EN ISO 8754:2003
(Main)Petroleum products - Determination of sulfur content - Energy-dispersive X-ray fluorescence spectrometry (ISO 8754:2003)
Petroleum products - Determination of sulfur content - Energy-dispersive X-ray fluorescence spectrometry (ISO 8754:2003)
ISO 8754:2003 specifies a method for the determination of the sulfur content of petroleum products, such as naphthas, unleaded motor gasolines, middle distillates, residual fuel oils, base lubricating oils and components. The method is applicable to products having sulfur contents in the range 0,03 % (by mass) to 5,00 % (by mass).
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes - Energiedispersives Röntgenfluoreszenz-Verfahren (ISO 8754:2003)
Diese Internationale Norm beschreibt ein Verfahren zur Bestimmung des Schwefelgehaltes in Mineralölerzeugnissen, wie z.B. Naphthas, unverbleite Ottokraftstoffe, Mitteldestillate, Rückstandsöle, Grundöle für Schmieröle und Komponenten. Das Verfahren ist anwendbar auf Produkte mit Schwefelgehalten im Bereich von 0,03 % (m/m) bis 5,00 % (m/m).
ANMERKUNG Für den Zweck dieser Internationalen Norm darf das Symbol % (m/m) verwendet werden, um Massenanteile in Prozent auszudrücken.
Schwermetalladditive, z.B. Bleialkyle, können die Bestimmung stören. Elemente wie Silizium, Phosphor, Calzium, Sauerstoff, Kalium, Zink, Molybdän, Barium und Halogene stören, wenn ihr Massenanteil mehr als einige hundert Milligramm je Kilogramm beträgt. Einige moderne Geräte ermöglichen dem Analytiker eine Kompensation von Matrix- und spektralen Störungen mit Hilfe von Spektrenentzerrung und Interelementkorrektur durch multiple Regression.
Bei Proben, deren Zusammensetzung sich in Bezug auf aromatische und paraffinische Kohlenwasserstoffe unterscheidet, kann das Verhältnis von Kohlenstoff zu Wasserstoff (C/H-Verhältnis) einer Probe ebenfalls zu einer Störung der Bestimmung führen, und zwar bei einer Abweichung des Verhältnisses der Probe von eins oder höher von dem Verhältnis der Referenzmaterialien, die zur Kalibrierung dienten.
Produits pétroliers - Détermination de la teneur en soufre - Spectrométrie de fluorescence X dispersive en énergie (ISO 8754:2003)
L'ISO 8754:2003 spécifie une méthode d'essai qui a pour but de déterminer la teneur en soufre des produits pétroliers tels que naphtas, essences sans plomb, distillats moyens, combustibles résiduels, huiles de base et constituants. La méthode est applicable aux produits dont la teneur en soufre est comprise entre 0,03 % (en masse) et 5 % (en masse).
Naftni proizvodi – Določevanje žvepla – Metoda z energijsko-disperzivno rentgensko fluorescenčno spektrometrijo (ISO 8754:2003)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-november-2003
1DGRPHãþD
SIST EN ISO 8754:1998
1DIWQLSURL]YRGL±'RORþHYDQMHåYHSOD±0HWRGD]HQHUJLMVNRGLVSHU]LYQR
UHQWJHQVNRIOXRUHVFHQþQRVSHNWURPHWULMR ,62
Petroleum products - Determination of sulfur content - Energy-dispersive X-ray
fluorescence spectrometry (ISO 8754:2003)
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes - Energiedispersives
Röntgenfluoreszenz-Verfahren (ISO 8754:2003)
Produits pétroliers - Détermination de la teneur en soufre - Spectrométrie de
fluorescence X dispersive en énergie (ISO 8754:2003)
Ta slovenski standard je istoveten z: EN ISO 8754:2003
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EUROPEAN STANDARD
EN ISO 8754
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2003
ICS 75.080 Supersedes EN ISO 8754:1995
English version
Petroleum products - Determination of sulfur content - Energy-
dispersive X-ray fluorescence spectrometry (ISO 8754:2003)
Produits pétroliers - Détermination de la teneur en soufre - Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes
Spectrométrie de fluorescence X dispersive en énergie - Energiedispersives Röntgenfluoreszenz-Verfahren (ISO
(ISO 8754:2003) 8754:2003)
This European Standard was approved by CEN on 10 July 2003.
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, Czech Republic, Denmark, Finland, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, 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
© 2003 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 8754:2003 E
worldwide for CEN national Members.
CORRECTED 2003-10-01
Foreword
This document (EN ISO 8754:2003) 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 January 2004, and conflicting national
standards shall be withdrawn at the latest by January 2004.
This document supersedes EN ISO 8754:1995.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium, Czech
Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and
the United Kingdom.
Endorsement notice
The text of ISO 8754:2003 has been approved by CEN as EN ISO 8754:2003 without any
modifications.
NOTE Normative references to International Standards are listed in Annex ZA (normative).
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions of
any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).
