SIST EN ISO 20846:2019
(Main)Petroleum products - Determination of sulfur content of automotive fuels - Ultraviolet fluorescence method (ISO 20846:2019)
Petroleum products - Determination of sulfur content of automotive fuels - Ultraviolet fluorescence method (ISO 20846:2019)
This document specifies an ultraviolet (UV) fluorescence test method for the determination of the sulfur content of the following products: - having sulfur contents in the range 3 mg/kg to 500 mg/ kg, - motor gasolines containing up to 3,7 % (m/m) oxygen [including those blended with ethanol up to about 10 % (V/V)], - diesel fuels, including those containing up to about 30 % (V/V) fatty acid methyl ester (FAME), - having sulfur contents in the range of 3 mg/kg to 45 mg/kg, - synthetic fuels, such as hydrotreated vegetable oil (HVO) and gas to liquid (GTL). Other products can be analysed and other sulfur contents can 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 document. Halogens interfere with this detection technique at concentrations above approximately 3 500 mg/kg.
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes von Kraftstoffen - Ultraviolettfluoreszenz-Verfahren (ISO 20846:2019)
Dieses Dokument enthält Festlegungen an ein Ultraviolettfluoreszenz Verfahren zur Bestimmung des Schwefelgehaltes von folgenden Erzeugnissen:
— mit einem Schwefelgehalt im Bereich von 3 mg/kg bis 500 mg/kg;
— Ottokraftstoffe, die bis 3,7 % (m/m) Sauerstoff (einschließlich solcher mit einem Gehalt bis 10 % (V/V) Ethanol) enthalten;
— Dieselkraftstoffe, die bis 30 % (V/V) Fettsäuremethylester (FAME) enthalten;
— mit einem Schwefelgehalt im Bereich von 3 mg/kg bis 45 mg/kg;
— synthetische Kraftstoffe, z. B. hydrogeniertem Pflanzenöl (HVO) und Gas to Liquid (GTL).
Andere Erzeugnisse und andere Schwefelgehalte können mit diesem Verfahren untersucht werden, jedoch wurden die in diesem Dokument angegebenen Präzisionsangaben nur für Kraftstoffe für Kraftfahrzeuge für den angegebenen Bereich ermittelt. Halogene stören die Bestimmung bei Konzentrationen oberhalb von etwa 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 dieses Dokuments wird zur Angabe des Massenanteils, w, einer Substanz „% (m/m)“ und für den Volumenanteil, φ, einer Substanz der Ausdruck „% (V/V)“ verwendet.
ANMERKUNG 4 Sulfatspuren in Ethanol haben zwar nicht denselben Umrechnungsfaktor wie organischer Schwefel in Ethanol, jedoch ist er diesem sehr ähnlich.
ANMERKUNG 5 Störungen durch Stickstoff können auftreten; siehe 6.5 für weitere Einzelheiten.
Produits pétroliers - Détermination de la teneur en soufre des carburants pour automobiles - Méthode par fluorescence ultraviolette (ISO 20846:2019)
Le présent document spécifie une méthode par fluorescence ultra-violette (FUV) pour le dosage du soufre dans les produits suivants:
— ceux dont la teneur en soufre est comprise dans l'intervalle de 3 à 500 mg/kg:
— les essences automobiles contenant jusqu'à 3,7 % (m/m) en oxygène [les mélanges avec de l'éthanol jusqu'à environ 10 % (V/V) inclus],
— les carburants diesel, dont ceux contenant jusqu'à 30 % (V/V) d'esters méthyliques d'acides gras.
— ceux dont la teneur en soufre est comprise dans l'intervalle de 3 à 45 mg/kg:
— les carburants synthétiques, tels que les huiles végétales hydrogénées (HVO) et les carburants liquides produits à partir de gaz («gas to liquid», GTL).
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 le présent document. Les halogènes, à des concentrations supérieures à environ 3 500 mg/kg, interfèrent.
