EN 16270:2012
(Main)Automotive fuels - Determination of high-boiling components including fatty acid methyl esters in petrol - Gas chromatographic method
Automotive fuels - Determination of high-boiling components including fatty acid methyl esters in petrol - Gas chromatographic method
This European Standard specifies a determination method of high boiling components in petrol according to EN 228 [1] 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.
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.
The measurement range for the high boiling fraction is from 0,7 % (m/m) to 2,5 % (m/m). For the FAME fraction, the range is from 0,2 % (m/m) to 2 % (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 standard, the terms "% (m/m)" and "% (V/V)" are used to represent the mass fraction (µ) and the volume fraction (µ) of a material respectively.
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.
Kraftstoffe für Kraftfahrzeuge - Bestimmung hochsiedender Komponenten einschließlich Fettsäure-Methylester in Ottokraftstoff - Gaschromatographisches Verfahren
Diese Europäische Norm legt ein Verfahren zur Bestimmung hochsiedender Komponenten in Ottokraftstoff nach EN 228 [1] mittels Kapillar-Gaschromatographie mit Flammenionisisationsdetektor fest. Dieses Verfahren ist anwendbar auf hochsiedende Substanzen wie Fettsäure-Methylester (FAME) oder Dieselkraftstoff, die einen Siedepunkt größer oder gleich 1-Methylnaphthalin besitzen.
Diese Europäische Norm ist anwendbar auf Stoffe mit einem Dampfdruck, der niedrig genug zur Probenahme bei Umgebungstemperatur ist, sowie einem Siedebereich von mindestens 100 °C. Dies Verfahren berücksichtigt speziell Fettsäuremethylester.
Der Messbereich für den hochsiedenden Anteil ist von 0,7 % (m/m) bis 2,5 % (m/m). Für FAME ist der Bereich von 0,2 % (m/m) bis 2 % (m/m).
ANMERKUNG 1 Für Berechnung des FAME Anteils werden im Rahmen dieses Verfahrens nur die C18-Methylester-Verbingungen berücksichtigt.
ANMERKUNG 2 Für die Zwecke dieser Europäischen Norm wird zur Angabe des Massenanteils, μ, einer Substanz der Ausdruck „% (m/m)“ und für den Volumenanteil, φ, einer Substanz der Ausdruck „% (V/V)“ verwendet.
WARNUNG — Die Anwendung dieser Norm kann den Einsatz gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese 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 composés à haut point d'ébullition dont les esters méthyliques d'acides gras dans l'essence - Méthode par chromatographie en phase gazeuse
La présente Norme européenne prescrit une méthode de détermination des composés à haut point d’ébullition dans l’essence conforme à l’EN 228 [1] par chromatographie en phase gazeuse sur colonne capillaire avec détection par ionisation de flamme. Cette méthode est applicable aux produits à haut point d’ébullition, comme les esters méthyliques d'acide gras (EMAG) ou comme le gazole, ayant un point d’ébullition supérieur ou égal à celui du 1-méthyl-naphtalène.
Cette Norme européenne s’applique aux produits ayant une pression de vapeur assez basse pour permettre un échantillonnage à température ambiante et un intervalle de distillation d’au moins 100 °C. Cette méthode est particulièrement adaptée aux esters méthyliques d'acide gras.
La gamme de mesure pour la fraction à haut point d’ébullition s’étend de 0,7 % (m/m) à 2,5 % (m/m). Pour la fraction des EMAG, la gamme de mesure s’étend de 0,2 % (m/m) à 2 % (m/m).
NOTE 1 Pour le calcul sur la fraction des EMAG, la méthode ne prend en compte que les esters méthyliques C18.
NOTE 2 Pour les besoins de la présente norme, les expressions «% (m/m)» et «% (V/V)» représentent respectivement les fractions massiques, µ, et volumiques, φ, des produits.
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 komponent z visokim vreliščem v nafti - Metoda plinske kromatografije
Ta evropski standard določa metodo določevanja komponent z visokim vreliščem v nafti v skladu z EN 228 [1] in sicer s kapilarno plinsko kromatografijo z zaznavanjem plamenske ionizacije. Ta metoda je primerna za material z visokim vreliščem, kot je metilni ester maščobnih kislin (FAME) ali dizelsko gorivo, ki ima 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. Merilno območje za frakcijo z visokim vreliščem je od 0,7 % (m/m) do 2,5 % (m/m). Območje za frakcijo FAME je od 0,2 % (m/m) do 2 % (m/m).
