Ethanol as a blending component for petrol - Determination of sulfur content - Ultraviolet fluorescence method

This document specifies an ultraviolet (UV) fluorescence test method for the determination of the sulfur content of ethanol from 5 mg/kg to 20 mg/kg. Other products may be analysed and higher sulfur contents may be determined according to this test method, however, no precision data for products other than ethanol and for results outside the specified range have been established for this document. Halogens interfere with this detection technique at concentrations above approximately 3 500 mg/kg.
NOTE   For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent the mass fraction and the volume fraction of a material respectively.
WARNING — The use of this standard may 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 the user of this standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use.

Ethanol zur Verwendung als Blendkomponente in Ottokraftstoff - Bestimmung des Schwefelgehaltes - Ultraviolettfloureszenz-Verfahren

Diese Internationale Norm legt ein Ultraviolett(UV-)fluoreszenz-Verfahren zur Bestimmung des Schwefelgehaltes in Ethanol im Bereich von 5 mg/kg bis 20 mg/kg fest. Andere Erzeugnisse sowie andere Schwefelgehalte können mit diesem Verfahren untersucht werden, jedoch gelten die in dieser Norm getroffenen Präzisionsangaben nicht für andere Erzeugnisse als Ethanol und auch nicht für andere als die angegebenen. Halogene stören die Bestimmung bei Konzentrationen von mehr als ungefähr 3 500 mg/kg.
ANMERKUNG    Für die Zwecke der vorliegenden Internationalen Norm werden die Bezeichnungen % (m/m) und % (V/V) für den Massenanteil in Prozent und für den Volumenanteil in Prozent verwendet.

Ethanol comme base de mélange a l'essence - Dosage du soufre - Méthode par fluorescence ultraviolette

La présente Norme européenne spécifie une méthode d’essai par fluorescence ultraviolette (UV) servant à doser le soufre dans l’éthanol entre 5 mg/kg et 20 mg/kg. Il est possible d’analyser d’autres produits et de déterminer des teneurs en soufre plus élevées grâce à cette méthode, mais aucune donnée de fidélité pour des produits autres que l’éthanol et pour des résultats hors de la plage spécifiée n’a été établie pour la présente Norme européenne. Les halogènes à des concentrations supérieures à 3 500 mg/kg environ perturbent cette technique de détection.
NOTE   Pour les besoins de la présente Norme internationale, les termes « % (m/m)” et “% (V/V) » sont utilisés pour représenter respectivement la fraction massique et la fraction volumique d’un produit.
AVERTISSEMENT – 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.

Etanol kot komponenta za dodajanje motornemu bencinu – Določevanje vsebnosti žvepla - Ultravijolična fluorescenčna metoda

General Information

Status
Published
Publication Date
24-Oct-2007
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
04-Oct-2007
Due Date
09-Dec-2007
Completion Date
25-Oct-2007

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Ethanol as a blending component for petrol - Determination of sulfur content - Ultraviolet fluorescence methodMHEthanol comme base de mélange a l'essence - Dosage du soufre - Méthode par fluorescence ultravioletteEthanol zur Verwendung als Blendkomponente in Ottokraftstoff - Bestimmung des Schwefelgehaltes - Ultraviolettfloureszenz-VerfahrenTa slovenski standard je istoveten z:EN 15486:2007SIST EN 15486:2007en75.160.20Liquid fuels71.080.60Alkoholi. EtriAlcohols. EthersICS:SLOVENSKI

STANDARDSIST EN 15486:200701-december-2007

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15486August 2007ICS 71.080.60 English VersionEthanol as a blending component for petrol - Determination ofsulfur content - Ultraviolet fluorescence methodEthanol comme base de mélange à l'essence - Dosage dusoufre - Méthode par fluorescence ultravioletteEthanol zur Verwendung als Blendkomponente inOttokraftstoff - Bestimmung des Schwefelgehaltes -Ultraviolettfluoreszenz-VerfahrenThis European Standard was approved by CEN on 30 June 2007.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 CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, 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© 2007 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15486:2007: E