NOTE 1 Certains catalyseurs utilisés dans le raffinage chimique et pétrolier peuvent être pollués lorsque des composés soufrés sont présents en trace dans les charges.
NOTE 2 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.
NOTE 3 Pour les besoins du présent document, «% (m/m)» et «% (V/V)» sont utilisés pour désigner respectivement la fraction massique, w, et la fraction volumique, φ, d'un produit.
NOTE 4 Le facteur de conversion des sulfates dans l'éthanol n'est pas le même que celui des composés organiques sulfurés dans l'éthanol. Ils sont cependant proches.
NOTE 5 Une interférence avec l'azote peut avoir lieu, voir 6.5 pour plus de précisions.
Naftni proizvodi - Določevanje žvepla v gorivih za motorna vozila - Ultravijolična fluorescenčna metoda (ISO 20846:2019)
Ta dokument določa ultravijolično fluorescenčno preskusno metodo za določevanje žvepla v naslednjih proizvodih: – proizvodih z vsebnostjo žvepla od 3 do 500 mg/kg; – bencinu za motorna vozila, ki vsebuje do 3,7 % (m/m) kisika (vključno z mešanicami z do 10-odstotno (V/V) vsebnostjo etanola); – dizelskih gorivih, vključno z gorivi, ki vsebujejo do 30 % (V/V) metilnih estrov maščobnih kislin (FAME); – proizvodih z vsebnostjo žvepla od 3 do 45 mg/kg; – sintetičnih gorivih, kot so z vodikom obdelano rastlinsko olje (HVO) in produkti pretvorbe plina v tekočino (GTL). To preskusno metodo je mogoče uporabiti za analizo drugih proizvodov in vsebnosti žvepla v drugih proizvodih, vendar za ta dokument niso bili določeni podatki o natančnosti za proizvode, ki niso goriva za motorna vozila, in za rezultate zunaj določenega obsega. Halogeni pri koncentracijah nad 3500 mg/kg vplivajo na to tehniko zaznavanja.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 20846:2019
01-december-2019
Nadomešča:
SIST EN ISO 20846:2011
Naftni proizvodi - Določevanje žvepla v gorivih za motorna vozila - Ultravijolična
fluorescenčna metoda (ISO 20846:2019)
Petroleum products - Determination of sulfur content of automotive fuels - Ultraviolet
fluorescence method (ISO 20846:2019)
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes von Kraftstoffen -
Ultraviolettfluoreszenz-Verfahren (ISO 20846:2019)
Produits pétroliers - Détermination de la teneur en soufre des carburants pour
automobiles - Méthode par fluorescence ultraviolette (ISO 20846:2019)
Ta slovenski standard je istoveten z: EN ISO 20846:2019
ICS:
75.160.20 Tekoča goriva Liquid fuels
SIST EN ISO 20846:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 20846:2019
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SIST EN ISO 20846:2019
EN ISO 20846
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2019
EUROPÄISCHE NORM
ICS 75.160.20; 75.160.30 Supersedes EN ISO 20846:2011
English Version
Petroleum products - Determination of sulfur content of
automotive fuels - Ultraviolet fluorescence method (ISO
20846:2019)
Produits pétroliers - Détermination de la teneur en Mineralölerzeugnisse - Bestimmung des
soufre des carburants pour automobiles - Méthode par Schwefelgehaltes von Kraftstoffen -
fluorescence ultraviolette (ISO 20846:2019) Ultraviolettfluoreszenz-Verfahren (ISO 20846:2019)
This European Standard was approved by CEN on 5 August 2019.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, 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: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 20846:2019 E
worldwide for CEN national Members.
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SIST EN ISO 20846:2019
EN ISO 20846:2019 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 20846:2019
EN ISO 20846:2019 (E)
European foreword
This document (EN ISO 20846:2019) has been prepared by Technical Committee ISO/TC 28 "Petroleum
and related products, fuels and lubricants from natural or synthetic sources" in collaboration with
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 April 2020, and conflicting national standards shall be
withdrawn at the latest by April 2020.
