EN 15991:2025
(Main)Testing of ceramic raw materials and ceramic materials - Direct determination of mass fractions of impurities in powders and granules of silicon carbide by inductively coupled plasma optical emission spectrometry with electrothermal vaporisation (ETV-ICP-OES)
Testing of ceramic raw materials and ceramic materials - Direct determination of mass fractions of impurities in powders and granules of silicon carbide by inductively coupled plasma optical emission spectrometry with electrothermal vaporisation (ETV-ICP-OES)
This document specifies a method for the determination of the mass fractions of the elements Al, Ca, Cr, Cu, Fe, Mg, Ni, Ti, V and Zr in powdered and granular silicon carbide.
Dependent on element, emission lines, plasma conditions and sample mass, this test method is applicable for mass fractions of the above trace contaminations from about 0,1 mg/kg to about 1 000 mg/kg, after evaluation also from 0,001 mg/kg to about 5 000 mg/kg.
NOTE 1 Generally for optical emission spectrometry using inductively coupled plasma and electrothermal vaporization (ETV-ICP-OES) there is a linear working range of up to four orders of magnitude. This range can be expanded for the respective elements by variation of the sample mass or by choosing emission lines with different sensitivity.
After adequate verification, this document is also applicable to further metallic elements (excepting Rb and Cs) and some non-metallic contaminations (like P and S) and other allied non-metallic powdered or granular materials like carbides, nitrides, graphite, soot, coke, coal, and some other oxidic materials (see [1], [4], [5], [6], [7], [8], [9] and [10]).
NOTE 2 There is positive experience with materials like, for example, graphite, boron carbide (B4C), silicon nitride (Si3N4), boron nitride (BN) and several metal oxides as well as with the determination of P and S in some of these materials.
Prüfung keramischer Roh- und Werkstoffe - Direkte Bestimmung der Massenanteile von Spurenverunreinigungen in pulver- und kornförmigem Siliciumcarbid mittels optischer Emissionsspektroskopie mit induktiv gekoppeltem Plasma und elektrothermischer Verdampfung (ETV-ICP-OES)
Dieses Dokument legt ein Verfahren zur Bestimmung der Massenanteile der Elemente Al, Ca, Cr, Cu, Fe, Mg, Ni, Ti, V und Zr in pulver- und kornförmigem Siliciumcarbid fest.
Dieses Prüfverfahren gilt in Abhängigkeit von Element, Emissionslinien, Plasmabedingungen und Probenmasse für Massenanteile der o. g. Spurenverunreinigungen von etwa 0,1 mg/kg bis etwa 1 000 mg/kg, nach Evaluierung auch von 0,001 mg/kg bis etwa 5 000 mg/kg.
ANMERKUNG 1 In der Regel gilt für die optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma und elektrothermischer Verdampfung (ETV-ICP-OES) ein linearer Arbeitsbereich von bis zu vier Größenordnungen. Dieser Bereich kann für die einzelnen Elemente durch Änderung der Probenmasse oder durch die Auswahl verschieden empfindlicher Emissionslinien erweitert werden.
Nach entsprechender Prüfung ist dieses Dokument auch auf weitere metallische Elemente (mit Ausnahme von Rb und Cs) und einige nichtmetallische Verunreinigungen (wie z. B. P und S) und andere verwandte nichtmetallische pulver- und kornförmige Werkstoffe, wie z. B. Carbide, Nitride, Graphit, Ruß, Koks, Kohle, sowie weiterer oxidischer Werkstoffe anwendbar (siehe [1], [4], [5], [6], [7], [8], [9] und [10]).
ANMERKUNG 2 Es gibt positive Erfahrungen zu Werkstoffen, wie z. B. Graphit, Borcarbid (B4C), Siliciumnitrid (Si3N4), Bornitrid (BN) und verschiedenen Metalloxiden sowie zur Bestimmung von P und S in einigen dieser Werkstoffe.
Essai des matières premières céramiques et des matériaux céramiques - Détermination directe des fractions massiques d'impuretés dans les poudres et les granulés de carbure de silicium par spectroscopie d'émission optique avec plasma induit par haute fréquence avec vaporisation électrothermique (ETV-ICP-OES)
Le présent document définit une méthode pour la détermination de la fraction massique des éléments Al, Ca, Cr, Cu, Fe, Mg, Ni, Ti, V et Zr dans les poudres et les granulés de carbure de silicium.
Selon l’élément, les raies d’émission, les conditions de plasma et la masse de l’échantillon, cette méthode d’essai s’applique aux fractions massiques des contaminants à l’état de traces précédemment mentionnés comprises entre 0,1 mg/kg environ et 1 000 mg/kg environ, après évaluation, également comprises entre 0,001 mg/kg et 5 000 mg/kg environ.