EN 15486:2007 (E) 2 Contents Page Foreword..............................................................................................................................................................3 1 Scope......................................................................................................................................................4 2 Normative references............................................................................................................................4 3 Principle..................................................................................................................................................4 4 Reagents and materials........................................................................................................................4 4.1 Inert gas..................................................................................................................................................4 4.2 Oxygen....................................................................................................................................................4 4.3 Solvent....................................................................................................................................................5 4.4 Sulfur compounds.................................................................................................................................5 4.4.1 General....................................................................................................................................................5 4.5 Sulfur stock solution.............................................................................................................................5 4.6 Calibration standards............................................................................................................................5 4.7 Quality control samples........................................................................................................................6 4.8 Quartz wool............................................................................................................................................6 5 Apparatus...............................................................................................................................................6 6 Sampling.................................................................................................................................................7 7 Apparatus preparation..........................................................................................................................7 8 Apparatus calibration and verification................................................................................................8 8.1 Multi-point calibration...........................................................................................................................8 8.2 One-point calibration.............................................................................................................................9 8.3 Verification...........................................................................................................................................10 9 Procedure.............................................................................................................................................10 10 Calculation............................................................................................................................................11 10.1 Using multi-point calibration..............................................................................................................11 10.2 Using one-point calibration................................................................................................................11 10.3 Calculation............................................................................................................................................12 11 Expression of results..........................................................................................................................12 12 Precision...............................................................................................................................................12 12.1 Repeatability, r.....................................................................................................................................12 12.2 Reproducibility, R................................................................................................................................13 13 Test report............................................................................................................................................13 Annex A (normative)

Ethanol density.............................................................................................................14

EN 15486:2007 (E) 3 Foreword This document (EN 15486:2007) 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 2008, and conflicting national standards shall be withdrawn at the latest by February 2008. The method described in this document is based on EN ISO 20846 [1]. 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EN 15486:2007 (E) 4 1 Scope This document specifies an ultraviolet (UV) fluorescence test method for the determination of the sulfur content of ethanol from 5 mg/kg to 20 mg/kg. Other products may be analysed and higher sulfur contents may be determined according to this test method, however, no precision data for products other than ethanol and for results outside the specified range have been established for this document. Halogens interfere with this detection technique at concentrations above approximately 3 500 mg/kg. NOTE For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent the mass fraction and the volume fraction of a material respectively. WARNING — The use of this standard may 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 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 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 ISO 1042, Laboratory glassware – one-mark volumetric flasks (ISO 1042:1998) EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170:2004) 3 Principle An ethanol sample is directly injected into a UV fluorescence detector. The sample enters into a high temperature combustion tube (1 000 °C to 1 100 °C), where the sulfur is oxidized to sulfur dioxide (SO2) in an oxygen-rich atmosphere. Water produced during the sample combustion is removed and the sample combustion gases are exposed to ultraviolet (UV) light. The SO2 absorbs the energy from the UV light and is converted to excited sulfur dioxide (SO2*). The fluorescence emitted from the excited SO2* as it returns to a stable state SO2, is detected by a photomultiplier tube and the resulting signal is a measure of the sulfur contained in the sample. CAUTION — Exposure to excessive quantities of ultraviolet (UV) light is injurious to health. The operator must avoid exposing any part of his/her person, especially his/her eyes, to not only direct UV light but also to secondary or scattered radiation that may be present. 4 Reagents and materials 4.1 Inert gas Argon or helium, high purity grade with a minimum purity of 99,998 % (V/V). 4.2 Oxygen High purity grade with a minimum purity of 99,75 % (V/V). CAUTION — Vigorously accelerates combustion.

