SIST EN ISO 14596:2007
Petroleum products - Determination of sulfur content - Wavelength-dispersive X-ray fluorescence spectrometry (ISO 14596:2007)
Petroleum products - Determination of sulfur content - Wavelength-dispersive X-ray fluorescence spectrometry (ISO 14596:2007)
This International Standard specifies a method for the determination of the sulfur content of liquid petroleum products, additives for petroleum products, and semi-solid and solid petroleum products that are either liquefied by moderate heating or soluble in organic solvents (see 4.1) of negligible or accurately known sulfur content. The method is applicable to products or additives having sulfur contents in the range 0,001 % (m/m) to 2,50 % (m/m); higher contents can be determined by appropriate dilution. Other elements do not interfere at concentrations anticipated in the materials subject to this analysis. High concentrations of phosphorus or chlorine [typically above 3 % (m/m)] can cause bias in the sulfur result by absorbing Zr-L and S-K to different extents. It is necessary in these cases to carry out studies to determine whether this potential interference is significant. When larger amounts of molybdenum are present (typically above 50 mg/kg to 100 mg/kg), increased background radiation and spectral overlap with the sulfur signal can occur. It is necessary in these cases to inspect the relevant spectral regions, for example, to investigate the significance of this potential source of bias.
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes - Wellenlängendispersive Röntgenfluoreszenz-Analyse (ISO 14596:2007)
Diese Internationale Norm legt ein Verfahren fest zur Bestimmung des Schwefelgehaltes von flüssigen Mineralölerzeugnissen, Additiven für Mineralölerzeugnisse sowie von halb-festen oder festen Mineralölerzeugnissen, die entweder durch mäßiges Erhitzen verflüssigt werden können oder löslich in organischen Lösemitteln (siehe 4.1) mit vernachlässigbarem oder aber genau bekanntem Schwefelgehalt sind. Das Verfahren ist anwendbar auf Produkte mit einem Schwefelanteil im Bereich von 0,001 % (m/m) bis 2,50 % (m/m) Massenanteil; höhere Gehalte sind durch entsprechende Verdünnung bestimmbar. Andere Elemente stören nicht in den Gehaltsbereichen, die in Materialien für diese Prüfung erwartet werden können.
ANMERKUNG 1 Für den Zweck dieser Internationalen Norm wird das Symbol "% (m/m)" für "Massenanteil in %" verwendet.
ANMERKUNG 2 Hohe Phosphorgehalte können Abweichungen für ein Schwefel-Ergebnis verursachen, da die Zr-L?-Linie und die S-K?-Linie in unterschiedlichem Ausmaß abgeschwächt werden. In solchen Fällen wird empfohlen, das Ausmaß dieser Störung durch Phosphor genauer zu untersuchen.
ANMERKUNG 3 Bei höheren Molybdängehalten (üblicherweise 50 mg/kg bis 100 mg/kg) kann es eine angestiegene Hintergrundstrahlung sowie spektrale Überlappungen mit dem Schwefelsignal geben. In diesen Fällen sollten die relevanten spektralen Bereiche hinsichtlich der Bedeutung potentieller Störungen untersucht werden.
Produits pétroliers - Détermination de la teneur en soufre - Spectrométrie de fluorescence X dispersive en longueur d'onde (ISO 14596:2007)
L'ISO 14596:2007 spécifie une méthode de détermination de la teneur en soufre dans les produits pétroliers liquides, dans les additifs pour produits pétroliers, et dans les produits pétroliers solides et semi-solides qui sont soit liquéfiés par un chauffage modéré, soit solubles dans des solvants organiques dont la teneur en soufre est négligeable ou connue avec précision. La méthode est applicable à des produits ou à des additifs dont la teneur en soufre est située de 0,001 % (m/m) à 2,50 % (m/m), des teneurs plus élevées pouvant être déterminées par des dilutions appropriées. Les autres éléments n'interfèrent pas dans le domaine de concentration visé pour les produits relevant de cette méthode.
Naftni proizvodi – Določevanje vsebnosti žvepla – Valovno disperzivna rentgenska fluorescenčna spektrometrija (ISO 14596:2007)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 14596:2007
01-december-2007
1DGRPHãþD
SIST EN ISO 14596:1999
1DIWQLSURL]YRGL±'RORþHYDQMHYVHEQRVWLåYHSOD±9DORYQRGLVSHU]LYQDUHQWJHQVND
IOXRUHVFHQþQDVSHNWURPHWULMD ,62
Petroleum products - Determination of sulfur content - Wavelength-dispersive X-ray
fluorescence spectrometry (ISO 14596:2007)
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes - Wellenlängendispersive
Röntgenfluoreszenz-Analyse (ISO 14596:2007)
Produits pétroliers - Détermination de la teneur en soufre - Spectrométrie de
fluorescence X dispersive en longueur d'onde (ISO 14596:2007)
Ta slovenski standard je istoveten z: EN ISO 14596:2007
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
SIST EN ISO 14596:2007 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
EUROPEAN STANDARD
EN ISO 14596
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2007
ICS 75.080 Supersedes EN ISO 14596:1998
English Version
Petroleum products - Determination of sulfur content -
Wavelength-dispersive X-ray fluorescence spectrometry (ISO
14596:2007)
Produits pétroliers - Détermination de la teneur en soufre - Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes
Spectrométrie de fluorescence X dispersive en longueur - Wellenlängendispersive Röntgenfluoreszenz-Analyse
d'onde (ISO 14596:2007) (ISO 14596:2007)
This European Standard was approved by CEN on 8 September 2007.
