DIN EN ISO 21068-3-2008 Chemical analysis of silicon-carbide-containing raw materials and refractory products - Part 3 Determination of nitrogen oxygen and metallic and oxidic cons.pdf

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1、December 2008DEUTSCHE NORM English price group 18No part of this standard 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 81.080!$Ty8“1498621ww

2、w.din.deDDIN EN ISO 21068-3Chemical analysis of silicon-carbide-containing raw materials andrefractory products Part 3: Determination of nitrogen, oxygen and metallic and oxidicconstituents (ISO 21068-3:2008)English version of DIN EN ISO 21068-3:2008-12Chemische Analyse von Siliciumcarbid enthaltend

3、en Rohstoffen und feuerfestenErzeugnissen Teil 3: Bestimmung des Gehaltes an Stickstoff, Sauerstoff sowie metallischen undoxidischen Bestandteilen (ISO 21068-3:2008)Englische Fassung DIN EN ISO 21068-3:2008-1221068-1:2008-12,supersedesDIN 51079-1:2004-08 andDIN 51079-2:2004-08www.beuth.deDocument co

4、mprises 45 pagesTogether with DIN EN ISODIN EN ISO 21068-3:2008-12 2 National foreword This standard has been published in accordance with a decision taken by Technical Committee CEN/TC 187 “Refractory products and materials” (Secretariat: BSI, United Kingdom) to adopt, without alteration, Internati

5、onal Standard ISO 21068-3:2008 as a European Standard. ISO 21068-3 was prepared by Technical Committee ISO/TC 33 “Refractories”. The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Technical Committee NA 062-02-64 AA

6、 Chemische Analyse von nichtoxidischen keramischen Roh- und Werkstoffen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 10058-1 DIN EN ISO 10058-1 ISO 10058-2 DIN EN ISO 10058-2 ISO 10058-3 DIN EN ISO 10058-3 ISO 10081-1 DIN EN ISO 100

7、81-1 ISO 10081-2 DIN EN ISO 10081-2 ISO 10081-3 DIN EN ISO 10081-3 ISO 12677 DIN EN ISO 12677 ISO 20565-1 DIN 51074-1, DIN 51074-2, DIN 51074-3, DIN 51074-4 and E DIN EN ISO 20565-1 ISO 20565-2 DIN 51074-1, DIN 51074-2, DIN 51074-3, DIN 51074-4 and E DIN EN ISO 20565-2 ISO 20565-3 DIN 51074-1, DIN 5

8、1074-2, DIN 51074-3, DIN 51074-4 and E DIN EN ISO 20565-3 ISO 21068-1 DIN EN ISO 21068-1 ISO 21068-2 DIN EN ISO 21068-2 ISO 21079-1 DIN EN ISO 21079-1 ISO 21079-2 DIN EN ISO 21079-2 ISO 21079-3 DIN EN ISO 21079-3 ISO 21587-1 DIN EN ISO 21587-1 ISO 21587-2 DIN EN ISO 21587-2 ISO 21587-3 DIN EN ISO 21

9、587-3 ISO 26845 DIN EN ISO 26845 In the German version only, the following corrections have been made as compared to the English reference version: a) In the heading of subclause 4.2, “CR” has been corrected to read “TC”. b) In subclause 5.4.3.2.3, the German translation of “ with electric furnace,

10、copper (II) oxide” has been corrected. Amendments This standard differs from DIN 51079-1:2004-08 and DIN 51079-2:2004-08 as follows: a) Specifications relating to sampling and preparation of the test sample have been deleted, as these are now included in DIN EN ISO 21068-1. b) The scope has been ext

11、ended to include the determination of nitrogen and oxygen. c) Acid pressure decomposition has been deleted. DIN EN ISO 21068-3:2008-12 3 d) Specifications relating to sodium carbonate boric acid fusion method have been modified and further fusion methods have been added. e) Methods for the determina

12、tion of nitrogen and oxygen, of free iron, free aluminium, free magnesium and some other oxides have been included. f) Statistical results have been included in an informative Annex A. g) The standard has been editorially revised. Previous editions DIN 51079-1: 1991-04, 2004-08 DIN 51079-2: 1998-03,