NOTE 1 Pour la spectroscopie d’émission optique avec plasma induit par haute fréquence et la vaporisation électrothermique (ETV-ICP-OES), on dispose généralement d’une plage de fonctionnement linéaire allant jusqu'à quatre ordres de grandeur. Cette plage peut être étendue pour les éléments respectifs en changeant la masse de l’échantillon ou en choisissant des raies d’émission de sensibilité différente.
Après vérification adéquate, le présent document est également applicable à d’autres éléments métalliques (excepté Rb et Cs), à certains contaminants non métalliques (tels que P et S) et à d’autres matériaux non métalliques voisins sous forme de poudres ou de granulés, tels que les carbures, les nitrures, le graphite, la suie, le coke, le charbon, et à certains autres matériaux obtenus par oxydation (voir [1], [4], [5], [6], [7], [8], [9] et [10]).
NOTE 2 L’expérience s’avère positive avec des matériaux comme, par exemple, le graphite, le carbure de bore (B4C), le nitrure de silicium (Si3N4), le nitrure de bore (BN) et plusieurs oxydes métalliques ainsi que la détermination du P et du S dans certains de ces matériaux.
Preskušanje keramičnih surovin in keramičnih materialov - Neposredno določevanje masnih frakcij nečistoč v prahu in zrnih silicijevega karbida z optično emisijsko spektroskopijo in induktivno sklopljeno plazmo z elektrotermičnim izparevanjem (ETV-ICP-OES)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-december-2025
Preskušanje keramičnih surovin in keramičnih materialov - Neposredno
določevanje masnih frakcij nečistoč v prahu in zrnih silicijevega karbida z optično
emisijsko spektroskopijo in induktivno sklopljeno plazmo z elektrotermičnim
izparevanjem (ETV-ICP-OES)
Testing of ceramic raw materials and ceramic materials - Direct determination of mass
fractions of impurities in powders and granules of silicon carbide by inductively coupled
plasma optical emission spectrometry with electrothermal vaporisation (ETV-ICP-OES)
Prüfung keramischer Roh- und Werkstoffe - Direkte Bestimmung der Massenanteile von
Spurenverunreinigungen in pulver- und kornförmigem Siliciumcarbid mittels optischer
Emissionsspektroskopie mit induktiv gekoppeltem Plasma und elektrothermischer
Verdampfung (ETV-ICP-OES)
Essai des matières premières céramiques et des matériaux céramiques - Détermination
directe des fractions massiques d'impuretés dans les poudres et les granulés de carbure
de silicium par spectroscopie d'émission optique avec plasma induit par haute fréquence
avec vaporisation électrothermique (ETV-ICP-OES)
Ta slovenski standard je istoveten z: EN 15991:2025
ICS:
81.060.10 Surovine Raw materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 15991
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2025
EUROPÄISCHE NORM
ICS 81.060.10 Supersedes EN 15991:2015
English Version
Testing of ceramic raw materials and ceramic materials -
Direct determination of mass fractions of impurities in
powders and granules of silicon carbide by inductively
coupled plasma optical emission spectrometry with
electrothermal vaporisation (ETV-ICP-OES)
Essai des matières premières céramiques et des Prüfung keramischer Roh- und Werkstoffe - Direkte
matériaux céramiques - Détermination directe des Bestimmung der Massenanteile von
fractions massiques d'impuretés dans les poudres et Spurenverunreinigungen in pulver- und kornförmigem
les granulés de carbure de silicium par spectroscopie Siliciumcarbid mittels optischer
d'émission optique avec plasma induit par haute Emissionsspektroskopie mit induktiv gekoppeltem
fréquence avec vaporisation électrothermique (ETV- Plasma und elektrothermischer Verdampfung (ETV-
ICP-OES) ICP-OES)
This European Standard was approved by CEN on 27 July 2025.
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, Türkiye 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
© 2025 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15991:2025 E
worldwide for CEN national Members.
Contents Page
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Spectrometry . 5
6 Apparatus . 7
7 Reagents and auxiliary material . 7
8 Sampling and sample preparation . 8
9 Calibration . 8
10 Procedure. 9
11 Emission lines and working range . 10
12 Calculation of the results and evaluation . 10
13 Reporting of results . 11
14 Precision . 11
14.1 Repeatability . 11
14.2 Reproducibility . 11
15 Test report . 11
Annex A (informative) Results of interlaboratory study . 12
Annex B (informative) Emission lines and working range . 17
Annex C (informative) Possible interferences and their elimination . 19
Annex D (informative) Information regarding the evaluation of the uncertainty of the mean
value . 22
Annex E (informative) Commercial certified reference materials . 23
Annex F (informative) Calibration using aqueous solutions and powdered calibration samples
........................................................................................................................................................................ 24
Bibliography . 27
European foreword
This document (EN 15991:2025) has been prepared by 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 March 2026, and conflicting national standards shall be
withdrawn at the latest by March 2026.
