SIST EN 14517:2004
(Main)Liquid petroleum products - Determination of hydrocarbon types and oxygenates in petrol - Multidimensional gas chromatography method
Liquid petroleum products - Determination of hydrocarbon types and oxygenates in petrol - Multidimensional gas chromatography method
This document specifies the gas chromatographic determination of saturated, olefinic and aromatic hydrocarbons in finished petrol according to EN 228. Additionally, the benzene content, oxygenate compounds and the total oxygenate content can be determined.
The method is applicable for finished petrol with total aromatic content up to 50 % (V/V), total olefin content from about 1,5 % (V/V) up to 30 % (V/V), oxygenate compounds up to 15 % (V/V), total oxygen content from about 1,5 % (m/m) to about 3 % (m/m) and benzene content less than 2 % (V/V).
NOTE 1 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.
NOTE 2 While developing this method the final boiling point was limited to 215 °C.
NOTE 3 For oxygenate compounds, precision data has only been established on samples containing ethyl-tert-butyl ether (ETBE), methyl-tert-butyl ether (MTBE), tert-amyl-methyl ether (TAME) and ethanol. Applicability of this test method has also been verified for the determination of methanol, n-propanol, i-propanol, i-butanol, tert-butanol, acetone, and di-isopropyl ether (DIPE). However, no precision data have been determined for these compounds. If any of these oxygenate compounds are present in the sample, their contents should be determined by use of the appropriate test methods given in EN 228.
NOTE 4 Although this test method may be used to determine higher olefin contents up to 50 % (V/V), the precision for olefins was only tested in the range from about 1,5 % (V/V) to about 30 % (V/V).
NOTE 5 Although specifically developed for the analysis of finished petrol that contains oxygenates, this test method may also be applied to other hydrocarbon streams having similar boiling ranges such as naphthas and reformates.
Flüssige Mineralölerzeugnisse - Bestimmung der Kohlenwasserstoffgruppen und sauerstoffhaltigen Verbindungen in Ottokraftstoffen - Multidimensionales gaschromatographisches Verfahren
Dieses Dokument legt ein Verfahren zur gaschromatographischen Bestimmung der Gehalte an gesättigten, olefinischen und aromatischen Kohlenwasserstoffen in handelsüblichen Ottokraftstoffen nach EN 228 fest. Zusätzlich können die Gehalte an Benzol, sauerstoffhaltigen Verbindungen und der Gesamtsauerstoffgehalt bestimmt werden.
Dieses Verfahren ist anwendbar für Ottokraftstoffe mit einem Gesamtaromatengehalt bis 50 % (V/V), einem Gesamtolefingehalt von 1,5 % (V/V) bis 30 % (V/V), einem Gehalt an sauerstoffhaltigen Verbindungen bis 15 % (V/V), einem Gesamtsauerstoffgehalt von etwa 1,5 % (m/m) bis etwa 3 % (m/m) und einem Benzolgehalt unter 2 % (V/V).
ANMERKUNG 1 Für die Zwecke dieser Europäischen Norm werden die "Begriffe" "% (m/m)" und "% (V/V)" verwendet, um den Massenanteil in Prozent bzw. den Volumenanteil in Prozent auszudrücken.
ANMERKUNG 2 Während der Entwicklung des Verfahrens war das Siedeende auf 215 °C eingeschränkt.
ANMERKUNG 3 Präzisionsdaten für sauerstoffhaltige Verbindungen wurden nur für Proben, die Ethyl-tert-butylether (ETBE), Methyl-tert-butylether (MTBE), tert-Amyl-methylether (TAME) und Ethanol enthalten, bestimmt. Dieses Verfahren ist ebenso für die Bestimmung des Gehaltes an Methanol, n-Propanol, i-Propanol, i-Butanol, tert-Butanol, Aceton und di Isopropylether (DIPE) geeignet, jedoch liegen hierfür keine Präzisionsdaten vor. Falls diese Verbindungen in der Probe enthalten sind, sollten deren Gehalte mit den entsprechenden, in EN 228 angegebenen Prüfverfahren bestimmt werden.
ANMERKUNG 4 Obwohl dieses Verfahren für die Bestimmung von Olefingehalten bis zu 50 % (V/V) verwendet werden kann, wurden die Präzisionsdaten lediglich für den Bereich von etwa 1,5 % (V/V) bis etwa 30 % (V/V) ermittelt.
ANMERKUNG 5 Obgleich dieses Verfahren zur Analyse von handelsüblichen Ottokraftstoffen entwickelt wurde, kann es ebenso für Kohlenwasserstoffschnitte mit ähnlichen Siedebereichen wie Naphthas und Reformaten angewendet werden.
Produits pétroliers liquides - Détermination des familles d'hydrocarbures et de la teneur en composés oxygénés de l'essence automobile - Méthode par chromatographie multidimensionnelle en phase gazeuse
Le présent document prescrit une méthode pour la détermination par chromatographie gazeuse des teneurs en hydrocarbures saturés, oléfiniques et aromatiques dans les essences pour l'automobile conformes a l'EN 228. En outre, les teneurs en benzene, en composés oxygénés et en oxygene total peuvent etre mesurées par cette norme.
