Liquid petroleum products - Determination of the sulfur content in Ethanol (E85) automotive fuel - Wavelength dispersive X-ray fluorescence spectrometric method

This European Standard specifies a wavelength-dispersive X-ray fluorescence (WDXRF) test method for
the determination of the sulfur content in ethanol (E85) automotive fuel [3], containing ethanol
between 50 % (V/V) and 85 % (V/V), from 5 mg/kg to 20 mg/kg, using instruments with either
monochromatic or polychromatic excitation.
NOTE 1 Sulfur contents higher than 20 mg/kg can be determined after sample dilution with an appropriate
solvent. However, the precision was not established for diluted samples.
NOTE 2 For the purposes of this European Standard, the terms “% (m/m)” and “% (V/V)” are used to represent
the mass fraction (μ) and the volume fraction (φ) of a material respectively.
WARNING — The use of this Standard can 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 users of this 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.

Flüssige Mineralölerzeugnisse - Bestimmung des Schwefelgehalts in Ethanolkraftstoff (E85) - Wellenlängendispersives Röntgenfluoreszenz-Spektrometrie-Verfahren

Diese Europäische Norm legt ein wellenlängendispersives Röntgenfluoreszenz-Prüfverfahren (en: wavelength-dispersive X-ray fluorescence, WDXRF) zur Bestimmung des Schwefelgehalts von 5 mg/kg bis 20 mg/kg in Ethanolkraftstoff (E85) [3], mit einem Ethanolgehalt von 50 % (V/V) bis 85 % (V/V), unter Verwendung von Instrumenten mit entweder monochromatischen oder mit polychromatischen Anregungsbedingungen, fest.
ANMERKUNG 1   Schwefelgehalte über 20 mg/kg können nach Probenverdünnung, mit einem geeigneten Lösungsmittel, bestimmt werden. Die Präzision wurde aber nicht für verdünnte Proben nachgewiesen.
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 die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Diese Norm beansprucht nicht, alle damit verbundenen Sicherheits¬probleme 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 ergreifen, und dafür Sorge zu tragen, dass behördliche und gesetzliche Maßnahmen eingehalten werden.

Produits pétroliers liquides - Détermination de la teneur en soufre dans le carburant éthanol pour automobiles (E85) - Méthode spectrométrique par fluorescence de rayons X dispersive en longueur d'onde

La présente Norme européenne spécifie une méthode d'essai par fluorescence de rayons X dispersive en longueur d'onde (FXDLO) pour le dosage du soufre dans le carburant pour automobiles Ethanol (E85) [3], dont la teneur en éthanol est comprise entre 50 et 85 % (V/V) pour des teneurs comprises entre 5 mg/kg et 20 mg/kg, à l'aide d’appareils avec excitation monochromatique ou polychromatique.
NOTE 1   Des teneurs en soufre supérieures à 20 mg/kg peuvent être déterminées après dilution de l’échantillon avec un solvant approprié mais la fidélité n’a pas été établie pour des échantillons dilués.
NOTE 2    Pour les besoins de la présente Norme européenne, les termes « % (m/m) » et « % (V/V) » sont utilisés pour représenter les fractions massique (µ) et volumique (φ) des produits, respectivement.
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 des utilisateurs de cette norme de prendre les mesures appropriées pour assurer la sécurité et préserver la santé du personnel avant son application, et pour répondre aux exigences réglementaires et statutaires à cette fin.

Tekoči naftni proizvodi - Določevanje žvepla v motornem gorivu etanol (E85) - Metoda z valovno-disperzno rentgensko fluorescenčno spektrometrijo

Ta evropski standard določa preskusno metodo z valovno-disperzno rentgensko fluorescenčno spektrometrijo (WDXRF) za določevanje vsebnosti žvepla v avtomobilskem gorivu etanol (E85) [3], ki vsebuje etanol 50–85 % (V/V) pri 5–20 mg/kg, z uporabo instrumentov z monokromatskim ali polikromatskim vzbujanjem.
OPOMBA 1 Vsebnost žvepla nad 20 mg/kg je mogoče določiti po redčenju vzorca z ustreznim
topilom. Kljub temu natančnost ni bila določena za razredčene vzorce.
OPOMBA 2 Za namene tega evropskega standarda izraza »% (m/m)« in »% (V/V)« predstavljata masni delež (µ) oziroma prostornino (φ) materiala.
OPOZORILO – Pri uporabi tega standarda so lahko prisotni nevarni materiali, postopki in oprema. Ta standard ne obravnava vseh varnostnih težav, ki se nanašajo na njegovo uporabo. Za sprejetje ustreznih ukrepov za zagotavljanje varnosti in zdravja osebja pred uporabo standarda ter izpolnjevanje zakonskih in regulativnih zahtev za ta namen so odgovorni uporabniki tega standarda.

