Spezifika¬tionen zur Kraftstoffqualität für dieses Produkt sind vorhanden, siehe Literaturhinweis [1].
Diese Norm ist anwendbar auf Kraftstoffe mit einem Methanolgehalt von etwa 0,5 % (V/V) bis etwa 1,5 % (V/V). Es können auch andere Methanolkonzentrationen bestimmt werden, jedoch liegen keine Präzisionsdaten für Ergebnisse außerhalb des festgelegten Bereichs vor.
ANMERKUNG   Für die Zwecke dieser Europäischen Norm werden die Begriffe '% (m/m)' und '% (V/V)' verwendet, um Massenanteile, μ, bzw. Volumenanteile, φ, anzugeben.
WARNUNG - Die Anwendung diese Norm kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Norm beansprucht nicht, alle damit verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung des Anwenders dieser Norm, vor ihrer Anwendung geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz des Personals zu ergreifen, und dafür Sorge zu tragen, dass behördliche und gesetzliche Maßnahmen eingehalten werden.

Carburants pour automobiles - Détermination de la teneur en méthanol dans l'automobile l'éthanol (E85) de carburant par chromatographie en phase gazeuse - Partie 2: Méthode utilisant coeur coupe technique

La présente Norme européenne spécifie une méthode de détermination de la teneur en méthanol dans le carburant éthanol (E85) pour automobiles par chromatographie en phase gazeuse sur colonne capillaire avec « heart-cutting » et un détecteur à ionisation de flamme. Il existe des spécifications sur la qualité de ce produit utilisé comme carburant ; voir [2].
La présente norme s'applique aux carburants ayant une teneur en méthanol comprise entre environ 0,5 % (V/V) et environ 1,6 % (V/V). La méthode décrite s'applique à une plus large plage, allant d'environ 0,1 % (V/V) à environ 2,2 % (V/V), mais aucune donnée de fidélité n'a été établie pour l'ensemble de cette plage.
NOTE    Pour les besoins de la présente Norme européenne, les termes « % (m/m) » et « % (V/V) » sont utilisés pour représenter les fractions massique, µ, et volumique, φ, respectivement.
ATTENTION — L'utilisation de la présente Norme européenne peut impliquer l'intervention de produits, d'opérations et d'équipements à caractère dangereux. La présente norme européenne n'est pas censée aborder tous les problèmes de sécurité concernés par son usage. Il est de la responsabilité de l'utilisateur de consulter et d'établir des règles de sécurité et d'hygiène appropriées et de déterminer l'applicabilité des restrictions réglementaires avant utilisation.

Goriva za motorna vozila - Določevanje metanola v motornem gorivu etanol (E85) s plinsko kromatografijo - 2. del: Metoda z uporabo tehnike "heart cut"

Ta evropski standard določa metodo določevanja metanola v motornem gorivu (E85) s kapilarno plinsko kromatografijo z uporabo tehnike »heart cut« in zaznavanjem plamenske ionizacije. Standard velja za goriva z vsebnostjo metanola od približno 0,5 do približno 1,6 % (V/V). Metoda velja za širok nabor, od približno 0,1 % do približno 2,2 % (V/V), vendar natančnost ni bila vzpostavljena za ta celoten nabor.

General Information

Status
Published
Public Enquiry End Date
30-Sep-2014
Publication Date
03-Jan-2016
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
16-Dec-2015
Due Date
20-Feb-2016
Completion Date
04-Jan-2016

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Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.FXWKraftstoffe für Kraftfahrzeuge - Bestimmung von Methanol im automotive Ethanol (E85) als Kraftstoff durch Gaschromatographie - Teil 2: Methode mit Herz schnitt TechnikCarburants pour automobiles - Détermination de la teneur en méthanol dans l'automobile l'éthanol (E85) de carburant par chromatographie en phase gazeuse - Partie 2: Méthode utilisant coeur coupe techniqueAutomotive fuels - Determination of methanol in automotive ethanol (E85) fuel by gas chromatography - Part 2: Method using heart cut technique75.160.20Liquid fuels71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysisICS:Ta slovenski standard je istoveten z:EN 16761-2:2015SIST EN 16761-2:2016en,fr,de01-februar-2016SIST EN 16761-2:2016SLOVENSKI
STANDARD