EN 15486:2007 (E) 5 4.3 Solvent 4.3.1 General Use either the solvent specified in 4.3.2 or 4.3.3 or a solvent similar to that occurring in the sample under analysis. Correction for sulfur contribution from solvents used in standard preparation and sample dilution is required. Alternatively, use of a solvent with non-detectable sulfur contamination relative to the unknown sample makes the blank correction unnecessary. 4.3.2 Ethanol, reagent grade. 4.3.3 Toluene, (optional), reagent grade. CAUTION — Flammable solvents. 4.4 Sulfur compounds 4.4.1 General Use compounds with a minimum purity of 99 % (m/m). Certified reference materials (CRMs) from accredited suppliers are suitable alternatives to the compounds listed in 4.4.2 to 4.4.4. 4.4.2 Dibenzothiophene (DBT), MW 184,26 g/mol with a nominal sulfur content of 17,399 % (m/m). 4.4.3 Dibutylsulfide (DBS), MW 146,29 g/mol with a nominal sulfur content of 21,915 % (m/m). 4.4.4 Thionaphthene (Benzothiophene) (TNA), MW 134,20 g/mol with a nominal sulfur content of 23,890 % (m/m). 4.5 Sulfur stock solution Prepare a stock solution of approximately 1 000 mg/l sulfur content by accurately weighing the appropriate quantity of sulfur compound (4.4) in a volumetric flask (5.9). Ensure complete dissolution with solvent (4.3). Calculate the sulfur concentration of the stock solution to the nearest 1 mg/l. This stock solution is used for the preparation of calibration standards.

As an alternative procedure, a sulfur stock solution of approximately 1 000 mg/kg can be prepared by accurately weighing the appropriate quantity of sulfur compound (4.4) in a volumetric flask (5.9) and reweighing the volumetric flask once it has been filled to the mark with the solvent (4.3).

Take precautions to ensure that evaporation of the solvent and/or sulfur compounds is not causing weighing errors. NOTE 1 The appropriate mass of sulfur compound described in 4.4.2 to 4.4.4 to add to the 100 ml flask is 0,574 8 g (DBT), 0,456 3 g (DBS) and 0,418 6 g (TNA). NOTE 2 The shelf life of the stock solution is approximately three months when stored at low temperature, typically in a refrigerator. 4.6 Calibration standards Prepare the calibration standards by dilution of the stock solution (4.5) with the selected solvent (4.3). Calculate the exact sulfur content of each calibration standard.

EN 15486:2007 (E) 6 Calibration standards with a known sulfur content in milligrams per litre (or milligrams per kilogram) can be obtained with a volume/volume (or mass/mass, respectively) dilution of the stock solution at 1 000 mg/l (or milligrams per kilogram, respectively). Other practices are possible but these ones above avoid any density correction. NOTE New calibration standards should be prepared on a regular basis depending upon the frequency of use and age. When stored at low temperature, typically in a refrigerator, the calibration standards, with sulfur content above 30 mg/kg (or mg/l), have a useful life of at least one month. Below this sulfur content (30 mg/kg), the shelf life should be reduced. 4.7 Quality control samples These are stable samples representative of the materials being analysed, that have a sulfur content that is known by this test method over a substantial period of time. Alternatively, there are standard materials with a certified value commercially available. Ensure before use, that the material is within its shelf life. 4.8 Quartz wool Follow the manufacturer's recommendations. 5 Apparatus 5.1 Furnace, comprising an electric device, capable of maintaining a temperature sufficient to pyrolyse all of the sample and oxidize all sulfur to sulfur dioxide (SO2). It can be set either in a horizontal or vertical position. 5.2 Combustion tube, of quartz, constructed to allow the direct injection of the sample into the heated oxidation zone of the furnace (5.1). The combustion tube shall have side arms for the introduction of oxygen and carrier gas. The oxidation section shall be large enough to ensure complete combustion of the sample. It can be set either in a horizontal or vertical position. 5.3 Flow controllers, capable of maintaining a constant supply of oxygen and carrier gas. 5.4 Vapour drier, capable of removing water vapour formed during combustion prior to measurement by the detector (5.5). 5.5 UV fluorescence detector, a selective and quantitative detector capable of measuring UV light emitted from the fluorescence of excited sulfur dioxide. 5.6 Microlitre syringe, capable of accurately delivering between 5 µl to 50 µl quantities. Follow the manufacturer’s instructions for determining the length of the needle

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