La méthode est applicable aux essences finies dont la teneur en aromatiques totaux est au plus de 50 % (V/V), la teneur en oléfines est comprise entre environ 1,5 % (V/V) et 30 % (V/V) au plus, la teneur en composés oxygénés est au plus de 15 % (V/V), la teneur en oxygene total est comprise entre environ 1,5 % (m/m) et 3 % (m/m), et la teneur en benzene est inférieure a 2 % (V/V).
NOTE 1 Pour les besoins de la présente Norme européenne, les expressions "% (m/m)" et "% (V/V)" sont utilisées pour désigner respectivement les fractions massiques et les fractions volumiques.
NOTE 2 Au moment du développement de la présente méthode, le point d'ébullition final était limité a 215 °C.
NOTE 3 En ce qui concerne les composés oxygénés, la fidélité n'a été établie que sur des échantillons contenant de l'éthyl tert-butyl éther (ETBE), du méthyl tert-butyl éther (MTBE), du tert-amyl méthyl éther (TAME) et de l'éthanol. L'applicabilité de la présente méthode d'essai a, en outre, été vérifiée pour le dosage du méthanol, du n-propanol, de l'iso-propanol, de l'iso-butanol, du tert-butanol, de l'acétone et du di-isopropyl éther (DIPE). Cependant, aucune donnée de fidélité concernant ces composés n'a été déterminée. Si l'un ou plusieurs de ces composés s'avéraient présents dans l'échantillon, il convient de déterminer leurs teneurs par les méthodes appropriées données dans l'EN 228.
NOTE 4 Bien que la présente méthode d'essai puisse etre utilisée pour mesurer des teneurs plus élevées en oléfines, jusqu'a 50 % (V/V), la fidélité pour les oléfines a seulement été établie pour des teneurs comprises entre environ 1,5 % (V/V) et 30 % (V/V).
Utekočinjeni naftni proizvodi – Določanje vrste ogljikovodikov in oksigenatov v bencinih – Metoda multidimenzionalne plinske kromatografije
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Flüssige Mineralölerzeugnisse - Bestimmung der Kohlenwasserstoffgruppen und sauerstoffhaltigen Verbindungen in Ottokraftstoffen - Multidimensionales gaschromatographisches VerfahrenProduits pétroliers liquides - Détermination des familles d'hydrocarbures et de la teneur en composés oxygénés de l'essence automobile - Méthode par chromatographie multidimensionnelle en phase gazeuseLiquid petroleum products - Determination of hydrocarbon types and oxygenates in petrol - Multidimensional gas chromatography method75.160.20Liquid fuelsICS:Ta slovenski standard je istoveten z:EN 14517:2004SIST EN 14517:2004en01-november-2004SIST EN 14517:2004SLOVENSKI
STANDARDSIST EN ISO 22854:20081DGRPHãþD
SIST EN 14517:2004
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14517September 2004ICS 75.160.20English versionLiquid petroleum products - Determination of hydrocarbon typesand oxygenates in petrol - Multidimensional gas chromatographymethodProduits pétroliers liquides - Détermination des famillesd'hydrocarbures et de la teneur en composés oxygénés del'essence automobile - Méthode par chromatographiemultidimensionnelle en phase gazeuseFlüssige Mineralölerzeugnisse - Bestimmung derKohlenwasserstoffgruppen und sauerstoffhaltigenVerbindungen in Ottokraftstoffen - Multidimensionalesgaschromatographisches VerfahrenThis European Standard was approved by CEN on 21 June 2004.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2004 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14517:2004: ESIST EN 14517:2004
EN 14517:2004 (E) 2 Contents page Foreword.3 1 Scope.4 2 Normative references.4 3 Terms and definitions.5 4 Principle.5 5 Reagents and Materials.6 5.1 Gases.6 5.2 Vials.6 5.3 Test mixtures.6 6 Apparatus.6 6.1 Gas chromatograph.6 6.2 Switching valves.6 6.3 Traps.7 7 Sampling.7 8 Procedure.7 8.1 Preparing the apparatus.7 8.2 Preparation of a sample for analysis.7 8.3 Injection volume.7 8.4 Verification of proper function.8 8.5 Validation.8 9 Preparation.8 9.1 Preparation of the analysis sample.8 9.2 Preparation of the instrument and test conditions.8 10 Calculation.8 10.1 Calculation as % (m/m).8 10.2 Calculation as % (V/V).10 10.3 Calculation of total oxygen content in % (m/m).12 10.4 Data report according to EN 228 specification.12 11 Expression of results.12 12 Precision.13 12.1 General.13 12.2 Repeatability.13 12.3 Reproducibility.13 13 Test report.13 Annex A
(informative)
Column specifications.14 Annex B
(informative)
Sample chromatograms.15 Bibliography.19
SIST EN 14517:2004
EN 14517:2004 (E) 3 Foreword This document (EN 14517:2004) has been prepared by Technical Committee CEN/TC 19 “Petroleum products, lubricants and related products”, 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 March 2005, and conflicting national standards shall be withdrawn at the latest by March 2005. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
SIST EN 14517:2004
