EN 15991:2015

Testing of ceramic and basic materials - Direct determination of mass fractions of impurities in powders and granules of silicon carbide by inductively coupled plasma optical emission spectrometry (ICP OES) with electrothermal vaporisation (ETV)

This European Standard defines a method for the determination of the trace element concentrations of Al, Ca, Cr, Cu, Fe, Mg, Ni, Ti, V and Zr in powdered and granular silicon carbide.
Dependent on element, wavelength, plasma conditions and weight, this test method is applicable for mass contents 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 (ICP OES) and electrothermal vaporization (ETV) 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 weight or by choosing lines with different sensitivity.
After adequate verification, the standard 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, B4C, Si3N4, 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 (ICP OES) und elektrothermischer Verdampfung (ETV)

Diese Europäische Norm legt ein Verfahren zur Bestimmung der Gehalte der Spurenelemente Al, Ca, Cr, Cu, Fe, Mg, Ni, Ti, V und Zr in pulver- und kornförmigem Siliciumcarbid fest.
Das festgelegte Prüfverfahren gilt in Abhängigkeit von Element, Wellenlänge, Plasmabedingungen und Einwaage für Massenanteile der o. g. Spurenverunreinigungen von etwa 0,1 mg/kg bis etwa 1 000 mg/kg, nach Prüfung 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 (ICP OES) und elektrothermischer Verdampfung (ETV) ein linearer Arbeitsbereich von bis zu vier Größenordnungen. Dieser Bereich kann für die einzelnen Elemente durch Änderung der Einwaage oder durch die Auswahl verschieden empfindlicher Linien erweitert werden.
Nach entsprechender Prüfung ist die Norm auch auf weitere metallische Elemente (mit Ausnahme von Rb und Cs) und einige nichtmetallische Verunreinigungen (wie z. B. P und S) und andere artverwandte nichtmetallische pulver  und kornförmige Werkstoffe, wie z. B. Carbide, Nitride, Graphit, Ruß, Koks, Kohle, sowie eine Reihe weiterer oxidischer Werkstoffe anwendbar (siehe [1], [4], [5], [6], [7], [8], [9] und [10]).
ANMERKUNG 2   Es liegen positive Erfahrungen zu Werkstoffen, wie z. B. Graphit, B4C, Si3N4, BN und verschiedenen Metalloxiden sowie zur Bestimmung von P und S in einigen dieser Werkstoffe vor.

Essais sur matériaux céramiques et basiques - Détermination directe des fractions massiques d'impuretés dans les poudres et les granulés de carbure de silicium par spectroscopie d'émission optique à plasma induit par haute fréquence (ICP OES) avec vaporisation électrothermique (ETV)

La présente Norme définit une méthode pour la détermination de concentrations d'éléments traces d'Al, Ca, Cr, Cu, Fe, Mg, Ni, Ti, V et Zr dans les poudres et les granulés de carbure de silicium.  
Selon l’élément, la longueur d’onde, les conditions de plasma et le poids, cette méthode d’essai s’applique à des teneurs en masse 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 (ICP OES) et la vaporisation électrothermique (ETV), 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 le poids ou en choisissant des raies de sensibilité différente.
Après vérification adéquate, la présente Norme 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 le graphite, B4C, Si3N4, BN, par exemple, et plusieurs oxydes métalliques et en déterminant le P et le S dans certains de ces matériaux.

Preskušanje keramičnih surovin in osnovnih materialov - Neposredno določevanje masnih frakcij nečistoč v prahu in zrnih silicijevega karbida z optično emisijsko spektroskopijo in induktivno sklopljeno plazmo (ICP OES) z elektrotermičnim uparevanjem (ETV)

Ta evropski standard opisuje metodo za določevanje koncentracij elementov v sledovih za Al, Ca, Cr, Cu, Fe, Mg, Ni, Ti, V in Zr v prahu in zrnih silicijevega karbida.
Odvisno od elementa, valovne dolžine, pogojev plazme in teže, se ta preskusna metoda uporablja za masne frakcije nečistoč nad ravnjo sledi od približno 0,1 mg/kg do približno 1 000 mg/kg, po ocenjevanju tudi od 0,001 mg/kg do približno 5 000 mg/kg.
OPOMBA 1: Splošno imata optična emisijska spektrometrija z induktivno sklopljeno plazmo (ICP OES) in elektrotermično uparjevanje (ETV) linearno delovno območje z do štirimi velikostnimi razredi. To območje je mogoče razširiti za zadevne elemente s spreminjanjem teže ali z izbiro linij z različnimi občutljivostmi.
Po zadostnem preverjanju se lahko standard uporablja tudi za druge kovinske elemente (z izjemo Rb in Cs) in nekatere nekovinske nečistoče (kot sta P in S) ter druge povezane nekovinske materiale v prahu in zrnih, kot so karbidi, nitridi, grafit, saje, premog, koks in nekateri drugi oksidni materiali (glejte [1], [4], [5], [6], [7], [8], [9] in [10]).
OPOMBA 2: Pozitivne izkušnje obstajajo za materiale, kot so grafit, B4C, Si3N4, BN in nekateri kovinski oksidi, ter za določevanje P in S v nekaterih od teh materialov.

