SIST EN 1601:2014
(Main)Liquid petroleum products - Unleaded petrol - Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography (O-FID)
Liquid petroleum products - Unleaded petrol - Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography (O-FID)
EN 1601 specifies a gas chromatographic method for the quantitative determination, in unleaded petrol having a final boiling point not greater than 220 °C, of individual organic oxygenate compounds in the range 0,17 % (m/m) to 15 % (m/m) in a direct analysis (without dilution), and total organically bound oxygen up to 3,9 % (m/m). For samples for which one of the oxygenate compounds content is higher than 15 % (m/m), a procedure with a dilution of the sample before the analysis is given.
Flüssige Mineralölerzeugnisse - Unverbleite Ottokraftstoffe - Bestimmung sauerstoffhaltiger organischer Verbindungen und des Gesamtgehalts an organisch gebundenem Sauerstoff mittels Gaschromatographie (O-FID)
Diese Europäische Norm legt ein direktes (ohne Verdünnung) gaschromatographisches Analysenverfahren zur quantitativen Bestimmung sauerstoffhaltiger Verbindungen im Bereich 0,17 % (m/m) bis 15 % (m/m) und des Gesamtgehaltes an organisch gebundenem Sauerstoff bis 3,9 % (m/m) in unverbleiten Ottokraftstoffen mit einem Siedeende nicht über 220 °C fest.
Für Proben, deren Gehalt an sauerstoffhaltigen Verbindungen höher als 15 % (m/m) ist, ist ein Verfahren mit der Verdünnung der Probe vor der Analyse gegeben.
ANMERKUNG 1 Präzisionsdaten für einen höheren Gehalt an sauerstoffhaltigen Verbindungen als 15 % (m/m) sind nicht verfügbar (siehe Vorwort).
ANMERKUNG 2 Für den Zweck dieser Europäischen Norm werden Massenanteil, µ, und Volumenanteil, φ, durch die Begriffe % (m/m) und % (V/V) ausgedrückt.
WARNUNG — Die Anwendung dieser Europäischen 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 zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln.
Produit pétroliers liquides - Essence sans plomb - Détermination des composés oxygénés organiques et de la teneur totale en oxygène organiquement lié par chromatographie en phase gazeuse (O-FID)
La présente Norme européenne prescrit une méthode de chromatographie en phase gazeuse pour le dosage des composés organiques oxygénés dans le domaine de 0,17 % (mlm) à 15 % (mlm) au moyen d’une analyse directe (sans dilution) et de l'oxygène total organiquement lié à une teneur maximale de 3,9 % (mlm) dans des essences sans plomb ayant un point d'ébullition final inférieur à 220 °C.
Pour les échantillons dont la teneur en oxygénés est supérieure à 15 % (m/m), une procédure de dilution de ces échantillons avant leur analyse est donnée.
NOTE 1 Les valeurs de fidélité ne sont pas disponibles pour des teneurs en composés oxygénés supérieures à
15 % (m/m).
NOTE 2 Pour les besoins du présent document, les termes «% (m/m)» et « % (V/V) » sont utilisés pour représenter la fraction massique (µ) et la fraction volumique (φ), respectivement.
AVERTISSEMENT: L'utilisation de la présente norme européenne implique l'intervention de produits, d'opérations et d'équipements à caractère dangereux. La présente norme européenne n'a pas la prétention d'aborder tous les problèmes de sécurité concernés par sa mise en oeuvre. 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'application des restrictions réglementaires avant utilisation.
Tekoči naftni proizvodi - Neosvinčeni motorni bencin - Določevanje organskih kisikovih spojin in celotnega organsko vezanega kisika s plinsko kromatografijo (O-FID)
Standard EN 1601 določa metodo plinske kromatografije za kvantitativno določevanje individualnih organskih kisikovih spojin v mejah od 0,17 % (m/m) do 15 % (m/m) z neposredno analizo (brez redčenja) in celotnega organsko vezanega kisika do 3,9 % (m/m) v neosvinčenem motornem bencinu, katerega končno vrelišče ne presega 220 °C. Na vzorcih, pri katerih je vsebnost ene kisikove spojine višja od 15 % (m/m), se pred analizo opravi proces redčenja.
