SIST EN 12698-2:2007
(Main)Chemical analysis of nitride bonded silicon carbide refractories - Part 2: XRD methods
Chemical analysis of nitride bonded silicon carbide refractories - Part 2: XRD methods
This standard describes methods for the determination of mineralogical phases typically apparent in nitride and oxy-nitride bonded silicon carbide refractory products using a Bragg-Brentano diffractometer.
It includes details of sample preparation and general principles for qualitative and quantitative analysis of mineralogical phase composition. Quantitative determination of ?-Si3N4, ?-Si3N4, Si2ON2, AlN, and SiAlON are described.
NOTE For the refinement procedures the total nitrogen content, analysed in accordance with EN 12698-1 is needed.
Chemische Analyse von feuerfesten Erzeugnissen aus nitridgebundenem Silicumcarbid - Teil 2: XRD-Verfahren
Analyse chimique des produits réfractaires contenant du carbure de silicium a liaison nitrure - Partie 2 : Méthodes de DRX
La présente norme décrit des méthodes destinées à déterminer les phases minéralogiques généralement présentes dans les produits réfractaires contenant du carbure de silicium lié au nitrure et à l’oxynitrure, au moyen d’un diffractomètre à géométrie Bragg-Brentano.
Elle contient des détails relatifs à la préparation des échantillons ainsi que des principes généraux de l’analyse qualitative et quantitative de la composition des phases minéralogiques. La détermination quantitative de -Si3N4, -Si3N4, Si2ON2, AlN et SiAlON est décrite.
NOTE Pour les modes opératoires d’affinement, il est nécessaire de connaître la teneur en azote total, analysée conformément au EN 12698-1.
Kemijska analiza nitrid silicijevega karbida - 2.del: XRD metode
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Chemical analysis of nitride bonded silicon carbide refractories - Part 2: XRD methodsKemijska analiza nitrid silicijevega karbida - 2.del: XRD metodeAnalyse chimique des produits réfractaires contenant du carbure de silicium a liaison nitrure
- Partie 2 : Méthodes de DRXChemische Analyse von feuerfesten Erzeugnissen aus nitridgebundenem Silicumcarbid
- Teil 2: XRD-VerfahrenTa slovenski standard je istoveten z:EN 12698-2:2007SIST EN 12698-2:2007en;de71.040.40Kemijska analizaChemical analysisICS:SLOVENSKI
STANDARDSIST EN 12698-2:200701-julij-2007
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 12698-2March 2007ICS 71.040.40 English VersionChemical analysis of nitride bonded silicon carbide refractories -Part 2: XRD methodsAnalyse chimique des produits réfractaires contenant ducarbure de silicium à liaison nitrure
- Partie 2 : Méthodesde DRXChemische Analyse von feuerfesten Erzeugnissen ausnitridgebundenem Silicumcarbid
- Teil 2: XRD-VerfahrenThis European Standard was approved by CEN on 15 February 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, 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 STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2007 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 12698-2:2007: E
EN 12698-2:2007 (E) 2 Contents Page Foreword.3 1 Scope.4 2 Normative references.4 3 Definitions.4 4 Apparatus.4 5 Sampling.5 6 Procedure.5 6.1 Sample preparation.5 6.2 Measuring parameters.5 6.3 Qualitative analysis.5 6.4 Quantitative analysis.6 7 Precision.10 7.1 Repeatability.10 7.2 Reproducibility.10 8 Test report.10 Annex A (normative)
X-ray diffraction data for the determination of ’-SiAlON content.11 A.1 General.11 A.2 Example of calculation of z-value for ’-SiAlON.12 Bibliography.13
EN 12698-2:2007 (E) 3 Foreword This document (EN 12698-2:2007) 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 September 2007, and conflicting national standards shall be withdrawn at the latest by September 2007. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, 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.
EN 12698-2:2007 (E) 4 1 Scope This standard describes methods for the determination of mineralogical phases typically apparent in nitride and oxy-nitride bonded silicon carbide refractory products using a Bragg-Brentano diffractometer.