General Information

Status
Published
Public Enquiry End Date
04-May-2016
Publication Date
06-Sep-2017
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
30-Aug-2017
Due Date
04-Nov-2017
Completion Date
07-Sep-2017

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.RFlüssige Mineralölerzeugnisse - Bestimmung des Schwefelgehalts in Ethanolkraftstoff (E85) - Wellenlängendispersives Röntgenfluoreszenz-Spektrometrie-VerfahrenProduits pétroliers liquides - Détermination de la teneur en soufre dans le carburant éthanol pour automobiles (E85) - Méthode spectrométrique par fluorescence de rayons X dispersive en longueur d'ondeLiquid petroleum products - Determination of the sulfur content in Ethanol (E85) automotive fuel - Wavelength dispersive X-ray fluorescence spectrometric method75.160.20Liquid fuels71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysisICS:Ta slovenski standard je istoveten z:EN 16997:2017SIST EN 16997:2017en,fr,de01-oktober-2017SIST EN 16997:2017SLOVENSKI

STANDARD
SIST EN 16997:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16997
August
t r s y ICS
y wä s x rä t r English Version

Liquid petroleum products æ Determination of the sulfur dispersive Xæray fluorescence spectrometric method Produits pétroliers liquides æ Détermination de la teneur en soufre dans le carburant éthanol pour fluorescence de rayons X dispersive en longueur d 5onde

Flüssige Mineralölerzeugnisse æ Bestimmung des Wellenlängendispersives RöntgenfluoreszenzæSpektrometrieæVerfahren This European Standard was approved by CEN on

s t June
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

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 { { yã t r s y ESIST EN 16997:2017

EN 16997:2017 (E) 2 Contents Page European foreword ....................................................................................................................................................... 3 1 Scope .................................................................................................................................................................... 4 2 Normative references .................................................................................................................................... 4 3 Principle ............................................................................................................................................................. 4 4 Reagents and materials ................................................................................................................................. 4 5 Apparatus ........................................................................................................................................................... 5 6 Sampling ............................................................................................................................................................. 5 7 Preparation of calibration solutions ........................................................................................................ 6 7.1 Interferences .................................................................................................................................................... 6 7.1.1 Background ....................................................................................................................................................... 6 7.1.2 FP-Method .......................................................................................................................................................... 7 7.1.3 Correction table ............................................................................................................................................... 7 7.2 Blank calibration solution ........................................................................................................................... 7 7.3 Stock solution ................................................................................................................................................... 7 7.4 Calibration solutions ...................................................................................................................................... 7 7.5 Storage and stability of the calibration solutions ............................................................................... 7 8 Settings ................................................................................................................................................................ 8 8.1 Measuring parameters .................................................................................................................................. 8 8.2 Optimization ..................................................................................................................................................... 8 8.2.1 Monochromatic excitation ........................................................................................................................... 8 8.2.2 Polychromatic excitation ............................................................................................................................. 8 8.3 Performance check of the spectrometer ................................................................................................ 8 9 Calibration ......................................................................................................................................................... 8 9.1 General ................................................................................................................................................................ 8 9.2 Calibration solutions ...................................................................................................................................... 8 9.3 Calibration curves ........................................................................................................................................... 9 9.3.1 Calibration without matrix correction .................................................................................................... 9 9.3.2 Calibration with matrix correction ........................................................................................................... 9 9.4 Checking .......................................................................................................................................................... 10 10 Procedure........................................................................................................................................................ 10 11 Expression of results ................................................................................................................................... 11 12 Precision .......................................................................................................................................................... 11 12.1 Repeatability .................................................................................................................................................. 11 12.2 Reproducibility ............................................................................................................................................. 11 13 Test report ...................................................................................................................................................... 12 Annex A (informative)

Fundamental parameters method background ............................................... 13 Bibliography ................................................................................................................................................................. 14

SIST EN 16997:2017

EN 16997:2017 (E) 3 European foreword This document (EN 16997:2017) 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. The methodology described in this document is based on EN ISO 20884 [1] and EN 15485 [2]. 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 16997:2017