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 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 Management Centre has the same status as the
official 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 STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2007 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 14596:2007: E
worldwide for CEN national Members.
---------------------- Page: 2 ----------------------
EN ISO 14596:2007 (E)
Contents Page
Foreword.3
2
---------------------- Page: 3 ----------------------
EN ISO 14596:2007 (E)
Foreword
This document (EN ISO 14596:2007) has been prepared by Technical Committee ISO/TC 28 "Petroleum
products and lubricants" 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 March 2008, and conflicting national standards shall be withdrawn at
the latest by March 2008.
This document supersedes EN ISO 14596:1998.
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 the United Kingdom.
Endorsement notice
The text of ISO 14596:2007 has been approved by CEN as a EN ISO 14596:2007 without any modification.
3
---------------------- Page: 4 ----------------------
INTERNATIONAL ISO
STANDARD 14596
Second edition
2007-09-15
Petroleum products — Determination of
sulfur content — Wavelength-dispersive
X-ray fluorescence spectrometry
Produits pétroliers — Détermination de la teneur en soufre —
Spectrométrie de fluorescence X dispersive en longueur d'onde
Reference number
ISO 14596:2007(E)
©
ISO 2007
---------------------- Page: 5 ----------------------
ISO 14596:2007(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
COPYRIGHT PROTECTED DOCUMENT
© ISO 2007
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2007 – All rights reserved
---------------------- Page: 6 ----------------------
ISO 14596:2007(E)
Contents Page
Foreword. iv
1 Scope .1
2 Normative references .1
3 Principle.2
4 Reagents and materials .2
5 Apparatus .2
6 Samples and sampling.3
7 Calibration solutions .3
8 Calibration .5
9 Procedure .7
10 Calculation.7
11 Expression of results .7
12 Precision.7
13 Test report .8
© ISO 2007 – All rights reserved iii
---------------------- Page: 7 ----------------------
ISO 14596:2007(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 14596 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants.
This second edition cancels and replaces the first edition (ISO 14596:1998), which has been technically
revised. It also incorporates the Technical Corrigendum ISO 14596:1998/Cor. 1:1999.
iv © ISO 2007 – All rights reserved
---------------------- Page: 8 ----------------------
INTERNATIONAL STANDARD ISO 14596:2007(E)
Petroleum products — Determination of sulfur content —
Wavelength-dispersive X-ray fluorescence spectrometry
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 a method for the determination of the sulfur content of liquid petroleum
products, additives for petroleum products, and semi-solid and solid petroleum products that are either
liquefied by moderate heating or soluble in organic solvents (see 4.1) of negligible or accurately known sulfur
content. The method is applicable to products or additives having sulfur contents in the range 0,001 % (m/m)
to 2,50 % (m/m); higher contents can be determined by appropriate dilution. Other elements do not interfere at
concentrations anticipated in the materials subject to this analysis.
NOTE For the purposes of this International Standard, the term “% (m/m)” is used to represent the mass fraction of a
material.
High concentrations of phosphorus or chlorine [typically above 3 % (m/m)] can cause bias in the sulfur result
by absorbing Zr-Lα and S-Kα to different extents. It is necessary in these cases to carry out studies to
determine whether this potential interference is significant.
When larger amounts of molybdenum are present (typically above 50 mg/kg to 100 mg/kg), increased
background radiation and spectral overlap with the sulfur signal can occur. It is necessary in these cases to
inspect the relevant spectral regions, for example, to investigate the significance of this potential source of
bias.
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 3170:2004, Petroleum liquids — Manual sampling
ISO 3171:1988, Petroleum liquids — Automatic pipeline sampling
© ISO 2007 – All rights reserved 1
---------------------- Page: 9 ----------------------
ISO 14596:2007(E)
3 Principle
The test portion and a zirconium solution as internal standard are mixed in a given mass ratio and exposed, in
a sample cell, to the primary radiation of an X-ray tube.
The count rates of the S-Kα at 0,537 3 nm and Zr-Lα1 at 0,607 0 nm fluorescence thus excited and the count
rate of the background radiation at 0,545 nm are measured and the ratio of these net count rates calculated.
The sulfur content of the sample is determined from a calibration curve prepared on the basis of sulfur
calibration standards.
NOTE The Siegbahn X-ray line notation (S-Kα) is used in this International Standard; the corresponding IUPAC X-ray
line notation is S K-L .
2,3
4 Reagents and materials
4.1 White oil (light paraffin oil, paraffinum perliquidum), high-purity grade, sulfur content 1 mg/kg
maximum.
4.2 Sulfur compounds, of sulfur content accurately known to the nearest 0,01 % (m/m), used for the
preparation of the primary standards.
The compounds given in 4.2.1 to 4.2.3 are suitable, and their nominal sulfur contents are given. Where the
purity of these compounds is less than 99 %, certified materials are required, or the nature of all impurities and
their contents should be accurately known to the nearest 0,01 % (m/m).
4.2.1 Dibenzothiophene (DBT), with a nominal sulfur content of 17,399 % (m/m).
4.2.2 Dibutyl sulfide (DBS), with a nominal sulfur content of 21,915 % (m/m).
4.2.3 Thionaphthene (benzothiophene) (TNA), with a nominal sulfur content of 23,890 % (m/m).
4.3 Certified sulfur reference materials.
Use
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.