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.NURPDWRJUDILMR2),'Flüssige Mineralölerzeugnisse - Unverbleite Ottokraftstoffe - Bestimmung sauerstoffhaltiger organischer Verbindungen und des Gesamtgehalts an organisch gebundenem Sauerstoff mittels Gaschromatographie (O-FID)Produit pétroliers liquides - Essence sans plomb - Détermination des composés oxygénés organiques et de la teneur totale en oxygène organiquement lié par chromatographie en phase gazeuse (O-FID)Liquid petroleum products - Unleaded petrol - Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography (O-FID)75.160.20Liquid fuels71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysisICS:Ta slovenski standard je istoveten z:EN 1601:2014SIST EN 1601:2014en,fr,de01-julij-2014SIST EN 1601:2014SLOVENSKI
STANDARDSIST EN 1601:19981DGRPHãþD
SIST EN 1601:2014
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 1601
April 2014 ICS 75.160.20 Supersedes EN 1601:1997English Version
Liquid petroleum products - Unleaded petrol - Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography (O-FID)
Produit pétroliers liquides - Essence sans plomb - Détermination des composés oxygénés organiques et de la teneur totale en oxygène organiquement lié par chromatographie en phase gazeuse (O-FID)
Flüssige Mineralölerzeugnisse - Unverbleite Ottokraftstoffe -Bestimmung sauerstoffhaltiger organischer Verbindungen und des Gesamtgehalts an organisch gebundenem Sauerstoff mittels Gaschromatographie (O-FID) This European Standard was approved by CEN on 18 January 2014.
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 © 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 1601:2014 ESIST EN 1601:2014
EN 1601:2014 (E) 2 Contents Foreword .3 1 Scope .4 2 Normative references .4 3 Principle .4 4 Reagents and materials .5 4.1 Gases .5 4.2 Reagents for the preparation of calibration samples .5 4.3 Internal standards .6 4.4 Oxygenate free petrol .6 5 Apparatus .6 5.1 Gas chromatographic assembly .6 5.2 Other equipment .7 6 Sampling .7 7 Procedure .8 7.1 Setting up the apparatus .8 7.2 Calibration .8 7.3 Determination of density of the sample .9 7.4 Preparation of test sample .9 7.5 Introduction of test portion .9 7.6 Examination of chromatogram .9 8 Calculation .9 8.1 Calculation of mass of each component in the test sample .9 8.2 Calculation of each component in the sample as a percentage by mass . 10 8.3 Calculation of each component in the sample as a percentage by volume . 10 9 Procedure for the determination of a higher oxygenate compound content . 11 9.1 General . 11 9.2 Dilution of the sample . 11 9.3 Preparation of the sample D for analysis . 12 9.4 Analysis of the test sample D . 12 9.5 Calculation and expression of results . 12 9.5.1 Calculation of the component of interest in the sample D as a percentage by mass . 12 9.5.2 Calculation of the component of interest in the test sample as a percentage by mass . 12 9.5.3 Calculation of the component of interest in the test sample as a percentage by volume . 12 10 Total organically bound oxygen content . 12 11 Expression of results . 13 12 Precision . 13 12.1 General . 13 12.2 Repeatability, r . 13 12.3 Reproducibility, R . 13 13 Test report . 14 Annex A (informative)
Guidance on the oxygen selective detection (O-FID) technique . 15 A.1 Description . 15 A.2 Summary of the analysis conditions . 16 Bibliography . 19
SIST EN 1601:2014
EN 1601:2014 (E) 3 Foreword This document (EN 1601:2014) 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 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 October 2014, and conflicting national standards shall be withdrawn at the latest by October 2014. 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 1601:1997. The major updates towards the former version are: — Inclusion of a dilution procedure to measure an oxygenate compound content higher than 15 % (m/m). In this procedure detailed in Clause 9, the sample is diluted (1:1 or 1:2 mass/mass) with an oxygenate free petrol, before the addition of the internal standard and the analysis. Precision data have not been evaluated for this procedure; — The previous precision data for oxygen content covered the range 1,5 % (m/m) to 3,0 % (m/m). The data precision for oxygen content has been updated for the range 2,1 % (m/m) to 3,9 % (m/m), based on Round Robins data from 2005 to 2011 available from DIN-FAM, Germany; — The scope of the test method has been updated to include petrol with higher total oxygen content and with higher oxygenate contents than mentioned in the former edition; the test method is now applicable for petrol (automotive motor gasoline) with a total oxygen content up to 3,9 % (m/m), and/or with an individual oxygenate compound content higher than 15 % (m/m). Such petrol is specified in EN 228 [1]. Precision data have not been evaluated for this procedure and consequently the previous precision data for a individual oxygenate compound content in the range of 0,17 % (m/m) higher thanto 15 % (m/m) have not been updated or extended above 15 % (m/m), in order to introduce for instance automotive ethanol (E85) fuel in the scope. — Deletion of the original Annex A on densities of oxygenate compounds and inclusion of some of them in Table 1; — Updated chromatograms and improved description of the gas chromatographic equipment with inclusion of a schematic instrument O-FID instrument configuration in the new Annex A. 