SIST EN ISO 20846:2004
(Main)Petroleum products - Determination of sulfur content of automotive fuels - Ultraviolet fluorescence method (ISO 20846:2004)
Petroleum products - Determination of sulfur content of automotive fuels - Ultraviolet fluorescence method (ISO 20846:2004)
Determination of total sulfur content of liquid hydrocarbons boiling in the range of 25 °C to 400 °C and with viscosities in the range of 0,2 mm2/s to 10 mm2/s at room temperature.
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes von Kraftstoffen für Kraftfahrzeuge - Ultraviolettfluoreszenz-Verfahren (ISO 20846:2004)
Diese Internationale Norm legt ein Verfahren zur Bestimmung des Schwefelgehaltes von Ottokraftstoffen, die bis zu 2,7 % (m/m) Sauerstoff enthalten können, und von Dieselkraftstoffen, die bis zu 5 % (V/V) Fettsäuremethylester (FAME) enthalten können, fest. Das Verfahren kann für Schwefelanteile im Bereich von 3 mg/kg bis 500 mg/kg angewendet werden. Andere Erzeugnisse mit anderen Schwefelgehalten können mit diesem Verfahren untersucht werden, jedoch wurden die in dieser Internationalen Norm angegebenen Präzisionsangaben nur für Kraftstoffe für Kraftfahrzeuge für den angegebenen Bereich ermittelt. Halogene stören die Bestimmung bei Konzentrationen von mehr als ungefähr 3 500 mg/kg.
ANMERKUNG 1 Einige der in Raffinerieprozessen der Erdöl- und chemischen Industrie verwendeten Katalysatoren können vergiftet werden, wenn in den Einsatzprodukten Spuren von schwefelhaltigen Substanzen enthalten sind.
ANMERKUNG 2 Dieses Prüfverfahren kann zur Bestimmung von Schwefel in Raffinerie-Zwischenprodukten und auch zur Kontrolle von Schwefel in Endprodukten verwendet werden.
ANMERKUNG 3 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.
Produits pétroliers - Détermination de la teneur en soufre des carburants pour automobiles - Méthode par fluorescence ultraviolette (ISO 20846:2004)
L'ISO 20846:2004 spécifie une méthode par fluorescence ultraviolette (UV) pour le dosage du soufre dans les essences pour automobiles, y compris celles contenant jusqu'à 2,7 % (m/m) en oxygène, et les carburants diesels (gazoles), y compris ceux contenant jusqu'à 5 % (V/V) d'esters méthyliques d'acide gras (EMAG), dont les teneurs en soufre se trouvent dans le domaine 3 mg/kg à 500 mg/kg. D'autres produits peuvent être analysés et d'autres teneurs en soufre peuvent être déterminées suivant cette méthode; cependant, il n'a pas été établi de données de fidélité pour des produits autres que les carburants pour automobiles et pour des résultats en dehors de la gamme spécifiée pour l'ISO 20846:2004. Les halogènes, à des concentrations supérieures à environ 3 500 mg/kg, interfèrent.
Certains catalyseurs utilisés dans le raffinage chimique et pétrolier peuvent être pollués lorsque des composés soufrés sont présents en trace dans les charges; cette méthode peut être utilisée pour déterminer la teneur en soufre des charges et peut aussi être utilisée pour contrôler la teneur en soufre des effluents.
Naftni proizvodi - Določevanje žvepla v gorivih za motorna vozila - Ultravijolična fluorescenčna metoda (ISO 20846:2004)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 20846:2004
01-september-2004
1DIWQLSURL]YRGL'RORþHYDQMHåYHSODYJRULYLK]DPRWRUQDYR]LOD8OWUDYLMROLþQD
IOXRUHVFHQþQDPHWRGD ,62
Petroleum products - Determination of sulfur content of automotive fuels - Ultraviolet
fluorescence method (ISO 20846:2004)
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes von Kraftstoffen für
Kraftfahrzeuge - Ultraviolettfluoreszenz-Verfahren (ISO 20846:2004)
Produits pétroliers - Détermination de la teneur en soufre des carburants pour
automobiles - Méthode par fluorescence ultraviolette (ISO 20846:2004)
Ta slovenski standard je istoveten z: EN ISO 20846:2004
ICS:
75.160.20 7HNRþDJRULYD Liquid fuels
SIST EN ISO 20846:2004 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 20846:2004
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SIST EN ISO 20846:2004
EUROPEAN STANDARD
EN ISO 20846
NORME EUROPÉENNE
EUROPÄISCHE NORM
March 2004
ICS 75.080; 75.160.30
English version
Petroleum products - Determination of sulfur content of
automotive fuels - Ultraviolet fluorescence method (ISO
20846:2004)
Produits pétroliers - Détermination de la teneur en soufre Mineralölerzeugnisse - Bestimmung des
des carburants pour automobiles - Méthode par Gesamtschwefelgehaltes von flüssigen
fluorescence ultraviolette (ISO 20846:2004) Mineralölerzeugnissen - Ultraviolettfluoreszenz-Verfahren
(ISO 20846:2004)
This European Standard was approved by CEN on 1 March 2004.
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 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 Management Centre has the same status as the official
versions.
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 STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2004 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 20846:2004 E
worldwide for CEN national Members.
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SIST EN ISO 20846:2004
EN ISO 20846:2004 (E)
Foreword
This document (EN ISO 20846:2004) has been prepared by Technical Committee ISO/TC 28
"Petroleum products and lubricants" in collaboration with 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 September 2004, and conflicting national
standards shall be withdrawn at the latest by September 2004.
