SIST EN ISO 14720-2:2013

SLOVENSKI STANDARD
SIST EN ISO 14720-2:2013
01-maj-2013
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Testing of ceramic raw and basic materials - Determination of sulfur in powders and
granules of non-oxidic ceramic raw and basic materials - Part 2: Inductively coupled
plasma optical emission spectrometry (ICP/OES) or ion chromatography after burning in
an oxygen flow (ISO 14720-2:2013)
Prüfung keramischer Roh- und Werkstoffe - Bestimmung des Schwefel-gehaltes in
pulver- und kornförmigen nichtoxidischen keramischen Roh- und Werkstoffen - Teil 2:
Atomemissionsspektroskopie mit induktiv gekoppeltem Plasma (ICP AES) oder
Ionenchromatographie (IC) nach Verbrennung im Sauerstoffstrom (ISO 14720-2:2013)
Essais des matières premières et matériaux de base céramiques - Dosage du soufre
dans des matières premières et matériaux de base céramiques non oxydiques sous
forme de poudre et de granulés - Partie 2: Spectrométrie d'émission atomique avec
plasma induit par haute fréquence (ICP/AES) ou chromatographie ionique après
combustion dans un courant d'oxygène (ISO 14720-2:2013)
Ta slovenski standard je istoveten z: EN ISO 14720-2:2013
ICS:
81.060.10 Surovine Raw materials
SIST EN ISO 14720-2:2013 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 14720-2:2013

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SIST EN ISO 14720-2:2013


EUROPEAN STANDARD
EN ISO 14720-2

NORME EUROPÉENNE

EUROPÄISCHE NORM
March 2013
ICS 81.060.10
English Version
Testing of ceramic raw and basic materials - Determination of
sulfur in powders and granules of non-oxidic ceramic raw and
basic materials - Part 2: Inductively coupled plasma optical
emission spectrometry (ICP/OES) or ion chromatography after
burning in an oxygen flow (ISO 14720-2:2013)
Essais des matières premières pour produits réfractaires - Prüfung keramischer Roh- und Werkstoffe - Bestimmung
Dosage du soufre dans les matières premières non des Schwefelgehaltes in pulver- und kornförmigen
oxydantes sous forme de poudre et de granulés - Partie 2: nichtoxidischen keramischen Roh- und Werkstoffen - Teil
Spectrométrie d'émission optique avec plasma induit par 2: Optische Emissionsspektrometrie mit induktiv
haute fréquence (ICP/OES) ou chromatographie ionique gekoppeltem Plasma (ICP OES) oder
après combustion dans un courant d'oxygène (ISO 14720- Ionenchromatographie (IC) nach Verbrennung im
2:2013) Sauerstoffstrom (ISO 14720-2:2013)
This European Standard was approved by CEN on 16 February 2013.

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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 14720-2:2013: E
worldwide for CEN national Members.

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SIST EN ISO 14720-2:2013
EN ISO 14720-2:2013 (E)
Contents Page
Foreword . 3

2

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SIST EN ISO 14720-2:2013
EN ISO 14720-2:2013 (E)
Foreword
This document (EN ISO 14720-2:2013) has been prepared by Technical Committee ISO/TC 33 "Refractories"
in collaboration with Technical Committee CEN/TC 187 “Refractory products and materials” the secretariat of
which is held by BSI.
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 2013, and conflicting national standards shall be
withdrawn at the latest by September 2013.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
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, Former Yugoslav Republic of Macedonia, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
Endorsement notice
The text of ISO 14720-2:2013 has been approved by CEN as EN ISO 14720-2:2013 without any modification.

3

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SIST EN ISO 14720-2:2013

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SIST EN ISO 14720-2:2013
INTERNATIONAL ISO
STANDARD 14720-2
First edition
2013-03-01
Testing of ceramic raw and basic
materials — Determination of sulfur
in powders and granules of non-oxidic
ceramic raw and basic materials —
Part 2:
Inductively coupled plasma optical
emission spectrometry (ICP/OES) or
ion chromatography after burning in
an oxygen flow
Essais des matières premières pour produits réfractaires — Dosage
du soufre dans les matières premières non oxydantes sous forme de
poudre et de granulés —
Partie 2: Spectrométrie d’émission optique avec plasma induit par
haute fréquence (ICP/OES) ou chromatographie ionique après
combustion dans un courant d’oxygène
Reference number
ISO 14720-2:2013(E)
©
ISO 2013

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SIST EN ISO 14720-2:2013
ISO 14720-2:2013(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2013
All rights reserved. Unless otherwise specified, 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
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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 2013 – All rights reserved

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SIST EN ISO 14720-2:2013
ISO 14720-2:2013(E)