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 ISO 20846:2011.
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, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO 20846:2019 has been approved by CEN as EN ISO 20846:2019 without any modification.
3
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SIST EN ISO 20846:2019
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SIST EN ISO 20846:2019
INTERNATIONAL ISO
STANDARD 20846
Third edition
2019-08
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 20846:2019(E)
©
ISO 2019
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SIST EN ISO 20846:2019
ISO 20846:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 20846:2019
ISO 20846:2019(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 2
5 Reagents and materials . 2
6 Apparatus . 4
7 Sampling and sample handling . 5
8 Apparatus preparation . 5
9 Apparatus calibration and verification . 6
9.1 Multi-point calibration . 6
9.2 One-point calibration . 8
9.3 V erification . 8
10 Procedure. 9
11 Calculation . 9
11.1 Using multi-point calibration . 9
11.2 Using one-point calibration .10
11.3 Calculation .10
12 Expression of results .10
13 Precision .11
13.1 General .11
13.2 Repeatability, r .11
13.3 Reproducibility, R .11
14 Test report .12
Bibliography .13
© ISO 2019 – All rights reserved iii
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SIST EN ISO 20846:2019
ISO 20846:2019(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing Documents 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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso
.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 28, Petroleum and related products, fuels
and lubricants from natural or synthetic sources.
This third edition cancels and replaces the second edition (ISO 20846:2011), which has been technically
revised. The main change compared to the previous edition is the extension of the Scope to include
hydrotreated vegetable oil (HVO) and the synthetic fuel “gas to liquid” (GTL).
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2019 – All rights reserved
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SIST EN ISO 20846:2019
INTERNATIONAL STANDARD ISO 20846:2019(E)
Petroleum products — Determination of sulfur content of
automotive fuels — Ultraviolet fluorescence method
WARNING — The use of this document can involve hazardous materials, operations and
equipment. This document does not purport to address all of the safety problems associated
with its use. It is the responsibility of users of this document to take appropriate measures to
ensure the safety and health of personnel prior to application of the document and fulfil other
applicable requirements for this purpose.
1 Scope
This document specifies an ultraviolet (UV) fluorescence test method for the determination of the
sulfur content of the following products:
— having sulfur contents in the range 3 mg/kg to 500 mg/kg,
— motor gasolines containing up to 3,7 % (m/m) oxygen [including those blended with ethanol up
to about 10 % (V/V)],
— diesel fuels, including those containing up to about 30 % (V/V) fatty acid methyl ester (FAME),
— having sulfur contents in the range of 3 mg/kg to 45 mg/kg,
— synthetic fuels, such as hydrotreated vegetable oil (HVO) and gas to liquid (GTL).
Other products can be analysed and other sulfur contents can 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 document. 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 can be poisoned when trace amounts
of sulfur-bearing materials are contained in the feedstocks.
NOTE 2 This test method can be used to determine sulfur in process feeds and can also be used to control
sulfur in effluents.
NOTE 3 For the purposes of this document, “% (m/m)” and “% (V/V)” are used to represent the mass fraction,
w, and the volume fraction, φ, of a material respectively.
NOTE 4 Sulfate species in ethanol do not have the same conversion factor of organic sulfur in ethanol.
Nevertheless, sulfates have a conversion factor close to that of organic sulfur.
NOTE 5 Nitrogen interference can occur, see 6.5 for further guidance.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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, Laboratory glassware — One-mark volumetric flasks
ISO 3170, Petroleum liquids — Manual sampling
ISO 3171, Petroleum liquids — Automatic pipeline sampling
© ISO 2019 – All rights reserved 1
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SIST EN ISO 20846:2019
ISO 20846:2019(E)
ISO 3675, Crude petroleum and liquid petroleum products — Laboratory determination of density —
Hydrometer method
ISO 12185, Crude petroleum and petroleum products — Determination of density — Oscillating U-tube
method
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
4 Principle
A hydrocarbon sample is either directly injected or placed in a sample boat. Then, it enters a high
temperature combustion tube (1 000 °C to 1 100 °C), where the sulfur is oxidized to sulfur dioxide
(SO ) in an oxygen-rich atmosphere. Water produced during the sample combustion is removed and the
2
sample combustion gases are exposed to 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
2 2
to a stable state SO is detected by a photomultiplier tube and the resulting signal is a measure of the
2
sulfur contained in the sample.