NOTE Where an International Publication has been modified by common modifications, indicated
by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 3170 1988 Petroleum liquids - Manual EN ISO 3170 1998
sampling
ISO 3171 1988 Petroleum liquids - Automatic EN ISO 3171 1999
pipeline sampling
INTERNATIONAL ISO
STANDARD 8754
Second edition
2003-07-15
Petroleum products — Determination of
sulfur content — Energy-dispersive X-ray
fluorescence spectrometry
Produits pétroliers — Détermination de la teneur en soufre —
Spectrométrie de fluorescence de rayons X dispersive en énergie
Reference number
ISO 8754:2003(E)
©
ISO 2003
ISO 8754:2003(E)
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ii © ISO 2003 — All rights reserved
ISO 8754:2003(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 8754 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants.
This second edition cancels and replaces the first edition (ISO 8754:1992), which has been technically
revised.
ISO 8754:2003(E)
Introduction
Specialized procedures, using the analytical technique described in this International Standard, for automotive
fuels with sulfur contents below 0,20 % (m/m), are under development.
iv © ISO 2003 — All rights reserved
INTERNATIONAL STANDARD ISO 8754:2003(E)
Petroleum products — Determination of sulfur content —
Energy-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 petroleum
products, such as naphthas, unleaded motor gasolines, middle distillates, residual fuel oils, base lubricating
oils and components. The method is applicable to products having sulfur contents in the range 0,03 % (m/m)
to 5,00 % (m/m).
NOTE For the purposes of this International Standard, the term "% (m/m)" is used to represent the mass fraction of a
material.
Heavy metal additives, such as lead alkyls, may interfere with the determination. Elements such as silicon,
phosphorus, calcium, oxygen, potassium, zinc, molybdenum, barium and halogens interfere, if present in
concentrations of more than a few hundred milligrams per kilogram. Some modern instruments allow the
analyst to compensate for matrix and spectral interferences by spectra deconvolution and inter-element
correction by multiple regression.
For samples varying in composition of aromatic hydrocarbons and paraffinic hydrocarbons, the ratio of carbon
to hydrocarbon in a sample (C/H ratio) may also interfere with the determination, when the ratio of the sample
differs by one or more from that of the reference materials from which the calibration is obtained.
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.
1)
ISO 3170:— , Petroleum liquids — Manual sampling
ISO 3171:1988, Petroleum liquids — Automatic pipeline sampling
3 Principle
The test portion is placed in the beam emitted from an X-ray source. The excitation energy may be derived
from a radioactive source, such as Fe, or from an X-ray tube. The resultant excited characteristic X radiation
is measured, and the accumulated count is compared with a calibration graph plotting counts against sulfur
content as percentage by mass [% (m/m)], on a series of calibration samples covering the range of sulfur
contents under examination.
1) To be published. (Revision of ISO 3170:1988)
ISO 8754:2003(E)
4 Reagents and materials
4.1 White oil (light paraffin oil), of high purity grade, with a maximum sulfur content of 20 mg/kg.
For measurements at very low levels of sulfur content [below approximately 0,1 % (m/m)], matrix effects are
minimized if a diluent of a type similar to the product being analysed is used for the production of the
calibration standards described in Clause 8. Such a diluent should be of very low sulfur content, preferably
below 2 mg/kg.
4.2 Sulfur compounds, of known sulfur content, used for the preparation of the primary standards.
NOTE 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 concentrations and nature of all
impurities are to be known.
4.2.1 Dibenzothiophene (DBT), with a nominal sulfur content of 17,399 % (m/m).
4.2.2 Dibutylsulfide (DBS), with a nominal sulfur content of 21,915 % (m/m).
4.2.3 Thionaphthene (benzothiophene) (TNA), with a nominal sulfur content of 23,89 % (m/m).
4.3 Certified reference materials: use materials from a national standards body or accredited supplier,
with a range of certified sulfur contents for the production of calibration curves for routine analysis. However,
particularly for some heavier materials, the excitation is slightly affected by the background matrix. Therefore,
in cases of dispute, the parties shall agree on a common range of certified standards, or shall both prepare
standards from the materials described in 4.1 and 4.2.
5 Apparatus
5.1 Energy-dispersive X-ray fluorescence analyser: use any suitable model, provided that the design
incorporates the features given in 5.1.1 to 5.1.6. It shall be set up according to the manufacturer’s instructions.
5.1.1 Source of X-ray excitation, with significant X-ray flux at energies above 2,5 keV.
5.1.2 Removable sample cup, providing a sample depth of at least 3 mm, and equipped with replaceable
X-ray transparent film.
NOTE Window material is normally 6 µm polyester, polypropylene or polycarbonate film. Commercial polyester film
may contain small but variable amounts of calcium, which may interfere. Samples of very high aromatic content may
dissolve polycarbonate film.
5.1.3 X-ray detector, with high sensitivity at 2,3 keV.
5.1.4 Filters, or other means of discriminating between sulfur Kα radiation and other X-rays.
5.1.5 Signal-conditioning electronics, that include the functions of pulse counting and pulse-height
analysis.
5.1.6 Display or printer, that provides a readout in counts, sulfur content as a percentage by mass
[% (m/m)], or both.
CAUTION — If the analyser contains a radioactive source, the equipment and manner of use shall
comply with the regulations governing the use of ionizing radiation and/or
...
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