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 1601:2014
EN 1601:2014 (E) 4 1 Scope This European Standard specifies a gas chromatographic method for the quantitative determination, in unleaded petrol having a final boiling point not greater than 220 °C, of individual organic oxygenate compounds in the range 0,17 % (m/m) to 15 % (m/m) in a direct analysis (without dilution), and total organically bound oxygen up to 3,9 % (m/m). For samples for which one of the oxygenate compounds content is higher than 15 % (m/m), a procedure with a dilution of the sample before the analysis is given. NOTE 1 Precision data are not available for an oxygenate compound content higher than 15 % (m/m); see Foreword. NOTE 2 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, 3. 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 European Standard to establish appropriate safety and health practices and 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 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 Principle After separation using a capillary column, the organic oxygenate compounds are selectively converted to carbon monoxide, hydrogen and carbon in a pyrolytic cracking reactor. In a hydrogenation reactor, carbon monoxide is then converted to methane and subsequently detected using a flame ionization detector (FID). NOTE Guidance on the oxygen selective detection (O-FID) technique is given in Annex A. SIST EN 1601:2014
EN 1601:2014 (E) 5 4 Reagents and materials 4.1 Gases 4.1.1 Carrier gas, helium, or nitrogen, free of hydrocarbons and oxygen and water. Few percentages of hydrogen (used as auxiliary gas) shall be mixed to the carrier gas (see Figure A.1). Hydrogen shall not be used as a carrier gas because it will interfere with the cracking reaction. IMPORTANT — It is important to minimize oxygen in the carrier gas. To reduce the background signal, it is essential to use oxygen and moisture filters. 4.1.2 Detector gases, hydrogen and air suitable for flame ionization detector. WARNING — Hydrogen is explosive when mixed with air at concentrations ranging approximately from 4 % (V/V) to 75 % (V/V). All joints and lines carrying hydrogen shall be made gas tight to prevent leakage of hydrogen into a confined space. 4.1.3 Cracking reactor gas, helium or nitrogen, used as purge gas to protect the platinum/rhodium element (see Figure A.1). 4.2 Reagents for the preparation of calibration samples Use only reagents of recognized analytical grade. Reagents shall be not less than 99,0 % (m/m) pure. Calibration samples should be combinations of the following reagents: 4.2.1 methanol (MeOH); 4.2.2 ethanol (EtOH); 4.2.3 propan-1-ol (NPA); 4.2.4 propan-2-ol (IPA); 4.2.5 butan-1-ol (NBA); 4.2.6 butan-2-ol (SBA); 4.2.7 2-methylpropan-2-ol (TBA); 4.2.8 2-methylpropan-1-ol (IBA); 4.2.9 pentan-2-ol (SAA); 4.2.10 tert-butyl methyl ether (MTBE); 4.2.11 methyl tert-pentyl ether (TAME); 4.2.12 Diisopropyl ether (DIPE); 4.2.13 tert-butyl ethyl ether (ETBE); 4.2.14 butan-2-one (MEK); 4.2.15 acetone. SIST EN 1601:2014
EN 1601:2014 (E) 6 4.3 Internal standards Use one of the reagents listed in 4.2. If all of these reagents are likely to be present in the sample under test, use a different organic oxygenate compound of the same purity. The internal standard of choice shall elute at a different retention time as components present in the test sample. 4.4 Oxygenate free petrol Petrol examined to ensure that it contains no organic oxygenate compounds detectable by this test method. Cool the oxygenate free petrol to between 5 °C and 10 °C before the preparation of the calibration samples and test samples. 5 Apparatus 5.1 Gas chromatographic assembly 5.1.1 Gas chromatograph, equipped with a variable split flow injector, an oxygen selective detection system (O-FID), and computer-controlled or other system permitting the recording of chromatograms and execution of quantitative calculations. A typical O-FID instrument configuration is given in Annex A. 5.1.2 Columns, the separation column shall
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