DIN EN ISO 21068-1-2008 Chemical analysis of silicon-carbide-containing raw materials and refractory products - Part 1 General information and sample preparation (ISO 21068-1 2008).pdf

1、December 2008DEUTSCHE NORM English price group 11No 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!$Ty5“1498618ww

2、w.din.deDDIN EN ISO 21068-1Chemical analysis of silicon-carbide-containing raw materials andrefractory products Part 1: General information and sample preparation (ISO 21068-1:2008)English version of DIN EN ISO 21068-1:2008-12Chemische Analyse von Siliciumcarbid enthaltenden Rohstoffen und feuerfest

3、enErzeugnissen Teil 1: Allgemeine Angaben und Probenvorbereitung (ISO 21068-1:2008)Englische Fassung DIN EN ISO 21068-1:2008-12Together with DIN EN ISO 21068-2:2008-12, supersedes DIN 51075-1:1982-10, DIN 51075-2:1984-03,DIN 51075-3:1982-10, DIN 51075-4:1982-10, DIN 51075-5:1982-10 and DIN 51076-1:1

4、991-04;together with DIN EN ISO 21068-3:2008-12, supersedes DIN 51079-1:2004-08 and DIN 51079-2:2004-08Supersedes: see belowwww.beuth.deDocument comprises 16 pagesDIN EN ISO 21068-1:2008-12 2 National foreword This standard has been published in accordance with a decision taken by Technical Committe

5、e CEN/TC 187 “Refractory products and materials” (Secretariat: BSI, United Kingdom) to adopt, without alteration, International Standard ISO 21068-1:2008 as a European Standard. ISO 21068-1 was prepared by Technical Committee ISO/TC 33 “Refractories”. The responsible German body involved in its prep

6、aration was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Technical 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 follo

7、ws: ISO 31-0 DIN 1313 and DIN 1338 ISO 5725-1 DIN ISO 5725-1 ISO 8656-1 DIN 51061-2 and DIN EN 1402-2 ISO 9286 DIN ISO 9286 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 10081-1 ISO 10081-2 DIN EN ISO 10081-2 ISO 10081-3 DIN EN IS

8、O 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 51074-2, DIN 51074-3, DIN 51074-4 and E DIN EN ISO 20565-3

9、 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 21587-3 ISO 26845 DIN EN ISO 26845 In the German version only, reference to ISO 21587-1 22

10、 has been corrected in the Introduction (last but two paragraph) to read “ISO 21587-2 23”. Amendments This standard differs from DIN 51075-1:1982-10, DIN 51075-2:1984-03, DIN 51075-3:1982-10, DIN 51075-4:1982-10, DIN 51075-5:1982-10, DIN 51076-1:1991-04, DIN 51079-1:2004-08 and DIN 51079-2:2004-08 a

11、s follows: a) Specifications relating to sampling and preparation of the test sample have been taken over and Clause 7 “Test report” has been brought in line with the modified scope. b) The standard has been editorially revised. DIN EN ISO 21068-1:2008-12 3 Previous editions DIN 51075-1: 1966-02, 19

12、82-10 DIN 51075-2: 1966-02, 1982-10, 1983-04, 1984-03 DIN 51075-3: 1966-02, 1982-10 DIN 51075-4: 1966-02, 1982-10 DIN 51075-5: 1982-10 DIN 51076-1: 1970-08, 1991-04 DIN 51079-1: 1991-04, 2004-08 DIN 51079-2: 1998-03, 2004-08 National Annex NA (informative) Bibliography DIN 1313, Quantities DIN 1338,

13、 Writing and typesetting of formulae DIN 51061-2, Testing of ceramic raw and finished materials Part 2: Sampling of ceramic raw materials DIN 51074-1, Testing of ceramic materials Chemical analysis of ceramic materials containing chromium oxide General instructions and test report DIN 51074-2, Testi

14、ng of ceramic material Chemical analysis of ceramic materials containing chromium oxide 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

15、analysis of ceramic materials containing chromium oxide Determination of calcium oxide DIN EN 1402-2, Unshaped refractory products Part 2: Sampling for testing DIN EN ISO 10058-1, Chemical analysis of magnesites and dolomites (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents

16、, dissolution and gravimetric silica DIN EN ISO 10058-2, Chemical analysis of magnesites and dolomites (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis DIN EN ISO 10058-3, Chemical analysis of magnesites and dolomites (alternative to the X-ray fluorescence method) Part 3:

17、 Flame Atomic Absorption Spectrophotometry (FAAS) and Inductively Coupled Plasma Emission Spectrometry (ICP-AES) DIN EN ISO 10081-1, Classification of dense shaped refractory products Part 1: Alumina-silica DIN EN ISO 10081-2, Classification of dense shaped refractory products Part 2: Basic products

