BS EN 15991:2015
$142.49
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)
| Published By | Publication Date | Number of Pages |
| BSI | 2015 | 30 |
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.
PDF Catalog
| PDF Pages | PDF Title |
|---|---|
| 5 | European foreword |
| 6 | 1 Scope 2 Principle 3 Spectrometry |
| 7 | Figure 1 — Schematic configuration of the ETV-gas regime with the gas flows carrier-gas, bypass-gas, reaction-gas and shield-gas Figure 2 — Schematic design of the ETV-ICP-combination with an axial plasma (example) |
| 8 | Figure 3 — Schematic configuration of the transition area between graphite- and transport-tube 4 Apparatus 5 Reagents and auxiliary material |
| 9 | 6 Sampling and sample preparation 7 Calibration |
| 10 | 8 Procedure |
| 11 | 9 Wavelength and working range 10 Calculation of the results and evaluation |
| 12 | 11 Reporting of results 12 Precision 12.1 Repeatability 12.2 Reproducibility 13 Test report |
| 13 | Annex A (informative) Results of interlaboratory study |
| 14 | Table A.1 — Data of precision determined at the SiC-sample nmp1 |
| 15 | Table A.2 — Data of precision determined at the SiC-sample 628 |
| 16 | Table A.3 — Data of precision determined at the SiC-sample 8517 certified later as reference material BAM-S003 |
| 17 | Table A.4 — Statistical results summarized in intervals |
| 18 | Annex B (informative) Wavelength and working range Table B.1 — Recommended spectral lines and working ranges for SiC |
| 19 | Annex C (informative) Possible interferences and their elimination C.1 General C.2 Spectral interferences C.2.1 Line coincidences C.2.2 Band coincidences |
| 20 | C.2.3 Background influence C.2.4 Line reversal, self-absorption C.2.5 Unspecific radiation C.3 Non-spectral interferences C.3.1 Interferences by the physical characteristics of the sample C.3.2 Interferences by depositions C.3.3 Interferences by carry-over |
| 21 | C.3.4 Ionization interferences C.3.5 Changing of the electrical coupling efficiency C.4 Conclusion |
| 22 | Annex D (informative) Information regarding the evaluation of the uncertainty of the mean value |
| 23 | Annex E (informative) Commercial certified reference materials |
| 24 | Annex F (informative) Information regarding the validation of an analytical method based on liquid standards in the example of SiC and graphite |
| 25 | Figure F.1 — Comparison of the calibration function of liquid calibration solutions and powdered calibration samples |
| 26 | Bibliography |