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Interferences . 2
5.1 ICP/OES . 2
5.2 Ion chromatography . 2
6 Apparatus . 3
7 Reagents . 3
8 Sampling and sample preparation . 4
9 Preparation . 4
9.1 Combustion device . 4
9.2 Oxygen (7.10) . 4
9.3 Inductively coupled plasma optical emission spectrometer (6.7) . 4
9.4 Ion chromatograph (6.8) . 4
10 Calibration . 4
10.1 Inductively coupled plasma optical emission spectrometer . 4
10.2 Ion chromatograph . 4
11 Performance . 5
11.1 Determination of the blank value . 5
11.2 Determination of the sulfur content . 5
12 Calculation and report of the results. 5
13 Precision . 6
13.1 Repeatability . 6
13.2 Reproducibility . 6
14 Test report . 6
Annex A (informative) Example of a combustion device . 7
Annex B (informative) Example for suitable operating parameters for the determination of sulfur
by ion chromatography . 8
Annex C (informative) Example for suitable operating parameters for the determination of sulfur
by inductively coupled plasma optical emission spectroscopy .9
Annex D (informative) Results of the round-robin test.10
Annex E (informative) Information regarding the validation of the uncertainty of the
mean value .13
Annex F (informative) Commercial Certified Reference Materials (CRM) .14
Bibliography .15
© ISO 2013 – All rights reserved iii

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SIST EN ISO 14720-2:2013
ISO 14720-2:2013(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 14720-2 was prepared by Technical Committee ISO/TC 33, Refractories.
ISO 14720 consists of the following parts, under the general title Testing of ceramic raw and basic
materials — Determination of sulfur in powders and granules of non-oxidic ceramic raw and basic materials:
— Part 1: Infrared measurement methods
— Part 2: Inductively coupled plasma optical emission spectrometry (ICP/OES) or ion chromatography
after burning in an oxygen flow
iv © ISO 2013 – All rights reserved

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SIST EN ISO 14720-2:2013
INTERNATIONAL STANDARD ISO 14720-2:2013(E)
Testing of ceramic raw and basic materials —
Determination of sulfur in powders and granules of non-
oxidic ceramic raw and basic materials —
Part 2:
Inductively coupled plasma optical emission
spectrometry (ICP/OES) or ion chromatography after
burning in an oxygen flow
1 Scope
This part of ISO 14720 defines a method for the determination of sulfur in powdered and granular non-
oxidic ceramic raw materials and materials, which are completely oxidized at a higher temperature in
an oxygen atmosphere, e.g. carbon and graphite materials.
For materials which are not completely oxidizable under these conditions, it is possible to determine
sulfur that can be released under these conditions, e.g. the adherent sulfur.
This part of ISO 14720 is applicable for materials with mass fractions of sulfur ≤ 10 % and mass fractions
of ash < 20 %, The defined method is limited for materials with mass fractions of barium < 10 mg/kg,
because the sulfur bonded in barium sulfate is not detectable with this method.
For the lower detection limit of this method, a mass fraction of sulfur of 0,5 mg/kg in the case of
inductively coupled plasma optical emission spectrometry (ICP/OES) and 5 mg/kg in the case of ion
chromatography (IC) has to be considered as a recommended value.
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 11885, Water quality — Determination of selected elements by inductively coupled plasma optical
emission spectrometry (ICP-OES)
ISO 10304-1, Water quality — Determination of dissolved anions by liquid chromatography of ions — Part 1:
Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
sulfur content
mass fraction of inorganic and organic bound sulfur
4 Principle
The dried sample is oxidized in a flow of oxygen at a temperature of 1 100 °C using a porcelain crucible.
The resulting sulfur oxides are absorbed in a solution of sodium hydroxide and hydrogen peroxide. The
© ISO 2013 – All rights reserved 1

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SIST EN ISO 14720-2:2013
ISO 14720-2:2013(E)

remaining material (ash) is dissolved and combined with the absorption liquid in the case of calcium-
sulfate-containing sample material. The concentration of sulfur in the sample solution is determined by
inductively coupled plasma optical emission spectrometry (ICP/OES) according to ISO 11885 or by ion
chromatography (IC) as sulfate according to ISO 10304-1 .
5 Interferences
5.1 ICP/OES
5.1.1 Spectral interferences
The compensation of spectral interferences is performed according to the manual of the manufacturer
of the spectrometer.
NOTE 1 Spectral interferences can be caused by:
a) Overlapping with the emission line of another element;
b) Overlapping with molecular bands;
c) Unspecific background (e.g. scattering, recombinations).
Overlapping of lines can be compensated for by arithmetical correction of the raw data if applicable.
Correction factors are determined by measuring at least one undisturbed additional emission line of the
interfering element and considering the relation of the intensity of this emission line to the emission line
which interferes with the analyte element.
In the case of overlapping with molecular bands, an alternative emission line has to be chosen.
NOTE 2 Unspecific background is usually compensated for by measuring the background signal in the
surroundings of the analyte emission line.
5.1.2 Physical interferences
To compensate physical interferences, suitable measures shall be taken.
NOTE Physical interferences occur as plasma interferences or as transport interferences. Both are caused by
a different behaviour of the calibration solution compared to the sample solution based on a different chemical
composition. Plasma interferences are caused by changes in plasma conditions, e.g. temperature distribution
and electron density, leading to a changed excitation of emission lines. Transport interferences are caused by
differences in physical characteristics of the calibration solution and sample solution, mainly density, viscosity
and surface tension.
Some of the transport interferences can be reduced by using appropriate (peristaltic) pumps. Plasma
interferences as well as transport interferences can be reduced significantly by using suitable reference
lines of a reference element with the same concentration in both the calibration and analyte solution
(internal standard). Other possibilities are to equalize the chemical composition of the calibration and
sample solution as much as possible (matrix matching) or to use
...