DIN 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 plh.pdf

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1、February 2016 English price group 13No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 81.060.10!%LSB“2414831www.din.d

2、eDIN EN 15991Testing 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);English version EN 15991:2015,English trans

3、lation of DIN EN 15991:2016-02Prfung keramischer Roh- und Werkstoffe Direkte Bestimmung der Massenanteile von Spurenverunreinigungen in pulver- und kornfrmigem Siliciumcarbid mittels optischer Emissionsspektroskopie mit induktiv gekoppeltem Plasma (ICP OES) und elektrothermischer Verdampfung (ETV);E

4、nglische Fassung EN 15991:2015,Englische bersetzung von DIN EN 15991:2016-02Essais sur matriaux cramiques et basiques Dtermination directe des fractions massiques dimpurets dans les poudres et les granuls de cabure de silicium par spectroscopie dmission optique plasma induit par haute frquence (ICP

5、OES) avec vaporisation lectrothermique (ETV);Version anglaise EN 15991:2015,Traduction anglaise de DIN EN 15991:2016-02SupersedesDIN EN 15991:2011-04www.beuth.deDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.Document comprises 27 p

6、ages 03.16 DIN EN 15991:2016-02 2 A comma is used as the decimal marker. National foreword This document (EN 15991:2015) has been prepared by Technical Committee CEN/TC 187 “Refractory products and materials” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation

7、 was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-02-64 AA Chemische Analyse von nichtoxidischen keramischen Roh- und Werkstoffen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: I

8、SO 5725-2 DIN ISO 5725-2 ISO 5725-4 DIN ISO 5725-4 Amendments This standard differs from DIN EN 15991:2011-04 as follows: a) dichlorodifluoromethane (CCl2F2) is only to be used as a halogenating agent; b) the standard has been editorially revised. Previous editions DIN 51096: 2008-07 DIN EN 15991: 2

9、011-04 National Annex NA (informative) Bibliography DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 5725-4, Accuracy (trueness and precision)

10、of measurement methods and results Part 4: Basic methods for the determination of the trueness of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15991 November 2015 ICS 81.060.10 Supersedes EN 15991:2011English Version Testing of ceramic and basic materials - Dire

11、ct 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 matriaux cramiques et basiques - Dtermination directe des fractions massiques dimpurets

12、dans les poudres et les granuls de carbure de silicium par spectroscopie dmission optique plasma induit par haute frquence (ICP OES) avec vaporisation lectrothermique (ETV) Prfung keramischer Roh- und Werkstoffe - Direkte Bestimmung der Massenanteile von Spurenverunreinigungen in pulver- und kornfrm

13、igem Siliciumcarbid mittels optischer Emissionsspektroskopie mit induktiv gekoppeltem Plasma (ICP OES) und elektrothermischer Verdampfung (ETV) This European Standard was approved by CEN on 3 October 2015. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the

14、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 e

15、xists 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

16、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

17、, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means res

18、erved worldwide for CEN national Members. Ref. No. EN 15991:2015 EEN 15991:2015 (E) 2 Contents Page European foreword . 3 1 Scope 4 2 Principle . 4 3 Spectrometry 4 4 Apparatus . 6 5 Reagents and auxiliary material 6 6 Sampling and sample preparation 7 7 Calibration . 7 8 Procedure. 8 9 Wavelength a

19、nd working range . 9 10 Calculation of the results and evaluation . 9 11 Reporting of results . 10 12 Precision 10 12.1 Repeatability 10 12.2 Reproducibility . 10 13 Test report 10 Annex A (informative) Results of interlaboratory study 11 Annex B (informative) Wavelength and working range . 16 Annex

20、 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 analy

21、tical method based on liquid standards in the example of SiC and graphite. 22 Bibliography . 24 DIN EN 15991:2016-02 EN 15991:2015 (E) 3 European foreword This document (EN 15991:2015) has been prepared by Technical Committee CEN/TC 187 “Refractory products and materials”, the secretariat of which i

22、s 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 May 2016 and conflicting national standards shall be withdrawn at the latest by May 2016. Attention is drawn to the possibility that

23、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. This document supersedes EN 15991:2011. According to the CEN-CENELEC Internal Regulations, the national standards organizations o

24、f 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, Net

25、herlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 15991:2016-02 EN 15991:2015 (E) 4 1 Scope This European Standard defines a method for the determination of the trace element concentrations of Al, Ca, Cr, Cu, Fe, Mg, Ni

26、, 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

27、 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 choos

28、ing 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, so

29、ot, 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 mat

30、erial, 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 o

31、ptical 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

32、 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 emis

33、sion 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. Contrary to the wet chemical analysis from dilution in

34、 ICP OES the classical sample digestion is replaced by electrothermal vaporization 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 th

35、e 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 incompletely or not evaporating need a suitable reaction gas (halogenating agent) to be converted into a form that is easy to transpo

36、rt (see 1, 3, 5 and 10.) Dichlorodifluoromethane (CCl2F2) shall be used as halogenating agent. Compared to other halogen containing carbon compounds CCl2F2provides optimum analyte release and transport efficiency. CCl2F2is required for simultaneous determination of the elements listed in Clause 1. T

37、he results of the interlaboratory study (see Annex A) were obtained using CCl2F2as reaction gas. The dry aerosol is introduced into the ICP plasma by the injector tube and there excited for the emission of light (see Figure 1, Figure 2 and Figure 3). DIN EN 15991:2016-02 EN 15991:2015 (E) 5 Key 1 gr

38、aphite 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 by

39、pass-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) DIN EN 15991:2016-02 EN 15991:2015 (E) 6 Key 1 Al2O3-tr

40、ansport 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 commercia

41、l 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 sign

42、al 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 backgr

43、ound. 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 sui

44、ted 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

45、 (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

46、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 materia

47、l Only analytical grade reagents shall be used unless stated otherwise. DIN EN 15991:2016-02 EN 15991:2015 (E) 7 5.1 Sample boats of graphite (spectral grade) adapted in size to the graphite tube of the ETV, baked out for the necessary purity. 5.2 Calibration samples with well-defined mass fractions

48、 of trace-impurities, preferably certified reference materials (CRM). NOTE For silicon nitride, silicon carbide and boron carbide certified reference material is available for main-, minor- and trace-components. (For CRMs, see Annex E.) 5.3 Calibration solutions, made of tested stock solutions of th

49、e elements to be analysed. 5.4 Reaction gas, Dichlorodifluoromethane (CCl2F2) NOTE Dichlorodifluoromethane is the most effective reaction gas, some alternative reaction gases have serious disadvantages. According to the EU-regulation (see 12) of materials influencing the ozone layer, this chemical product is allowed for laboratory use and for the use as a starting substance. CCl2F2is completely decomposed in the hot graph