SIST EN 1601:2017

Liquid petroleum products - Determination of organic oxygenate compounds and total organically bound oxygen content in unleaded petrol - Method by gas chromatography (O-FID)

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.
The revision concerns updating the test method with data discussed in WG9 and comments received at formal vote.

Flüssige Mineralölerzeugnisse - Bestimmung sauerstoff-haltiger organischer Verbindungen und des Gesamtgehalts an organisch gebundenem Sauerstoff in Unverbleitem Ottokraftstoff - Methode mittels Gaschromatographie (O-FID)

Diese Europäische Norm legt ein direktes gaschromatographisches Analyseverfahren (ohne Verdünnung) zur quantitativen Bestimmung sauerstoffhaltiger Verbindungen im Bereich 0,17 % (m/m) bis 15 % (m/m) und des Gesamtgehalts 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 Verdünnung der Probe vor der Analyse beschrieben.
ANMERKUNG 1   Die Umwandlung von Massenprozent in Volumenprozent wird unter Anwendung der in 8.3 und 9.5.3 angegebenen Berechnung vorgenommen.
ANMERKUNG 2   Präzisionsdaten für einen höheren Gehalt an sauerstoffhaltigen Verbindungen als 15 % (m/m) sind nicht verfügbar (siehe Einleitung).
ANMERKUNG 3   Für den Zweck dieser Europäischen Norm werden Massenanteil, µ, bzw. Volumenanteil, φ, durch die Begriffe "% (m/m)" und "% (V/V)" ausgedrückt.
WARNUNG - Die Anwendung dieser Europäischen Norm kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Europäische 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 gewährleisten, und dafür Sorge zu tragen, dass behördliche und gesetzliche Maßnahmen eingehalten werden.

Produit pétroliers liquides - Détermination des composés oxygénés organiques et de la teneur totale en oxygène organiquement lié en essence sans plomb - Technique 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 individuels 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 l’un des composés oxygénés est supérieure à 15 % (m/m), une procédure de dilution de l’échantillon avant leur analyse est décrite.
NOTE 1   Les conversions des pourcentages massiques en pourcentages volumiques sont effectuées selon le calcul mentionné en 8.3 et 9.5.3.
NOTE 2   Les valeurs de fidélité ne sont pas disponibles pour des teneurs en composés oxygénés supérieures à
15 % (m/m) ; voir l’Introduction.
NOTE 3       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 œuvre. Il est de la responsabilité des utilisateurs de prendre les mesures appropriées qui assurent la sécurité et préservent la santé du personnel avant son application, et pour répondre aux exigences réglementaires et statutaires à cette fin.

Tekoči naftni proizvodi - Določevanje organskih kisikovih spojin in celotnega organsko vezanega kisika v neosvinčenem motornem bencinu - Metoda s plinsko kromatografijo (O-FID)

Ta evropski standard 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.
Revizija obravnava posodabljanje preskusne metode s podatki, obravnavanimi v WG9, in pripombami, prejetimi med uradnim glasovanjem.

General Information

• Status: Published
• Public Enquiry End Date: 02-Jun-2016
• Publication Date: 06-Sep-2017
• ICS: 71.040.50 - Physicochemical methods of analysis
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: NAD - Petroleum products, lubricants and related products
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 30-Aug-2017
• Due Date: 04-Nov-2017
• Completion Date: 07-Sep-2017
• Ref Project: EN 1601:2017 - Liquid petroleum products - Determination of organic oxygenate compounds and total organically bound oxygen content in unleaded petrol - Method by gas chromatography (O-FID)

Relations

• Replaces: SIST EN 1601:2014 - Liquid petroleum products - Unleaded petrol - Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography (O-FID)
• Effective Date: 01-Oct-2017
• Replaces: SIST EN 1601:2014/AC:2014 - Liquid petroleum products - Unleaded petrol - Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography (O-FID)
• Effective Date: 01-Oct-2017

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Flüssige Mineralölerzeugnisse - Bestimmung sauerstoff-haltiger organischer Verbindungen und des Gesamtgehalts an organisch gebundenem Sauerstoff in Unverbleitem Ottokraftstoff - Methode mittels Gaschromatographie (O-FID)Produit pétroliers liquides - Détermination des composés oxygénés organiques et de la teneur totale en oxygène organiquement lié en essence sans plomb - Technique par chromatographie en phase gazeuse (O-FID)Liquid petroleum products - Determination of organic oxygenate compounds and total organically bound oxygen content in unleaded petrol - Method by gas chromatography (O-FID)75.160.20Liquid fuels71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysisICS:Ta slovenski standard je istoveten z:EN 1601:2017SIST EN 1601:2017en,fr,de01-oktober-2017SIST EN 1601:2017SLOVENSKI
STANDARDSIST EN 1601:2014/AC:2014SIST EN 1601:20141DGRPHãþD