18、 containing less than 7 % residual carbon DIN EN ISO 21068-1:2008-12 4 DIN EN ISO 10081-3, Classification of dense shaped refractory products Part 3: Basic products containing from 7 % to 50 % residual carbon DIN EN ISO 12677, Chemical analysis of refractory products by XRF Fused cast bead method E

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

20、d 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-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 3: Flame Atomic Absorption Sp

21、ectrophotometry (FAAS) and Inductively Coupled Plasma Emission Spectrometry (ICP-AES) 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 DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 9286, Abrasive grains and crude Chemical analysis of silicon carbide EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21

28、068-1 August 2008 ICS 81.080 English Version Chemical analysis of silicon-carbide-containing raw materials and refractory products - Part 1: General information and sample preparation (ISO 21068-1:2008) Analyse chimique des matires premires et des produits rfractaires contenant du carbure de siliciu

29、m - Partie 1: Informations gnrales et prparation des chantillons (ISO 21068-1:2008) Chemische Analyse von Siliciumcarbid enthaltenden Rohstoffen und feuerfesten Erzeugnissen - Teil 1: Allgemeine Angaben und Probenvorbereitung (ISO 21068-1:2008) This European Standard was approved by CEN on 11 July 2

30、008. 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

31、 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 translation under the responsibility of a CEN member into its own language and notified to the CEN Management

32、 Centre has the same status as the official 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,

33、Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE 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 an

34、d by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 21068-1:2008: EContents Page Foreword .3 Introduction.4 1 Scope5 2 Normative references7 3 Definitions 7 4 Sampling and preparation of the test sample 8 4.1 General .8 4.2 Sample pretreatment.8 5 Preliminary analyses.9 6 Exp

35、ression of results10 7 Test report10 Bibliography11 2 DIN EN ISO 21068-1:2008-12 EN ISO 21068-1:2008 (E) 3 Foreword This document (EN ISO 21068-1:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration with Technical Committee CEN/TC 187 “Refractory products and mate

36、rials” 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 national standards shall be withdrawn at the latest by February 2009.

37、 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/CENELEC Internal Regulations, the national standards organizatio

38、ns 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,

39、 Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 21068-1:2008 has been approved by CEN as a EN ISO 21068-1:2008 without any modification. DIN EN ISO 21068-1:2008-12 EN ISO 21068-1:2008 (E) Introduction ISO 21068, Parts 1 to 3, have been devel

40、oped from the combination of a Japanese standard JIS 2011 2and work items originally developed within CEN. As there is a wide variety of laboratory equipment in use, the most commonly used methods are described. ISO 21068, Parts 1 to 3, are applicable to the analysis of all refractory products as cl

41、assified in ISO 10081 10 to 13(shaped) and ISO 1927 3(unshaped) and raw materials containing carbon and/or silicon carbide. Therefore, ISO 21068, Parts 1 to 3, covers the full range of analysis from pure silicon carbide to oxidic refractory composition with low-content silicon carbide and/or nitride

42、s. Primarily, ISO 21068, Parts 1 to 3, 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, the standard includes different types of temperature treat

43、ment 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 ISO 21068, Parts 1 to 3, are free metals, free silicon (Sifree), free aluminum (Alfree), free magnesium (Mgfree)

44、, free iron (Fefree) and the group of oxides from main to trace components. ISO 21068, Parts 1 to 3, also describe the chemical analysis of silicon dioxide, total silicon, oxygen and nitrogen and other oxidic bound metals that typically occur in the materials. It represents a listing of analytical m

45、ethods 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. The most broadly used analytical techniques such as X-ray fluorescence spectroscopy (XRF)

46、and inductively coupled plasma-optical emission spectrometry (ICP-OES) suffer from the disadvantage that the analytical results are chemical bond independent. For carbon-containing ceramic raw materials and compositions ISO 21068, Parts 1 to 3, provide analytical methods for the determination of fre

47、e carbon, and SiC in the presence of oxidic compounds in particular SiO2. Because of the diversity of laboratory equipment, the three parts of ISO 21068 summarize broadly used analytical techniques which lead to equivalent results. In principle, the determination of carbon is based in all itemized m

48、ethods on the oxygen extraction method, where carbon is oxidized at elevated temperatures. Thereafter carbon is analysed as CO2. As well as carbon and carbidic compounds, metallic silicon, aluminium and magnesium are considered. While metallic silicon is in majority a precursor material which remain

49、s after the production process of SiC in the raw material, metallic aluminium is added as an antioxidant in carbon-containing refractory formulations. Mostly oxidic bound components, such as Al2O3, CaO, MgO, TiO2, Cr2O3, ZrO2and alkalines, can be determined by XRF as described in ISO 12677, ICP-AES or wet chemical methods (see ISO 26845 25, ISO 21587-1 22and ISO 21587-3 24). These results can be corrected by formulas provided by ISO 21068, Parts 1 to 3, in considera