5 Reagents and materials
5.1 Inert gas, argon or helium, high purity grade with a minimum purity of 99,998 % (V/V).
5.2 Oxygen, high purity grade with a minimum purity of 99,75 % (V/V).
CAUTION — Oxygen vigorously accelerates combustion.
5.3 Solvent.
5.3.1 General
Use either that specified in 5.3.2 or 5.3.3, 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.
5.3.2 Toluene, reagent grade.
5.3.3 Isooctane, reagent grade.
CAUTION — Flammable solvents.
2 © ISO 2019 – All rights reserved
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SIST EN ISO 20846:2019
ISO 20846:2019(E)
5.4 Sulfur compounds
5.4.1 General
Compounds with a minimum purity of 99 % (m/m). Examples are given in 5.4.2 to 5.4.4. Where the
purity of these compounds is less than 99 % (m/m), the concentrations and nature of all impurities shall
be established.
NOTE 1 A correction for chemical impurity can be applied when the sulfur content is known with accuracy.
[3]
NOTE 2 Certified reference materials (CRM) produced in accordance with ISO 17034 are suitable
alternatives to the compounds listed in 5.4.2 to 5.4.4.
5.4.2 Dibenzothiophene (DBT), of molar mass 184,26 g/mol, with a nominal sulfur content of
17,399 % (m/m).
5.4.3 Dibutyl sulfide (DBS), of molar mass 146,29 g/mol, with a nominal sulfur content of
21,915 % (m/m).
5.4.4 Thionaphthene (benzothiophene) (TNA), of molar mass 134,20 g/mol, with a nominal sulfur
content of 23,890 % (m/m).
5.5 Sulfur stock solution
Prepare a stock solution of approximately 1 000 mg/l sulfur content by accurately weighing the
appropriate quantity of sulfur compound (5.4) in a volumetric flask (6.9). Ensure complete dissolution
with solvent (5.3). 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 (5.4) in a volumetric flask (6.9) and reweighing the volumetric
flask once it has been filled to the mark with the solvent (5.3). Take precautions to ensure that
evaporation of the solvent and/or sulfur compounds is not causing weighing errors.
The appropriate mass of sulfur compound described in 5.4.2 to 5.4.4 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 The shelf life of the stock solution is approximately three months when stored at low temperature,
typically in a refrigerator.
5.6 Calibration standards
Prepare the calibration standards by dilution of the stock solution (5.5) with the selected solvent (5.3).
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 dilution (or mass/mass dilution,
respectively) of the stock solution at 1 000 mg/l (or 1 000 mg/kg respectively). Other practices are
possible, but those mentioned above av
...