13、 2004-08 National Annex NA (informative) Bibliography DIN 51074-1, Testing of ceramic materials Chemical analysis of ceramic materials containing chromium oxide General instructions and test report DIN 51074-2, Testing of ceramic material Chemical analysis of ceramic materials containing chromium ox

14、ide Methods of dissolution DIN 51074-3, Testing of ceramic materials Chemical analysis of ceramic materials containing chromium oxide Determination of chromic oxide DIN 51074-4, Testing of ceramic materials Chemical analysis of ceramic materials containing chromium oxide Determination of calcium oxi

15、de DIN EN ISO 10058-1, Chemical analysis of magnesites and dolomites (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and gravimetric silica DIN EN ISO 10058-2, Chemical analysis of magnesites and dolomites (alternative to the X-ray fluorescence method) Part 2:

16、 Wet chemical analysis DIN EN ISO 10058-3, Chemical analysis of magnesites and dolomites (alternative to the X-ray fluorescence method) Part 3: Flame Atomic Absorption Spectrophotometry (FAAS) and Inductively Coupled Plasma Emission Spectrometry (ICP-AES) DIN EN ISO 10081-1, Classification of dense

17、shaped refractory products Part 1: Alumina-silica DIN EN ISO 10081-2, Classification of dense shaped refractory products Part 2: Basic products containing less than 7 % residual carbon DIN EN ISO 10081-3, Classification of dense shaped refractory products Part 3: Basic products containing from 7 % t

18、o 50 % residual carbon DIN EN ISO 12677, Chemical analysis of refractory products by XRF Fused cast bead method DIN EN ISO 21068-3:2008-12 4 E DIN EN ISO 20565-1, Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) P

19、art 1: Apparatus, reagents, dissolution and gravimetric silica E DIN EN ISO 20565-2, Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis E DIN EN ISO 20565-3, Chemical analysis of chrome

20、-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 3: Flame Atomic Absorption Spectrophotometry (FAAS) and Inductively Coupled Plasma Emission Spectrometry (ICP-AES) DIN EN ISO 21068-1, Chemical analysis of silicon-carbide-containing raw

21、 materials and refractory products Part 1: General information and sample preparation DIN EN ISO 21068-2, Chemical analysis of silicon-carbide-containing raw materials and refractory products Part 2: Determination of loss on ignition, total carbon, free carbon and silicon carbide, total and free sil

22、ica and total and free silicon DIN EN ISO 21079-1, Chemical analysis of refractories containing alumina, zirconia and silica Refractories containing 5 % to 45 % of ZrO2(alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents and dissolution DIN EN ISO 21079-2, Chemical analysis of

23、refractories containing alumina, zirconia and silica Refractories containing 5 % to 45 % of ZrO2(alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis DIN EN ISO 21079-3, Chemical analysis of refractories containing alumina, zirconia and silica Refractories containing 5 % to 45

24、 % of ZrO2(alternative to the X-ray fluorescence method) Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) DIN EN ISO 21587-1, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method)

25、 Part 1: Apparatus, reagents, dissolution and gravimetric silica DIN EN ISO 21587-2, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis DIN EN ISO 21587-3, Chemical analysis of aluminosilicate refractory products (alt

26、ernative to the X-ray fluorescence method) Part 3: Inductively coupled plasma and atomic absorption spectrometry methods DIN EN ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emis

27、sion spectrometry (ICP-AES) methods EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21068-3 August 2008 ICS 81.080 English Version Chemical analysis of silicon-carbide-containing raw materials and refractory products - Part 3: Determination of nitrogen, oxygen and metallic and oxidic consti

28、tuents (ISO 21068-3:2008)Analyse chimique des matires premires et des produits rfractaires contenant du carbure de silicium - Partie 3: Dosage de lazote, de loxygne et des constituants mtalliques et oxyds (ISO 21068-3:2008) Chemische Analyse von Siliciumcarbid enthaltenden Rohstoffen und feuerfesten

29、 Erzeugnissen - Teil 3: Bestimmung des Gehaltes an Stickstoff, Sauerstoff sowie metallischen und oxidischen Bestandteilen (ISO 21068-3:2008) This European Standard was approved by CEN on 11 July 2008. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the condi