SIST EN 1601:2017



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 1601
August
t r s y ICS
y wä s x rä t r Supersedes EN
s x r sã t r s vEnglish Version
Liquid petroleum products æ Determination of organic oxygenate compounds and total organically bound oxygen content in unleaded petrol æ Method by gas Produits pétroliers liquides æ Détermination des composés oxygénés organiques et de la teneur totale en oxygène organiquement lié dans l 5essence sans plomb æ Méthode par chromatographie en phase
Flüssige Mineralölerzeugnisse æ Bestimmung sauerstoffhaltiger organischer Verbindungen und des Gesamtgehalts an organisch gebundenem Sauerstoff in unverbleitem Ottokraftstoff æ Methode mittels This European Standard was approved by CEN on
s { May
t r s yä
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 Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United 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 y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x r sã t r s y ESIST EN 1601:2017



EN 1601:2017 (E) 2 Contents Page European foreword . 3 Introduction . 4 1 Scope . 5 2 Normative references . 5 3 Principle . 5 4 Reagents and materials . 6 4.1 Gases . 6 4.2 Reagents for the preparation of calibration samples . 6 4.3 Internal standards . 7 4.4 Oxygenate free petrol . 7 5 Apparatus . 7 5.1 Gas chromatographic assembly . 7 5.2 Other equipment . 7 6 Sampling . 8 7 Procedure. 8 7.1 Setting up the apparatus. 8 7.2 Calibration . 9 7.3 Determination of density of the sample . 9 7.4 Preparation of the test sample . 9 7.5 Injection of the test portion . 10 7.6 Examination of the chromatogram . 10 8 Calculation . 10 8.1 Calculation of mass of each component in the test sample . 10 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. 11 9 Procedure for the determination of a higher oxygenate compound content . 12 9.1 General . 12 9.2 Dilution of the sample . 12 9.3 Preparation of the test sample D for analysis . 13 9.4 Analysis of the test sample D . 13 9.5 Calculation and expression of results . 13 10 Total organically bound oxygen content . 14 11 Expression of results . 14 12 Precision . 14 12.1 General . 14 12.2 Repeatability, r . 14 12.3 Reproducibility, R . 14 13 Test report . 15 Annex A (informative)
Guidance on the oxygen selective detection (O-FID) technique . 16 A.1 Description . 16 A.2 Summary of the analysis conditions . 17 Bibliography . 20 SIST EN 1601:2017



EN 1601:2017 (E) 3
European foreword This document (EN 1601:2017) 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 February 2018, and conflicting national standards shall be withdrawn at the latest by February 2018. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 1601:2014. Significant changes between this document and EN 1601:2014 include: — Improved description of the carrier gases, equipment and procedure for cooling the samples; — Expansion of Table 1 on the oxygenate compounds data, a.o. the addition of ETBE and TAEE; — Editorial changes in order to clarify the test procedure. 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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 1601:2017



EN 1601:2017 (E) 4 Introduction This European Standard is an update of the first edition (EN 1601:1997). 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]. The previous precision data for an individual oxygenate compound content in the range of 0,17 % (V/V) to 15 % (V/V) has not been updated or extended above 15 % (V/V). A dilution procedure to measure an oxygenate compound content higher than 15 % (m/m) is included in the standard. 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. SIST EN 1601:2017



EN 1601:2017 (E) 5 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 The conversion from percent mass to percent volume is done using the calculation mentioned in 8.3 and 9.5.3. NOTE 2 Precision data are not available for an oxygenate compound content higher than 15 % (m/m); see Introduction. NOTE 3 For the purposes of this European Standard, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass fraction, µ, respectively the volume fraction, . WARNING —The use of this European Standard can 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 users of this European 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 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 1601:2017



EN 1601:2017 (E) 6 4 Reagents and materials 4.1 Gases 4.1.1 Carrier gas, helium, or nitrogen, free of hydrocarbons and oxygen and water. Hydrogen shall be dosed exactly and mixed properly to the carrier gas to ensure a stable operation of the cracking reactor (see Figure A.1 and the recommendation in A.2). It is important to minimize the oxygen content of 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 4.2.1 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: 4.2.2 methanol (MeOH); 4.2.3 ethanol (EtOH); 4.2.4 propan-1-ol [n-propyl alcohol (NPA)]; 4.2.5 propan-2-ol [iso-propyl alcohol (IPA)]; 4.2.6 butan-1-ol [n-butyl alcohol (NBA)]; 4.2.7 butan-2-ol [s-butyl alcohol (SBA)]; 4.2.8 2-methylpropan-2-ol [tert-butyl alcohol (TBA)]; 4.2.9 2-methylpropan-1-ol [iso-butyl alcohol (IBA)]; 4.2.10 2-pentanol (SAA); 4.2.11 2-methoxy-2-methylpropane [Methyl tert-butyl ether (MTBE)]; 4.2.12 2-methoxy-2-methylbutane [tert-Amyl methyl ether (TAME)]; 4.2.13 2-Isopropoxypropane [Diisopropyl ether (DIPE)]; 4.2.14 2-Ethoxy-2-methyl-propane [Ethyl tert-butyl ether (ETBE)]; 4.2.15 2-Ethoxy-2-methylbutane [tert-Amyl ethyl ether (TAEE)]; 4.2.16 butan-2-one [methyl-ethyl ketone (MEK)]; SIST EN 1601:2017



EN 1601:2017 (E) 7 4.2.17 acetone [dimethyl ketone (DMK)]. 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 oxygenate compounds detectable by this test method. Cool the oxygenate free petrol to between 0 °C and 5 °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
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