EN 15991:2011
(Main)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)
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 vaporisation (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 Emissionsspektrometrie 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. angeführten 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 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 standard opredeljuje metodo za določevanje koncentracij elementov v sledovih Al, Ca, Cr, Cu, Fe, Mg, Ni, Ti, V in Zr v prahu in zrnih silicijevega karbida.
Glede na element, valovno dolžino, pogoje plazme in težo ta preskusna metoda velja za masne vsebnosti zgoraj navedenih kontaminacij v sledovih od okrog 0,1 mg/kg do okrog 1000 mg/kg, po ovrednotenju tudi od 0,001 mg/kg do okrog 5000 mg/kg.
OPOMBA 1 V splošnem za optično emisijsko spektroskopijo z induktivno sklopljeno plazmo (ICP OES) in elektrotermično uparevanje (ETV) velja linearni delovni razpon do štirih redov velikosti. Ta razpon se lahko razširi za posamezne elemente s spreminjanjem teže ali z izbiro linij z drugačno občutljivostjo.
Po ustreznem preverjanju standard velja tudi za druge kovinske elemente (razen Rb in Cs) in nekatere nekovinske kontaminacije (kot sta P in S) ter druge sorodne nekovinske materiale v prahu ali zrnih, kot so karbidi, nitridi, grafit, saje, koks, premog in nekateri drugi oksidni materiali (glej [1], [4], [5], [6], [7], [8], [9] in [10]).
OPOMBA 2 Obstajajo pozitivne izkušnje z materiali, kot so npr. grafit, B4C, Si3N4, BN in več kovinskih oksidov, ter z določevanjem P in S v nekaterih od teh materialov.
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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 Emissionsspektrometrie 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 15991:2011SIST EN 15991:2011en,fr,de01-november-2011SIST EN 15991:2011SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15991
January 2011 ICS 81.060.10 English Version
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) 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)
Prüfung keramischer Roh- und Werkstoffe - Direkte Bestimmung der Massenanteile von Spurenverunreinigungen in pulver- und kornförmigem Siliciumcarbid mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES) und elektrothermischer Verdampfung (ETV) This European Standard was approved by CEN on 10 December 2010.
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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15991:2011: ESIST EN 15991:2011
Results of interlaboratory study . 11Annex B (informative)
Wavelength and working range . 16Annex C (informative)
Possible interferences and their elimination . 18Annex D (informative)
Information regarding the evaluation of the uncertainty of the mean value . 21Annex E (informative)
Commercial certified reference materials . 22Annex F (informative)
Information regarding the validation of an analytical method based on liquid standards at the example of SiC and graphite . 23Bibliography . 26 SIST EN 15991:2011
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 vaporisation (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. 2 Principle 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 unit. The evaporation products containing the element traces are transported as a dry aerosol into the plasma of the ICP-torch and there excited for the emission of optical radiation. In a simultaneous emission spectrometer in, for example Paschen-Runge- or Echelle-configuration, the optical radiation is dispersed. The intensities of suited spectral lines or background positions are registered with applicable detectors like photomultipliers (PMT), charge coupled devices (CCD), charge injection devices (CID), and serial coupled devices (SCD). By comparison of the intensities of the element-specific spectral lines of the sample with calibration samples of known composition, the mass fractions of the sample elements are determined. 3 Spectrometry Optical emission spectrometry is based on the generation of line spectra of excited atoms or ions, where each spectral line is associated with an element and the line intensities are proportional to the mass fractions of the elements in the analysed sample.
In contrary to the wet chemical analysis from dilution in ICP OES the classical sample digestion is replaced by electrothermal vaporisation at high temperatures in a graphite furnace. By a suitable design of the furnace (see Figures 1 and 2) and a suited gas regime in the transition area graphite tube / transport tube (see Figure 1), it is ensured that the sample vapour is carried over into a form that is to transport effectively (see [5], [6], [7], [8], [10]). Carbide forming elements, for example titanium, zirconium, that are not or incompletely evaporating need a suited modifier, like a halogenation agent, preferably dichlorodifluoromethane, to be converted into a form that is easy to transport (see [1], [3], [5] and [10].) The dry aerosol is introduced into the ICP plasma by the injector tube and there excited for the emission of light (see Figures 1 to 3). SIST EN 15991:2011
Key 1 graphite tube with boat and sample 5 bypass gas (Ar) 2 carrier gas (Ar) 6 aerosol 3 reaction gas (Freon) 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 and shield-gas
Key 1 graphite tube furnace 6 bypass-gas (Ar) 2 pyrometer 7 aerosol 3 carrier gas (Ar) + reaction gas 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 15991:2011
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 Figures 1 to 3 show a well established commercial instrument. 4 Apparatus 4.1 Common 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 vaporisation 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 Echelle or similar CID systems are 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 vaporisation 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 measurement of the graphite boat connected to a feed forward control of the power supply) 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. SIST EN 15991:2011
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