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 15991:2015.
— Clause 2 and Clause 3 have been added, noting that they neither add any normative references nor
terms and definitions to the document;
— Clause 4 adds significantly more detail about the analysis and process;
— Clause 5 provides additional information on the spectrometry methodology;
— Annex B, Table B.1 provides additional information on the limits of determination.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Türkiye and the United
Kingdom.
1 Scope
This document specifies a method for the determination of the mass fractions of the elements Al, Ca, Cr,
Cu, Fe, Mg, Ni, Ti, V and Zr in powdered and granular silicon carbide.
Dependent on element, emission lines, plasma conditions and sample mass, this test method is applicable
for mass fractions of the above trace contaminations from about 0,1 mg/kg to about 1 000 mg/kg, after
evaluation also from 0,001 mg/kg to about 5 000 mg/kg.
NOTE 1 Generally for optical emission spectrometry using inductively coupled plasma and electrothermal
vaporization (ETV-ICP-OES) there is a linear working range of up to four orders of magnitude. This range can be
expanded for the respective elements by variation of the sample mass or by choosing emission lines with different
sensitivity.
After adequate verification, this document is also applicable to further metallic elements (excepting Rb
and Cs) and some non-metallic contaminations (like P and S) and other allied non-metallic powdered or
granular materials like carbides, nitrides, graphite, soot, coke, coal, and some other oxidic materials (see
[1], [4], [5], [6], [7], [8], [9] and [10]).
NOTE 2 There is positive experience with materials like, for example, graphite, boron carbide (B C), silicon
nitride (Si N ), boron nitride (BN) and several metal oxides as well as with the determination of P and S in some of
3 4
these materials.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
4 Principle
For the determination of impurities in silicon carbide, ICP-OES is a suited method. The classic application
of ICP-OES is based on the nebulization of sample solutions. For silicon carbide, sample digestion by wet-
chemical methods is required to obtain these sample solutions, for example by melt-fusion or
acid/pressure-decomposition. These sample digestion procedures are time-consuming, require the use
of hazardous chemicals, deteriorate the detection limits due to the dilution of the sample and the
possibility of introduction of impurities as well as analyte losses represents a source of systematic errors.
With ETV-ICP-OES, the impurities are measured directly from the powdered silicon carbide sample, thus
avoiding sample digestion and the associated disadvantages. Compared to wet-chemical ICP-OES
methods, ETV-ICP-OES requires more effort for method development and is therefore particularly
suitable when many samples of one matrix are to be measured with high sample throughput and with
high detection sensitivity.
In ETV-ICP-OES, sample introduction by nebulization of liquids is replaced by the electrothermal
vaporization of solid samples at high temperatures in the graphite tube furnace of the ETV-system.
The sample material, crushed if necessary, is evaporated in an argon carrier-gas stream in a graphite boat
in the graphite tube furnace of the ETV-system. A suitable design of the furnace (see Figures 1 and 2) and
an optimized gas flow in the transition area between graphite tube and transport tube (see Figure 3)
ensure that the sample vapour is transferred into a form that is transported to the ICP-OES with almost
no losses (see [5], [6], [7], [8], [10]). Elements, for example titanium or zirconium, forming refractory
carbides that are incompletely or not evaporating need to be converted in the graphite tube furnace into
a chemical form which easily evaporates. For this purpose, a suitable reaction gas (halogenating agent)
is mixed to the argon carrier-gas stream (see Figures 1 and 2) which converts the carbides into volatile
halides (see [1], [3], [5] and [10].)
The evaporation products containing the element traces are transported by the transport tube as dry
aerosol to the ICP-torch, injected into the plasma and there excited for the emission of optical radiation
(see Figure 2).
5 Spectrometry
Optical emission spectrometry is based on the generation of line spectra of excited atoms or ions, where
each emission line is associated with an element and the line intensities are proportional to the mass
fractions of the elements in the analysed sample.
In a simultaneous emission spectrometer in, for example Paschen-Runge- or Echelle-configuration, the
optical radiation is dispersed. The intensities of suited emission lines or background positions are
registered with applicable detectors like photomultipliers (PMT), charge coupled devices (CCD),
complementary metal-oxide semiconductor (CMOS), charge injection devices (CID), and ser
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.