SLOVENSKI STANDARD
oSIST prEN ISO 20846:2018
01-december-2018
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Petroleum products - Determination of sulfur content of automotive fuels - Ultraviolet
fluorescence method (ISO/DIS 20846:2018)
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes von Kraftstoffen -
Ultraviolettfluoreszenz-Verfahren (ISO/DIS 20846:2018)
Produits pétroliers - Détermination de la teneur en soufre des carburants pour
automobiles - Méthode par fluorescence ultraviolette (ISO/DIS 20846:2018)
Ta slovenski standard je istoveten z: prEN ISO 20846
ICS:
75.160.20 7HNRþDJRULYD Liquid fuels
oSIST prEN ISO 20846:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST prEN ISO 20846:2018
---------------------- Page: 2 ----------------------
oSIST prEN ISO 20846:2018
DRAFT INTERNATIONAL STANDARD
ISO/DIS 20846
ISO/TC 28 Secretariat: NEN
Voting begins on: Voting terminates on:
2018-10-05 2018-12-28
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
ICS: 75.160.20; 75.160.30
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 20846:2018(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2018
---------------------- Page: 3 ----------------------
oSIST prEN ISO 20846:2018
ISO/DIS 20846:2018(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2018
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST prEN ISO 20846:2018
ISO/DIS 20846:2018(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 2
5 Reagents and materials . 2
6 Apparatus . 3
7 Sampling . 5
8 Apparatus preparation . 5
9 Apparatus calibration and verification . 6
9.1 Multi-point calibration . 6
9.2 One-point calibration . 7
9.3 Verification . 8
10 Procedure. 8
11 Calculation . 9
11.1 Using multi-point calibration . 9
11.2 Using one-point calibration .10
11.3 Calculation .10
12 Expression of results .10
13 Precision .11
13.1 General .11
13.2 Repeatability, r . 11
13.3 Reproducibility, R . 11
14 Test report .12
Bibliography .13
© ISO 2018 – All rights reserved iii
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oSIST prEN ISO 20846:2018
ISO/DIS 20846:2018(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing Documents 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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso
.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 28, Petroleum and related products, fuels
and lubricants from natural or synthetic sources.
This third edition cancels and replaces the second edition (ISO 20846:2011), which has been technically
revised following a new interlaboratory study executed by CEN/TC 19/WG 27, Elemental analysis, that
confirmed the method precision. The main changes however compared to the previous edition are as
follows:
— In this edition the scope has been extended and now includes hydrotreated vegetable oil (HVO) and
the synthetic fuel Gas To Liquid (GTL).
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
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oSIST prEN ISO 20846:2018
DRAFT INTERNATIONAL STANDARD ISO/DIS 20846:2018(E)
Petroleum products — Determination of sulfur content of
automotive fuels — Ultraviolet fluorescence method
WARNING — the use of this document may involve hazardous materials, operations and
equipment. This document does not purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this document to establish appropriate safety
and health practices and determine the applicability of regulatory limitations prior to use.
1 Scope
This document specifies an ultraviolet (UV) fluorescence test method for the determination of the
sulfur content of motor gasolines containing up to 3,7 % (m/m) oxygen [including those blended with
ethanol up to about 10 % (V/V)], diesel fuels, including those containing up to about 30 % (V/V) fatty
acid methylester (FAME), having sulfur contents in the range 3 mg/kg to 500 mg/kg and synthetic
fuels, such as Hydrotreated Vegetable Oil (HVO) and Gas To Liquid (GTL), having sulfur contents in the
range of 3 mg/kg to 45 mg/kg.
Other products can be analysed and other sulfur contents can 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 document. 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 can be poisoned when trace amounts
of sulfur-bearing materials are contained in the feedstocks.
NOTE 2 This test method can be used to determine sulfur in process feeds and can also be used to control
sulfur in effluents.
NOTE 3 For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent the mass
fraction, μ, and the volume fraction, φ, of a material respectively.
NOTE 4 Sulfate species in ethanol do not have the same conversion factor of organic sulfur in ethanol.
Nevertheless, sulfates have a conversion factor close to that of organic sulfur.
NOTE 5 It is preferable to check the nitrogen interference and to take it into account, especially when sulfur
content is measured on diesel blended with cetane improver containing nitrogen. For example, alkyl nitrate, as
2‑ethyl hexyl nitrate (EHN), added as cetane improver to diesel fuel shows an enhancing effect on sulfur content
that can range from (0 to 1,7) mg/kg when 2 000 mg/kg EHN is added to diesel fuel containing 10 mg/kg sulfur.