General Information

• Status: Published
• Publication Date: 24-Nov-2015
• ICS: 81.060.10 - Raw materials
• Technical Committee: CEN/TC 187 - Refractory products and materials
• Drafting Committee: CEN/TC 187/WG 4 - Chemical analysis
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Completion Date: 11-Oct-2021
• Ref Project: SIST EN 15991:2016 - Testing of ceramic and basic materials - Direct determination of mass fractions of impurities in powders and granules of silicon carbide by inductively coupled plasma optical emission spectrometry (ICP OES) with electrothermal vaporisation (ETV)

Relations

• Replaces: EN 15991:2011 - Testing of ceramic and basic materials - Direct determination of mass fractions of impurities in powders and granules of silicon carbide by inductively coupled plasma optical emission spectrometry (ICP OES) with electrothermal vaporisation (ETV)
• Effective Date: 08-May-2013
• Revised: prEN 15991 - 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)
• Effective Date: 19-Jul-2023

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.RWHUPLþQLPPrüfung keramischer Roh- und Werkstoffe - Direkte Bestimmung der Massenanteile von Spurenverunreinigungen in pulver- und kornförmigem Siliciumcarbid mittels optischer Emissionsspektroskopie mit induktiv gekoppeltem Plasma (ICP OES) und elektrothermischer Verdampfung (ETV)Essais sur matériaux céramiques et basiques - Détermination directe des fractions massiques d'impuretés dans les poudres et les granulés de carbure de silicium par spectroscopie d'émission optique à plasma induit par haute fréquence (ICP OES) avec vaporisation électrothermique (ETV)Testing of ceramic and basic materials - Direct determination of mass fractions of impurities in powders and granules of silicon carbide by inductively coupled plasma optical emission spectrometry (ICP OES) with electrothermal vaporisation (ETV)81.060.10SurovineRaw materialsICS:Ta slovenski standard je istoveten z:EN 15991:2015SIST EN 15991:2016en,fr,de01-januar-2016SIST EN 15991:2016SLOVENSKI
STANDARDSIST EN 15991:20111DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15991
November
t r s w ICS
z sä r x rä s r Supersedes EN
s w { { sã t r s sEnglish Version
Testing of ceramic and basic materials æ Direct determination of mass fractions of impurities in powders and granules of silicon carbide by inductively coupled Essais sur matériaux céramiques et basiques æ Détermination directe des fractions massiques d 5impuretés dans les poudres et les granulés de carbure de silicium par spectroscopie d 5émission
Prüfung keramischer Rohæ und Werkstoffe æ Direkte Bestimmung der Massenanteile von Spurenverunreinigungen in pulveræ und kornförmigem Siliciumcarbid mittels optischer Emissionsspektroskopie mit induktiv gekoppeltem This European Standard was approved by CEN on
u October
t r s wä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
t r s w CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s w { { sã t r s w ESIST EN 15991:2016

Results of interlaboratory study . 11 Annex B (informative)
Wavelength and working range . 16 Annex C (informative)
Possible interferences and their elimination . 17 Annex D (informative)
Information regarding the evaluation of the uncertainty of the mean value . 20 Annex E (informative)
Commercial certified reference materials . 21 Annex F (informative)
Information regarding the validation of an analytical method based on liquid standards in the example of SiC and graphite. 22 Bibliography . 24
Key 1 graphite tube with boat and sample 5 bypass gas (Ar) 2 carrier gas (Ar) 6 aerosol 3 reaction gas (CCl2F2) 7 to the ICP torch 4 shield gas (Ar)
Figure 1 — Schematic configuration of the ETV-gas regime with the gas flows carrier-gas, bypass-gas, reaction-gas and shield-gas
Key 1 graphite tube furnace 6 bypass-gas (Ar) 2 pyrometer 7 aerosol 3 carrier gas (Ar) + reaction gas (CCl2F2) 8 transport tube 4 solid sample 9 ICP-torch 5 vapour 10 power supply 0 A to 400 A Figure 2 — Schematic design of the ETV-ICP-combination with an axial plasma (example) SIST EN 15991:2016

Key 1 Al2O3-transport tube 5 carrier gas evaporated sample 2 Al2O3-transition ring 6 bypass gas 3 nozzle 7 gas mixture in laminar flow 4 graphite tube
Figure 3 — Schematic configuration of the transition area between graphite- and transport-tube NOTE Figure 1, Figure 2 and Figure 3 show a well-established commercial instrument. 4 Apparatus 4.1 Common laboratory instruments and laboratory instruments according to 4.2 to 4.7. 4.2 ICP-emission spectrometer, simultaneous, preferably with the possibility to register transient emission signals and suited for the synchronised start of ETV vaporization cycle and signal registration. NOTE Especially for changing matrices the measurement of the spectral background near the analysis lines is beneficial, because by this the systematic and stochastic contributions of the analysis uncertainty can be decreased, the latter only by simultaneous measurement of the background. The use of spectrometers equipped with area- or array-detectors is an advantage in such cases as they allow a simultaneous background measurement, in addition to their possibility to save a lot of time in the analysis cycle. 4.3 Electrothermal vaporization system with graphite furnace with suited transition zone graphite tube / transport tube for optimised aerosol formation, to be connected to the injector tube of the ICP torch by a transport tube for example made of corundum, PTFE, PFA, PVC (cross-linked), with controlled gas flows (preferably with mass-flow-control) and furnace control (preferably with continuous online-temperature control of the graphite boat) for a reproducible control of the temperature development. 4.4 Tweezers, self-closing, made of a material preventing contamination. 4.5 Micro spatula, made of a material preventing contamination. 4.6 Microbalance, capable of reading to the nearest 0,01 mg. NOTE A microbalance with a direct reading of 0,001 mg is advantageous. 4.7 Mill or crusher, free of contamination, for example mortar made of a material that does not contaminate the sample with any of the analytes to be determined. 5 Reagents and auxiliary material Only analytical grade reagents shall be used unless stated otherwise. SIST EN 15991:2016
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