30、tions 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 Management Centre or to any CEN member. This European Standard exists in thre

31、e 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 Management Centre has the same status as the official versions. CEN members are the national standards bodies of A

32、ustria, 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 C

33、OMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 21068-3:2008: E2 DIN EN ISO

34、21068-3:2008-12EN ISO 21068-3:2008 (E)Contents Page Foreword .3 Introduction.4 1 Scope5 2 Normative references5 3 Terms and definitions .6 4 Determination of nitrogen and oxygen .6 4.1 General .6 4.2 Combined determination of nitrogen and oxygen by an analyser with thermal conductivity (CR) and infr

35、ared absorption (IR) detection.6 5 Determination of nitrogen calculated as Si3N48 5.1 General .8 5.2 Acid decomposition Titration method9 5.3 Acid decomposition Photometry method 13 5.4 Inert-gas fusion Thermal conductivity method .16 5.5 Determination of total nitrogen21 6 Determination of free Iro

36、n by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)21 6.1 General .21 6.2 Copper sulfate method .22 6.3 Bromine/methanol method.23 7 Determination of free aluminium and free magnesium.26 7.1 General .26 7.2 Acid decomposition Inductively coupled plasma atomic emission spectroscopy

37、 (ICP-AES)26 7.3 Acid decomposition Flame Atomic Absorption Spectrometry (FAAS).28 7.4 Hydrogen generating method 29 8 Analysis of oxides.30 8.1 General .30 8.2 Wet methods 30 8.3 Flame atomic absorption and/or inductively coupled plasma atomic emission spectrometer30 8.4 XRF fusion method after ign

38、ition of the sample 31 8.5 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, calcium oxide, magnesium oxide, sodium oxide, potassium oxide, chromium(III) oxide, zirconium oxide, and boron oxide.33 9 Expression of results35 10 Test report35 Annex A (informative

39、) Statistical results obtained with analysis of refractories containing carbon and/or silicon carbide .36 Bibliography41 3 EN ISO 21068-3:2008 (E)DIN EN ISO 21068-3:2008-12Foreword This document (EN ISO 21068-3:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration

40、with 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 February 2009, and conflicting nati

41、onal standards shall be withdrawn at the latest by February 2009. Attention is drawn to the possibility that 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. According to the CEN

42、/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, L

43、uxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 21068-3:2008 has been approved by CEN as a EN ISO 21068-3:2008 without any modification. Introduction ISO 21068, Parts 1 to 3, h

44、ave been developed from the combination of a Japanese standard JIS 20118and work items originally developed within CEN. Because there is a wide variety of laboratory equipment in use, the most commonly used methods are described. This part of ISO 21068 is applicable to the analysis of all refractory

45、 products as classified in ISO 10081 (all parts) 3, 4, 5, 6(shaped) and ISO 1927 1(unshaped) and raw materials containing carbon and/or silicon carbide. Therefore, this part of ISO 21068 covers the full range of analysis from pure silicon carbide to oxidic refractory composition with a low content o

46、f silicon carbide and/or nitrides. Primarily, this part of ISO 21068 provides methods to distinguish between different carbon bound types like total carbon (Ctotal) and free carbon (Cfree) and derives from these two the silicon carbide content. If free carbon is present, this part of ISO 21068 inclu

47、des different types of temperature treatment in order to determine the mass changes gravimetrically. Frequently, the resulting residue is used for other determinations. The determination of other groups of analytes described in this part of ISO 21068 are free metals, free silicon (Sifree), free alum

48、inum (Alfree), free magnesium (Mgfree), free iron (Fefree) and the group of oxides from main to trace components. This part of ISO 21068 also describes the chemical analysis of SiO2, total Si, oxygen and nitrogen and other oxidic bound metals which typically occur in the materials. This part of ISO

49、21068 represents a listing of analytical methods which is approximately structured according to material composition. However, it is still the user who should prove the applicability of the method depending on the material and analytical requirements. 4 DIN EN ISO 21068-3:2008-12EN ISO 21068-3:2008 (E)1 Scope This part of ISO 21068 specifies methods for the determination of total nitrogen and nitrogen calculated as silicon nitride, total oxygen, and free metallic and oxidic components in