2 Normative references
The follo3675
wing 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, Laboratory glassware — One-mark volumetric flasks
ISO 3170, Petroleum liquids — Manual sampling
ISO 3171, Petroleum liquids — Automatic pipeline sampling
ISO 3675, Crude petroleum and liquid petroleum products — Laboratory determination of density —
Hydrometer method
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ISO 12185, Crude petroleum and petroleum products — Determination of density — Oscillating U-tube
method
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
4 Principle
A hydrocarbon sample is injected into a UV fluorescence detector. The sample enters a high
temperature combustion tube (1 000 °C to 1 100 °C), where the sulfur is oxidized to sulfur dioxide
(SO ) in an oxygen‑rich atmosphere. Water produced during the sample combustion is removed and
2
the sample combustion gases are exposed to UV light. The SO absorbs the energy from the UV light
2
and is converted to excited sulfur dioxide (SO *). The fluorescence emitted from the excited SO * as it
2 2
returns to a stable state SO is detected by a photomultiplier tube and the resulting signal is a measure
2
of the sulfur contained in the sample.
5 Reagents and materials
5.1 Inert gas, argon or helium, high purity grade with a minimum purity of 99,998 % (V/V).
5.2 Oxygen, high purity grade with a minimum purity of 99,75 % (V/V).
CAUTION — Oxygen vigorously accelerates combustion.
5.3 Solvent
5.3.1 General
Use either that specified in 5.3.2 or 5.3.3, 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.
5.3.2 Toluene, reagent grade.
5.3.3 Isooctane, reagent grade.
CAUTION — Flammable solvents.
5.4 Sulfur compounds
5.4.1 General
Compounds with a minimum purity of 99 % (m/m). Examples are given in 5.4.2 to 5.4.4. Where the
purity of these compounds is less than 99 % (m/m), the concentrations and nature of all impurities shall
be established.
NOTE A correction for chemical impurity can be applied when the sulfur content is known with accuracy.
Certified reference materials (CRM) from accredited suppliers are suitable alternatives to the
compounds listed in 5.4.2 to 5.4.4.
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oSIST prEN ISO 20846:2018
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5.4.2 Dibenzothiophene (DBT), of molecular mass 184,26, with a nominal sulfur content of
17,399 % (m/m).
5.4.3 Dibutyl sulfide (DBS), of molecular mass 146,29, with a nominal sulfur content of
21,915 % (m/m).
5.4.4 Thionaphthene (Benzothiophene) (TNA), of molecular mass 134,20, with a nominal sulfur
content of 23,890 % (m/m).
5.5 Sulfur stock solution
Prepare a stock solution of approximately 1 000 mg/l sulfur content by accurately weighing the
appropriate quantity of sulfur compound (5.4) in a volumetric flask (6.9). Ensure complete dissolution
with solvent (5.3). 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 (5.4) in a volumetric flask (6.9) and reweighing the volumetric
flask once it has been filled to the mark with the solvent (5.3). Take precautions to ensure that
evaporation of the solvent and/or sulfur compounds is not causing weighing errors.
The appropriate mass of sulfur compound described in 5.4.2 to 5.4.4 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 The shelf life of the stock solution is approximately three months when stored at low temperature,
typically in a refrigerator.
5.6 Calibration standards
Prepare the calibration standards by dilution of the stock solution (5.5) with the selected solvent (5.3).
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 dilution (or mass/mass dilution,
respectively) of the stock solution at 1 000 mg/l (or 1 000 mg/kg 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 shelf life of at least one month. Below this sulfur
content (30 mg/kg), the shelf life should be reduced.
5.7 Quality control samples
Quality control samples are stable samples representative of the materials being analysed, which 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. Prior to use, ensure that the
material is within its shelf life.
5.8 Quartz wool
Follow the manufacturer's recommendations.
6 Apparatus
Figure 1 illustrates the basic pieces of the UVF.
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oSIST prEN ISO 20846:2018
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Key
1 UV source 6 inert gas input
2 photomultiplier 7 gases output
3 output signal 8 vapour drier (6.5)
4 furnace, 1 000 °C to 1 100 °C (6.1) 9 quartz tube
5 oxygen input 10 microlitre syringe
Figure 1 — Synopsis of the apparatus
6.1 F
...
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