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.
Endorsement notice
The text of ISO 20846:2004 has been approved by CEN as EN ISO 20846:2004 without any
modifications.
2
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SIST EN ISO 20846:2004
INTERNATIONAL ISO
STANDARD 20846
First edition
2004-03-15
Petroleum products — Determination of
sulfur content of automotive fuels —
Ultraviolet fluorescence method
Produits pétroliers — Détermination de la teneur en soufre des
carburants pour automobiles — Méthode par fluorescence ultraviolette
Reference number
ISO 20846:2004(E)
©
ISO 2004
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SIST EN ISO 20846:2004
ISO 20846:2004(E)
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ii © ISO 2004 – All rights reserved
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SIST EN ISO 20846:2004
ISO 20846:2004(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 Principle . 2
4 Reagents and materials. 2
5 Apparatus. 3
6 Sampling . 4
7 Apparatus preparation. 5
8 Apparatus calibration and verification . 5
9 Procedure. 8
10 Calculation. 8
11 Expression of results. 10
12 Precision . 10
13 Test report. 11
Bibliography . 12
© ISO 2004 – All rights reserved iii
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SIST EN ISO 20846:2004
ISO 20846:2004(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 20846 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants.
iv © ISO 2004 – All rights reserved
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SIST EN ISO 20846:2004
INTERNATIONAL STANDARD ISO 20846:2004(E)
Petroleum products — Determination of sulfur content of
automotive fuels — Ultraviolet fluorescence method
WARNING — The use of this International Standard may involve hazardous materials, operations and
equipment. This International Standard does not purport to address all of the safety problems
associated with its use. It is the responsibility of the user of this International Standard to establish
appropriate safety and health practices and determine the applicability of regulatory limitations prior
to use.
1 Scope
This International Standard specifies an ultraviolet (UV) fluorescence test method for the determination of the
sulfur content of motor gasolines, including those containing up to 2,7 % (m/m) oxygen, and of diesel fuels,
including those containing up to 5 % (V/V) fatty acid methyl ester (FAME), having sulfur contents in the range
3 mg/kg to 500 mg/kg. Other products may be analysed and other sulfur contents may be determined
according to this test method; however, no precision data for products other than automotive fuels and for
results outside the specified range have been established for this International Standard. Halogens interfere
with this detection technique at concentrations above approximately 3 500 mg/kg.
NOTE 1 Some process catalysts used in petroleum and chemical refining might be polluted when trace amounts of
sulfur-bearing materials are contained in the feedstocks.
NOTE 2 This test method may be used to determine sulfur in process feeds and may also be used to control sulfur in
effluents.
NOTE 3 For the purposes of this International Standard, the terms “% (m/m)” and “% (V/V)” are used to represent the
mass fraction and the volume fraction of a material respectively.
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.
ISO 1042:1998, Laboratory glassware — One-mark volumetric flasks
ISO 3170:2004, Petroleum liquids — Manual sampling
ISO 3171:1988, Petroleum liquids — Automatic pipeline sampling
ISO 3675:1998, Crude petroleum and liquid petroleum products — Laboratory determination of density —
Hydrometer method
ISO 12185:1996, Crude petroleum and petroleum products — Determination of density — Oscillating U-tube
method (including Technical Corrigendum 1:2001)
© ISO 2004 – All rights reserved 1
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SIST EN ISO 20846:2004
ISO 20846:2004(E)
3 Principle
A hydrocarbon 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 (SO )
2
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 SO absorbs the energy from the UV light and is
2
converted to excited sulfur dioxide (SO *). The fluorescence emitted from the excited SO * as it returns to a
2 2
stable state SO is detected by a photomultiplier tube and the resulting signal is a measure of the sulfur
2
contained in the sample.
4 Reagents and materials
4.1 Inert gas, argon or helium, of high purity grade with a minimum purity of 99,998 % (V/V).
4.2 Oxygen, of high purity grade with a minimum purity of 99,75 % (V/V).
CAUTION — Vigorously accelerates combustion.
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 Toluene, reagent grade.
4.3.3 Isooctane, reagent grade.
CAUTION — Flammable solvents.
4.4 Sulfur compounds
4.4.1 Compounds with a minimum purity of 99 % (m/m). Examples are given in 4.4.1.1 to 4.4.1.3. Where the
purity of these compounds is less than 99 % (m/m), the concentrations and nature of all impurities are to be
established.
NOTE 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 4.4.1.1 to 4.4.1.3.
4.4.1.1 Dibenzothiophene (DBT), of molecular mass 184,26 with a nominal sulfur content of
17,399 % (m/m).
4.4.1.2 Dibutyl sulfide (DBS), of molecular mass 146,29 with a nominal sulfur content of 21,915 % (m/m).
4.4.1.3 Thionaphthene (benzothiophene) (TNA), of molecular mass 134,20 with a nominal sulfur
content of 23,890 % (m/m).
2 © ISO 2004 – All rights reserved
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SIST EN ISO 20846:2004
ISO 20846:2004(E)
4.5 Sulfur stock solution
Prepare a stock solution of sulfur content approximately 1 000 mg/l 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 exact 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 4.4.1.1 to 4.4.1.3 to add to the 100 ml flask is
0,574 8 g (DBT), 0,456 3 g (DBS) or 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.
Calibration standards with a known sulfur concentration, in milligrams per litre (or content in 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 those mentioned above
avoid any density correction.
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 a 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 (SO ).
2
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.
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SIST EN ISO 20846:2004
ISO 20846:2004(E)
5.4 Vapour drier, capable of removing water vapour for
...
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