DIN EN ISO 21068-2-2008 Chemical analysis of silicon-carbide-containing raw materials and refractory products - Part 2 Determination of loss on ignition total carbon free carbon an.pdf

1、December 2008DEUTSCHE NORM English price group 21No 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!$Ty7“1498620ww

2、w.din.deDDIN EN ISO 21068-2Chemical analysis of silicon-carbide-containing raw materials andrefractory products Part 2: Determination of loss on ignition, total carbon, free carbon andsilicon carbide, total and free silica and total and free silicon(ISO 21068-2:2008)English version of DIN EN ISO 210

3、68-2:2008-12Chemische Analyse von Siliciumcarbid enthaltenden Rohstoffen und feuerfestenErzeugnissen Teil 2: Bestimmung des Glhverlustes und Gehaltes an Gesamtkohlenstoff, freiemKohlenstoff und Siliciumcarbid, des Gehaltes an gesamtem und freiem Silicium(IV)-oxidsowie an gesamtem und freiem Silicium

4、 (ISO 21068-2:2008)Englische Fassung DIN EN ISO 21068-2:2008-12Together with DIN EN ISO 21068-1:2008-12, 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 51076-1:1991-04Supersedes: see belowwww.beuth.deDocument comprises 57 pag

5、esDIN EN ISO 21068-2:2008-12 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, International Standard ISO 21068-2:2008 as a Eu

6、ropean Standard. ISO 21068-2 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 Chemische Analyse von nichtoxidischen

7、 keramischen Roh- und Werkstoffen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5725-2 DIN ISO 5725-2 ISO 9286 DIN ISO 9286 ISO 10081-1 DIN EN ISO 10081-1 ISO 10081-2 DIN EN ISO 10081-2 ISO 10081-3 DIN EN ISO 10081-3 ISO 21068-1 DIN

8、EN ISO 21068-1 In the German version only, the following corrections have been made as compared to the English reference version: a) In subclause 5.2.2.5, the formula for lead borate has been corrected to read 2 PbO B2O3; and in subclause 5.3.1, the formula for barium perchlorate solution has been c

9、orrected to read Ba(CIO4)2. b) In subclause 5.3.2, Figure 3, items 8, 9, 10 and 11 of the key have been corrected. c) Symbol “w” for mass fraction has been added in subclause 6.4.1, NOTE; in subclause 6.4.4.5, first sentence; in subclause 6.5.1, fifth paragraph and in c), fifth line; in subclause 6.

10、5.4, equations (21), (22) and in the penultimate line as well as in subclause 10.2, equation (32). d) In subclause 6.5.1 a), third item, symbol “w” for mass fraction before Ctotalhas been deleted. e) In subclause 6.5.2.4, first equation of the NOTE, the fraction line has been added. f) The explanati

11、ons to equations (22) and (32) have been corrected (e.g. “w” and “mass fraction expressed as a percentage” have been added). g) In subclause 9.3.3.6, in the heading, “Henpel” has been corrected to read “Hempel”. h) In subclause 9.4.3.3, the English version “250 mg 0,000 1 g” has been replaced by “(2

12、50 0,1) mg”. i) In subclause 10.4, in the heading, “SiO2” has been rendered more precise to read “SiO2surf”. 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 and DIN 51076-1:1991-04 as follows: a) Specificat

13、ions relating to sampling and preparation of the test sample have been deleted, as these are now included in DIN EN ISO 21068-1. b) In addition to the ignition under argon, the determination of change in mass has been supplemented by further methods. DIN EN ISO 21068-2:2008-12 3 c) The determination

14、 of free carbon by wet oxidation has been included upon the withdrawal of draft standard DIN 51079-3. d) The determination of the total carbon content and the free carbon content has been extended by detection techniques using infrared absorption and thermal conductivity. e) The determination of sil

15、icon carbide by chemical method has been added. f) The determination of total silicon content has been added. g) The determination of free silicon content by silver displacement has been added. h) The determination of silica content, SiO2, has been added. i) Annex A (informative) “Examples of CRMs f

16、or calibration of carbon analyser” has been added. j) The standard has been editorially revised. Previous editions DIN 51075-1: 1966-02, 1982-10 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

17、-04 National Annex NA (informative) Bibliography 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 containing less than 7 % residual carbon DIN EN ISO 10081-3, Cl

18、assification of dense shaped refractory products Part 3: Basic products containing from 7 % to 50 % residual carbon DIN EN ISO 21068-1, Chemical analysis of silicon-carbide-containing raw materials and refractory products Part 1: General information and sample preparation DIN ISO 5725-2, Accuracy (t

19、rueness 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 9286, Abrasive grains and crude Chemical analysis of silicon carbide DIN EN ISO 21068-2:2008-12 4 This page is intentiona

20、lly blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21068-2 August 2008 ICS 81.080 English Version 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 an