SIST EN 16761-2:2016



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16761-2
December
t r s w ICS
y wä s x rä t r English Version
Automotive fuels æ Determination of methanol in Part
tã Method using heart cut technique Carburants pour automobiles æ Détermination de la pour automobiles par chromatographie en phase gazeuse æ Partie
tã Méthode
5 5heartæcutting 5 5
Kraftstoffe für Kraftfahrzeuge æ Bestimmung des Gaschromatographie æ Teil
tã Verfahren mittels HeartæCutæTechnik This European Standard was approved by CEN on
s r October
t r s wä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s w CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x y x sæ tã t r s w ESIST EN 16761-2:2016



EN 16761-2:2015 (E) 2 Contents
Page European foreword . 3 1 Scope . 4 2 Normative references . 4 3 Terms and definitions . 4 4 Principle . 5 5 Reagents and materials . 6 6 Apparatus . 6 7 Sampling . 7 8 Preparation of the apparatus . 7 9 Density determination . 8 10 Calibration . 9 11 Linearity check . 10 12 Procedure. 10 13 Calculation . 11 14 Expression of results . 12 15 Precision . 12 15.1 General . 12 15.2 Repeatability, r . 12 15.3 Reproducibility, R . 12 16 Test report . 12 Bibliography . 13
SIST EN 16761-2:2016



EN 16761-2:2015 (E) 3 European foreword This document (EN 16761-2:2015) 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 June 2016, and conflicting national standards shall be withdrawn at the latest by June 2016. 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. The determination of a significant amount of methanol in ethanol (E85) automotive fuels was deemed to be necessary to check the product for compliance against EU emission regulations. The CEN/TC 19 Ethanol Fuels Task Force requested the development of such a determination technique. In EN 16761, Automotive fuels — Determination of methanol in automotive ethanol (E85) fuel by gas chromatography, two test methods were developed that comply with this scope: — Part 1: Method using single column technique; — Part 2: Method using heart cut technique [the present document]. 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, 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 16761-2:2016



EN 16761-2:2015 (E) 4 1 Scope This European Standard specifies a determination method of methanol in automotive ethanol (E85) fuel (also designated as ethanol (E85) automotive fuel or shortly "E85") by capillary gas chromatography using heart cutting technique. Fuel quality specifications for this product exist, see Bibliography Entry [1]. This standard is applicable to fuels having a methanol content from about 0,5 % (V/V) to about 1,5 % (V/V). Other methanol contents can also be determined, however no precision data for results outside the specified range is available. NOTE For the purposes of this European Standard, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass fraction, µ, and the volume fraction, . WARNING — The use of this standard can involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of users of this standard to take appropriate measures to ensure the safety and health of personnel prior to application of the standard, and fulfil statutory and regulatory requirements for this purpose. 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 228, Automotive fuels — Unleaded petrol — Requirements and test methods EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170) EN ISO 3171, Petroleum liquids — Automatic pipeline sampling (ISO 3171) EN ISO 3675, Crude petroleum and liquid petroleum products — Laboratory determination of density — Hydrometer method (ISO 3675) EN ISO 3838, Crude petroleum and liquid or solid petroleum products — Determination of density or relative density — Capillary-stoppered pyknometer and graduated bicapillary pyknometer methods (ISO 3838) EN ISO 12185, Crude petroleum and petroleum products — Determination of density — Oscillating U-tube method (ISO 12185) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 methanol calibration area area of the methanol peak in the calibration chromatogram Note 1 to entry: Figure 4 shows an example of a calibration chromatogram. 3.2 methanol sample area As area of methanol peak in the sample chromatogram SIST EN 16761-2:2016



EN 16761-2:2015 (E) 5 Note 1 to entry: Figure 6 shows an example of a sample chromatogram. 4 Principle This standard describes the analysis of methanol content in automotive ethanol (E85) fuels using the heart cut technique. The analyser is based upon the principle described by D.R. Deans [3]. This technique controls the pressure between two columns and directs the effluent of a (pre) column to usually two columns, an analytical column and a monitor column. By using columns of a very different nature as pre column and analytical column (e.g. a non-polar and a polar column) separations can be achieved that are difficult to obtain using a single column. This allows the analysis of methanol to be independent of any impurities or high boiling material that may be present in the sample. The method uses external standard calibration. The sample is injected onto a methyl silicone pre column which elutes the methanol and part of the ethanol plus any light hydrocarbons to the analytical column (Figure 1). After methanol has fully eluted onto the analytical column, the valve and thus a Pressure Control Module (PCM) pressure is switched and the components coming from the pre column are
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