EN 16997:2017 (E) 4 1 Scope This European Standard specifies a wavelength-dispersive X-ray fluorescence (WDXRF) test method for the determination of the sulfur content in ethanol (E85) automotive fuel [3], containing ethanol between 50 % (V/V) and 85 % (V/V), from 5 mg/kg to 20 mg/kg, using instruments with either monochromatic or polychromatic excitation. NOTE 1 Sulfur contents higher than 20 mg/kg can be determined after sample dilution with an appropriate solvent. However, the precision was not established for diluted samples. NOTE 2 For the purposes of this European Standard, the terms “% (m/m)” and “% (V/V)” are used to represent the mass fraction (µ) and the volume fraction () of a material respectively. WARNING — The use of this Standard can 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 users of this 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 22854, Liquid petroleum products - Determination of hydrocarbon types and oxygenates in automotive-motor gasoline and in ethanol (E85) automotive fuel - Multidimensional gas chromatography method (ISO 22854) 3 Principle The sample under analysis is exposed in a sample cell to the primary radiation of an X-ray tube. The count rates of the S K-L2,3. X-ray fluorescence and the count rate of the background radiation are measured. The correlation between the pulse rate and the concentration is calculated by software. The matrix effects are compensated either on the basis of fundamental parameters or using a correction table. The sulfur content is then determined using this calibration. 4 Reagents and materials 4.1 General Compounds with a minimum purity of 99 % (m/m) as in 4.2 to 4.4. Where the purity of these compounds is less than 99 % (m/m), the concentrations and nature of all impurities shall be established. A correction for chemical impurity may be applied when the sulfur content is known with accuracy. Certified reference materials (CRMs) from accredited suppliers are suitable alternatives to the compounds listed in 4.2 to 4.4. 4.2 Dibutylsulfide, of nominal sulfur content 21,92 % (m/m), or dibutyldisulfide, of nominal sulfur content 35,95 % (m/m), used as a calibrating substance for sulfur. SIST EN 16997:2017

EN 16997:2017 (E) 5 4.3 Ethanol absolute, of a purity not less than 99 %, for use as a compound of the blank solution (7.2), high purity grade, with a sulfur content < 1 mg/kg. Check the blank solution (7.2) prior to use with the spectrometer (5.1). A signal for sulfur shall not be detectable. 4.4 n-Heptane, of a purity not less than 99 %, for use as a compound of the blank solution (7.2), high purity grade, with a sulfur content < 1 mg/kg. Check the blank solution (7.2) prior to use with the spectrometer (5.2). A signal for sulfur shall not be detectable. 5 Apparatus 5.1 Software to set up a calibration and for the application to the fundamental parameter method of calculating the corresponding correction factor for the varying ethanol content in the sample in the calibration and the in use of such a calibration during the evaluation of samples. The software can be part of the device software, separate software is also possible. If software for the application of the fundamental parameter method isn’t available, the correction table (Table 3) may be used. The correction factors of Table 3 are only applicable for monochromatic excitation. 5.2 Wavelength-dispersive X-ray fluorescence spectrometer, with the capability for measuring the count rates of the S K-L2,3 X-ray fluorescence radiation and the background radiation. Due to the inherently low background radiation produced by instruments utilizing monochromatic radiation for excitation, it is not mandatory to measure the background radiation when this type of instrument is used. The minimum requirements for the spectrometer are given in Table 1. 5.3 Analytical balance, capable of weighing to the nearest 0,1 mg. 6 Sampling Unless otherwise specified, laboratory samples shall be obtained by the procedures described in EN ISO 3170 or EN ISO 3171. Samples should be analysed as soon as possible after removal from bulk supplies to prevent loss of sulfur. Thoroughly mix samples in their containers prior to withdrawal of the test portions. IMPORTANT — Particular attention should be paid to avoid contamination of sampling bottles from phosphorus containing detergents and thus to prevent the risk of interference with sulfur. SIST EN 16997:2017

EN 16997:2017 (E) 6 Table 1 — Spectrometer requirements Component Polychromatic excitation Monochromatic excitation Anode Rhodium, scandium or chromium Rhodium, scandium, chromium or titanium Voltagea No less than 30 kV (S) No less than 50 kV (Compton) No less than 30 kV Currenta No less than 33 mA (S) No less than 20 mA (Compton) No less than 0,1 mA Collimator or optic Coarse collimator Monochromator Analysing crystal Germanium, pentaerythrite or graphite LIF200 for Rh (Compton) Germanium, pentaerythrite or graphite Optical pathb Vacuum or helium Vacuum or helium Sample cup windowc Polyester film, 4 µm maximum Polyester film, 4 µm maximum Detector Proportional counter with pulse-height analyser (S) Scintillation counter with pulse-height analyser (Compton) Proportional counter with single channel analyser Wavelengths S K-L2,3 at 0,537 3 nm Background radiation at 0,545 nm Tube anode element’s Compton signal d S K-L2,3 at 0,537 3 nm a Lower-power systems may be used, provided they have been validated to meet the precision requirements specified in Clause 12. b In instruments using vacuum, the sample is not exposed directly to the vacuum of the optical path, but is separated by a secondary window. Helium, minimum purity 99,9 %. c Polyester film is the preferred choice as samples of very high aromatic content may dissolve polycarbonate film. There are possibly trace amounts of silicon, calcium and sulfur in some types of film. However, the effects should be cancelled out when samples and standards are analysed using the same batch of film. It is important that samples, standards and blanks be measured using the same batch of film to avoid bias. Other sample window materials with the same or better absorptivity, p

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