EN ISO 14596:1998
(Main)Petroleum products - Determination of sulfur content - Wavelength-dispersive X-ray fluorescence spectrometry (ISO 14596:1998)
Petroleum products - Determination of sulfur content - Wavelength-dispersive X-ray fluorescence spectrometry (ISO 14596:1998)
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes - Wellenlängendispersive Röntgenfluoreßenz-Analyse (ISO 14596:1998)
Diese Internationale Norm beschreibt ein Verfahren 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 bekannten Schwefelgehalt sind. Das Verfahren ist anwendbar auf Produkte mit einem Schwefelanteil im Bereich von 0,001 bis 2,50 % (m/m) Massenanteil; höhere Gehalte sind durch entsprechende Verdünnung bestimmbar.
Produits pétroliers - Dosage du soufre - Spectrométrie de fluorescence X dispersive en longueur d'onde (ISO 14596:1998)
Naftni proizvodi – Določevanje žvepla – Valovno disperzivna rentgenska fluorescenčna spektrometrija (ISO 14596:1998)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 14596:1999
01-november-1999
1DIWQLSURL]YRGL±'RORþHYDQMHåYHSOD±9DORYQRGLVSHU]LYQDUHQWJHQVND
IOXRUHVFHQþQDVSHNWURPHWULMD ,62
Petroleum products - Determination of sulfur content - Wavelength-dispersive X-ray
fluorescence spectrometry (ISO 14596:1998)
Mineralölerzeugnisse - Bestimmung des Schwefelgehaltes - Wellenlängendispersive
Röntgenfluoreßenz-Analyse (ISO 14596:1998)
Produits pétroliers - Dosage du soufre - Spectrométrie de fluorescence X dispersive en
longueur d'onde (ISO 14596:1998)
Ta slovenski standard je istoveten z: EN ISO 14596:1998
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
SIST EN ISO 14596:1999 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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INTERNATIONAL ISO
STANDARD 14596
First edition
1998-06-15
Petroleum products — Determination
of sulfur content — Wavelength-dispersive
X-ray fluorescence spectrometry
Produits pétroliers — Dosage du soufre — Spectrométrie de fluorescence X
dispersive en longueur d'onde
A
Reference number
ISO 14596:1998(E)
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ISO 14596:1998(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.
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.
International Standard ISO 14596 was prepared by Technical Committee
ISO/TC 28, Petroleum products and lubricants.
© ISO 1998
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 the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet iso@iso.ch
Printed in Switzerland
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©
INTERNATIONAL STANDARD ISO ISO 14596:1998(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 may be determined by appropriate dilution. Other elements do not interfere at concentrations
anticipated in the materials subject to this analysis.
NOTE 1 For the purposes of this International Standard, the term "% (m/m)" is used to represent the mass fraction.
2 Normative references
The following standards contain provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of publication, the editions indicated were valid. All standards are subject to
revision, and parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain
registers of currently valid International Standards.
ISO 3170:1988, Petroleum liquids — Manual sampling.
ISO 3171:1988, Petroleum liquids — Automatic pipeline sampling.
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-K at 0,537 3 nm and Zr-L at 0,607 0 nm fluorescence thus excited and the count rate of
α α1
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.
4 Reagents and materials
4.1 White oil (light paraffin oil), 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.
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ISO
ISO 14596:1998(E)
NOTE 2 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 concentrations
should be accurately known to the nearest 0,01 % (m/m).
4.2.1 Dibenzothiophene (DBT), nominal sulfur content 17,399 % (m/m).
4.2.2 Dibutyl sulfide (DBS), nominal sulfur content 21,915 % (m/m).
4.2.3 Thionaphthene (Benzothiophene)(TNA), nominal sulfur content 23,890 % (m/m).
4.3 Certified sulfur reference materials
Use materials from a national standards body or accredited suppliers, if available.
4.4 Zirconium solution A
Zirconium octoate solution with a zirconium content in the range of 12 % (m/m) to 18 % (m/m), or another oil-soluble
zirconium compound dissolved in white oil (4.1) to provide a zirconium content in the range of 12 % (m/m) to
18 % (m/m).
4.5 Zirconium solution B
Dilute the zirconium solution A (4.4) with white oil (4.1) to provide a content of approximately 1 % (m/m) zirconium.
5 Apparatus
5.1 Wavelength-dispersive X-ray fluorescence spectrometer, use any suitable spectrometer, provided that
the design incorporates the features given in table 1. It shall be set up according to the manufacturer's instructions.
Table 1 — General requirements of spectrometer
Component Requirement
Anode Rhodium, scandium or chromium target
1)
Voltage 30 kV to 50 kV
1)
Current 30 mA to 70 mA
Collimator Coarse
Analysing crystal Germanium, pentaerythritol, or graphite
Optical path Helium
Cell window Polyester or polypropylene film, sulfur-free, thickness 2 μm to 6 μm
Detector Gas flow proportional counter with a pulse-height analyser
1) Lower power systems may be used, provided that they have been validated to meet the requirements
specified in 8.3 and clause 12.
5.2 Analytical balance, capable of weighing to the nearest 0,1 mg.
5.3 Homogenizer, non-aerating, high speed shear type, or heatable magnetic or ultrasonic stirrer.
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ISO
ISO 14596:1998(E)
5.4 Flasks, of 50 ml capacity, narrow-necked, conical, made of borosilicate glass, and fitted with ground-glass
stoppers. Use flasks of higher capacity for stock solutions (7.2).
6 Samples and sampling
6.1 Unless otherwise specified, samples shall be taken according to the procedure described in ISO 3170 or
ISO 3171.
6.2 Test portions from the samples shall be drawn after thorough mixing and subdivision. Heat viscous samples
to a temperature which renders the sample liquid, and homogenize, using the homogenizer (5.3) as necessary.
NOTE 3 For the purpose of this procedure, the term "sample" also includes solutions prepared from additives, semi-solid or
solid petroleum products that have been appropriately pre-treated and/or diluted.
7 Calibration solutions
7.1 General
Use either certified reference materials (4.3) or primary standards prepared from sulfur compounds (4.2) dissolved
in white oil (4.1) as
...
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