It includes details of sample preparation and general principles for qualitative and quantitative analysis of mineralogical phase composition. Quantitative determination of α-Si3N4, β-Si3N4, Si2ON2, AlN, and SiAlON are described. NOTE For the refinement procedures the total nitrogen content, analysed in accordance with EN 12698-1 is needed. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 12475-4:1998, Classification of dense shaped refractory products — Part 4: Special products EN 12698-1, Chemical analysis of nitride bonded silicon carbide refractories — Part 1: Chemical methods ISO 836:2001, Terminology for refractories ISO 5022, Shaped refractory products — Sampling and acceptance testing ISO 8656-1, Refractory products — Sampling of raw materials and unshaped products — Part 1: Sampling scheme 3 Definitions For the purposes of this document the terms and definitions given in ISO 836:2001, EN 12475-4:1998 and the following apply.
3.1 nitride and oxynitride bonded silicon carbide refractories
refractory products predominantly consisting of silicon carbide with minor amounts of nitride phases as a matrix component NOTE
In general, metallic silicon is used as a precursor material, which undergoes a phase transformation in
an oxygen-free nitrogen atmosphere. 4 Apparatus
Bragg-Brentano diffractometers with a copper X-ray tube, graphite monochromator and scintillation counter and the following experimental setting for data collection are used: goniometer with a measurement uncertainty of ≤ 0,5 ° at a confidence level of 95 %; primary soller slit with a divergence
≤ 2,5 °; divergence slit 1 °; receiving slit ≤ 0,2
mm;
EN 12698-2:2007 (E) 5 scatter slit ≤ 1 °; narrow line focus; tube settings 40 kV and 20 mA to 45 mA. 5 Sampling Sample shaped and unshaped products using the procedures given in ISO 5022 and ISO 8656-1. When sampling large fragments, take care to collect samples from different points of individual pieces. Homogenize the sample by reducing the maximum particle size to 150 µm and take the test sample from this material. 6 Procedure 6.1 Sample preparation Grind the sample using a mill so that the resultant powder can pass through a 100 mesh sieve. NOTE Care should be taken not to grind the sample excessively as this has been found to cause the silicon nitride, and silicon phases in particular, to reduce in intensity. This is believed to be due to a build up of an amorphous layer on their particles due to damage induced by the silicon carbide. Press the powder into the cavity holder from the reverse side of the cavity to that which is to be presented to the x-ray beam (to reduce preferred orientation). The depth of the cavity shall be sufficient to exceed the critical depth of CuK. radiation for the sample analysed. 6.2 Measuring parameters Scan the sample on the instrument using the following parameters: start angle, 2 10 °; end angle, 2 70 °, 130 ° if β-SiAlON determination is required; step-spec, 2
0,02 ° or continuous; integration time 4 s. An additional scan using the same conditions as above between 60 ° and 70 ° 2 may be required if aluminium and/or iron is thought to be present. NOTE Parameters for tube settings should be: voltage 40 kV, excitation current 20 mA to 45 mA. 6.3 Qualitative analysis Use an automatic or manual search to identify different phases in accordance with the ICDD, JCPDS and ASTM databases. NOTE 1 A deconvolution program should be used for overlapping peaks.
EN 12698-2:2007 (E) 6 NOTE 2 The following phases are commonly found in nitride bonded silicon carbide: α-SiC, β-SiC, α-Si3N4, β-Si3N4, Si (free), Si2ON2, SiO2 (cristobalite), FeSi2 and WC (from grinding). Less common phases include: FeSi, Fe, Al, AlN, C (graphite), SiO2 (quartz), SiAlON. Some potential line overlaps to be aware of include the (111) cristobalite at 28,4 ° with the (111) silicon and the (110) iron at 44,7 ° with the (200) aluminium, there is also an interference of monoclinic zirconia on silicon. 6.4 Quantitative analysis 6.4.1 General For quantitative analysis the net peak intensities of the test sample are compared to a sample of known concentration. The intensities shall be evaluated by measuring the peak height or preferably the peak area. For the determin
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