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kraftstoffe für Kraftfahrzeuge - Bestimmung von hoch-siedenden Komponenten in Ottokraftstoff - Gaschromatographisches VerfahrenCarburants pour automobiles - Détermination des components haute-bouillantes dans l'essence - Méthode par chromatographie en phase gazeuseAutomotive fuels - Determination of high-boiling components in petrol - Gas chromatographic method75.160.20Liquid fuelsICS:Ta slovenski standard je istoveten z:EN 16270:2012SIST EN 16270:2012en,de01-november-2012SIST EN 16270:2012SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16270
September 2012 ICS 75.160.20 English Version
Automotive fuels - Determination of high-boiling components including fatty acid methyl esters in petrol - Gas chromatographic method
Carburants pour automobiles - Détermination des composés à haut point d'ébullition dont les esters méthyliques d'acides gras dans l'essence - Méthode par chromatographie en phase gazeuse
Kraftstoffe für Kraftfahrzeuge - Bestimmung hochsiedender Komponenten einschließlich Fettsäure-Methylester in Ottokraftstoff - Gaschromatographisches Verfahren This European Standard was approved by CEN on 27 July 2012.
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
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Avenue Marnix 17,
B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16270:2012: ESIST EN 16270:2012
NOTE 2 For the purposes of this standard, the terms “% (m/m)” and “% (V/V)” are used to represent the mass fraction (µ) and the volume fraction (3) of a material respectively. 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. 3.1
start of high boiling fraction first peak to be included in the high boiling fraction Note 1 to entry: In this determination method, this is the peak of 1-methyl-naphthalene. 3.2
end of high boiling fraction last peak to be included in the high boiling fraction Note 1 to entry: In this determination method, this is the peak of dotriacontane (n-C32). SIST EN 16270:2012
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 1. This only takes the C18-compounds into account as other methyl esters compounds such as C16:0 can only be present in very limited amounts. In addition, C16:0 co-elutes with an n-paraffin which would affect the quantification. Note 2 to entry: Figure 1 presents visual explanation of the definitions on the basis of an exemplary chromatogram.
Key
1 start of high boiling fraction from 1-methyl-naphthalene elution 6 FAME peak used for FAME calculation 2 area corresponding to high boilers (including FAME peaks) 7 baseline for FAME calculation 3 integration baseline 8 end of C32's elution 4 area under FAME baseline is high boiling material and is not considered FAME t time (min) 5 1-methyl-naphthalene Y FID Signal Figure 1 — Example chromatogram with explanation of definitions 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 for further explanation. SIST EN 16270:2012
Key 1 1-Methyl-naphthalene – start of high boiling fraction 2 C18-FAME 3 dotriacontane – end of high boiling fraction t time (min) Y FID signal Figure 2 — Example of a calibration mixture chromatogram 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 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 recognised analytical quality shall be used. SIST EN 16270:2012
5.5 Calibration mixture Prepare about 100 g of a calibration mixture by gravimetrically 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 mass percentage of each calibration component in the mixture and round to the nearest 0,001 % (m/m).
A typical solvent to be used is n-heptane (≥ 99 % purity). Other solvents or mixtures of hydrocarbons may be used provided their boiling point is in the range of about 80 °C to about 160 °C to limit possible evaporation when preparing the mixture and overcome interference with the boiling point of 1-methyl-naphthalene. The boiling point range of the solvent shall not interfere with the calibration components. The calibration sample may contain mixtures of different origin of FAME’s such as rapeseed or soy, as is most representative for a specific application. 6 Apparatus 6.1 Gas chromatograph, with the following performance characteristics: 6.1.1 Flame ionisation detector, which shall be capable of operating at a temperature at least equivalent to the maximum column temperature employed in the method. It is recommended that the capillary column sits just below the flame tip and that the orifice of the jet has an 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 vaporiser (PTV) or a temperature programmable cool on-column (COC) injection port.
The maximum temperature of the injection device shall be higher than the final oven temperature. The minimum temperature shall be low enough to prevent sample or solvent flashback, but high enough to allow sample focusing at the front of the column. Table 1 presents typical operating conditions. SIST EN 16270:2012
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