EN 14517:2004 (E) 4 1 Scope This document specifies the gas chromatographic determination of saturated, olefinic and aromatic hydrocarbons in finished petrol according to EN 228. Additionally, the benzene content, oxygenate compounds and the total oxygenate content can be determined. The method is applicable for finished petrol with total aromatic content up to 50 % (V/V), total olefin content from about 1,5 % (V/V) up to 30 % (V/V), oxygenate compounds up to 15 % (V/V), total oxygen content from about 1,5 % (m/m) to about 3 % (m/m) and benzene content less than 2 % (V/V). NOTE 1 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. NOTE 2 While developing this method the final boiling point was limited to 215 °C. NOTE 3 For oxygenate compounds, precision data has only been established on samples containing ethyl-tert-butyl ether (ETBE), methyl-tert-butyl ether (MTBE), tert-amyl-methyl ether (TAME) and ethanol. Applicability of this test method has also been verified for the determination of methanol, n-propanol, i-propanol, i-butanol, tert-butanol, acetone, and di-isopropyl ether (DIPE). However, no precision data have been determined for these compounds. If any of these oxygenate compounds are present in the sample, their contents should be determined by use of the appropriate test methods given in EN 228. NOTE 4 Although this test method may be used to determine higher olefin contents up to 50 % (V/V), the precision for olefins was only tested in the range from about 1,5 % (V/V) to about 30 % (V/V). NOTE 5 Although specifically developed for the analysis of finished petrol that contains oxygenates, this test method may also be applied to other hydrocarbon streams having similar boiling ranges such as naphthas and reformates. 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 228, Automotive fuels – Unleaded petrol – Requirements and test methods. EN 1601, Liquid petroleum products – Unleaded petrol – Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography (O-FID). EN 13132, Liquid petroleum products – Unleaded petrol – Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography using column switching.
EN ISO 3170, Petroleum liquids – Manual sampling (ISO 3170:2004). EN ISO 3171, Petroleum liquids – Automatic pipeline sampling (ISO 3171:1988). SIST EN 14517:2004
EN 14517:2004 (E) 5 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 hydrocarbon group (singular) family of hydrocarbons such as saturated hydrocarbons, olefinic hydrocarbons, etc. 3.1.1 saturated hydrocarbon hydrocarbon type such as the n-paraffins, iso-paraffins, naphthenes and poly-naphthenes with 3 to 12 carbon number 3.1.2 olefinic hydrocarbon hydrocarbon type such as the n-olefins, i-olefins and cyclic olefins with 3 to 10 carbon number 3.1.3 aromatic hydrocarbon hydrocarbon type benzene, toluene and higher homologous series with 6 to 10 carbon number and naphthalenes up to 12 carbon number 3.1.4 oxygenated hydrocarbon hydrocarbon type alcohols and ethers, which addition is allowed according to EN 228 (see NOTE 3 in Clause 1). 3.2 partial group one carbon number in an individual group, being either a single compound like toluene or an isomeric mixture like n-butane and i-butane 4 Principle 4.1 The sample to be analyzed is separated into hydrocarbon groups by means of gas chromatographic analysis using special column-coupling and column-switching procedures. The sample is injected in the gas chromatographic system and after vaporization separated into the different groups. Detection is always done by a flame ionization detector (FID). 4.2 The mass concentration of each detected compound or hydrocarbon group is determined by the application of relative response factors (see 10.1) to the area of the detected peaks, followed by normalization to 100 %. For samples containing oxygenates that cannot be determined by this test method, the hydrocarbon results are normalized to 100 % minus the value of oxygenates as determined by another method such as EN 1601 or EN 13132. The liquid volume concentration of each detected compound or hydrocarbon group is determined by application of density values (see 10.2) to the calculated mass concentration of the detected peaks followed by normalization to 100 %. 4.3 After this analysis the petrol is separated into hydrocarbon groups and carbon numbers. By the use of the corresponding relative response factors (see Table 1 and Table 2) the mass distributions of the groups can be calculated. SIST EN 14517:2004
EN 14517:2004 (E) 6 5 Reagents and Materials 5.1 Gases 5.1.1 Hydrogen, 99,999 % pure 5.1.2 Helium, 99,999 % pure 5.1.3 Compressed air NOTE Installation of suitable moisture filters is recommended for Helium and Hydrogen lines. 5.2 Vials Use airtight and inert vials, e.g. with rubber-membrane caps covered with self-sealing poly-tetra-fluorethylene (PTFE). 5.3 Test mixtures Finished petrol(s) as reference containing compone
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