21、d free silica and total and free silicon (ISO 21068-2:2008) Analyse chimique des matires premires et des produits rfractaires contenant du carbure de silicium - Partie 2: Dtermination de la perte au feu, du carbone total, du carbone libre et du carbure de silicium, de la silice totale et libre, et d

22、u silicium total et libre (ISO 21068-2:2008) Chemische Analyse von Siliciumcarbid enthaltenden Rohstoffen und feuerfesten Erzeugnissen - Teil 2: Bestimmung des Glhverlustes und Gehaltes an Gesamtkohlenstoff, freiem Kohlenstoff und Siliciumcarbid, des Gehaltes an gesamtem und freiem Silicium(IV)-oxid

23、 sowie an gesamtem und freiem Silicium (ISO 21068-2:2008) 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 conditions for giving this European Standard the status of a national standard without a

24、ny 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 three official versions (English, French, German). A version in any other language made

25、 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 Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, Franc

26、e, 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 STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR

27、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 21068-2:2008: E2 DIN EN ISO 21068-2:2008-12 EN ISO 21068-2:2008 (E)Contents Page Foreword4 Introduction .5 1 Sc

28、ope 6 2 Normative references 6 3 Terms and definitions .6 4 Determination of change in mass 7 4.1 General7 4.2 Determination of the loss on drying at 250 C (LOD250) gravimetric method .7 4.3 Determination of the loss on calcination in argon (LOIAr) 8 4.4 Determination of the change in mass by heat p

29、retreatment in air 10 4.5 Determination of the change in mass at 750 C (LOI750) 10 4.6 Determination of loss on ignition at 850 C (LOI850). 11 4.7 Determination of loss on ignition at 1 050 C (LOI1 050) . 12 5 Determination of the total carbon content .13 5.1 General. 13 5.2 Combustion techniques. 1

30、3 5.3 Detection techniques . 17 5.4 Detection methods 21 6 Determination of free carbon content 29 6.1 General. 29 6.2 Sample decomposition by combustion 29 6.3 Detection techniques . 29 6.4 Direct detection methods. 29 6.5 Indirect detection methods 33 6.6 Direct determination of free carbon by wet

31、 oxidation 38 7 Determination of silicon carbide content, SiC. 38 7.1 General. 38 7.2 Determination of silicon carbide, SiC, by indirect quantitative method . 38 7.3 Determination of silicon carbide, SiC, by direct quantitative method 39 7.4 Determination of silicon carbide SiC by ignition method at

32、 750 C 40 7.5 Determination of silicon carbide, SiC, by chemical method 41 8 Determination of total silicon content via silica 43 8.1 Principle. 43 8.2 Reagents 43 8.3 Apparatus 43 8.4 Procedure 43 8.5 Blank test. 44 8.6 Calculation. 44 9 Determination of free silicon content . 45 9.1 Principle. 45

33、9.2 Pretreatment with hydrochloric acid 45 9.3 Silicon determination by hydrogen evolution . 45 9.4 Silicon determination by silver displacement . 48 10 Determination of silica content, SiO2. 50 10.1 General. 50 10.2 Determination of free and/or combined silica content, SiO2. 50 3 EN ISO 21068-2:200

34、8 (E)DIN EN ISO 21068-2:2008-12 10.3 Determination of free silica, SiO250 10.4 Determination of surface silicon dioxide, SiO251 11 Expression of results51 12 Test report51 Annex A (informative) Examples of CRMs for calibration of carbon analyser.52 Bibliography53 4 DIN EN ISO 21068-2:2008-12 EN ISO

35、21068-2:2008 (E)Foreword This document (EN ISO 21068-2:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration 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 s

36、tatus 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. Attention is drawn to the possibility that some of the elements of this document may be th

37、e 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 organizations of the following countries are bound to implement this European Standard: Austria, Belgi

38、um, 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 the United Kingdom. Endorsement notice

39、The text of ISO 21068-2:2008 has been approved by CEN as a EN ISO 21068-2:2008 without any modification. Introduction ISO 21068, Parts 1 to 3, have been developed from the combination of a Japanese standard JIS 20116and work items originally developed within CEN. Because there is a wide variety of l

40、aboratory equipment in use, the most commonly used methods are described. This part of ISO 21068 is applicable to the analysis of all refractory products classified in ISO 100812 to 5(shaped) and ISO 19271(unshaped) and raw materials containing carbon and/or silicon carbide. Therefore, this part of

41、ISO 21068 covers the full range of analysis from pure silicon carbide to oxidic refractory composition with a low content of 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 car

42、bon (Cfree) and derives from these two the silicon carbide content. If free carbon is present, this part of ISO 21068 includes different types of temperature treatment, in order to determine the mass changes gravimetrically. Frequently, the resulting residue is used for other determinations. The det

43、ermination of other groups of analytes described in this part of ISO 21068 are free metals, free silicon (Sifree), free aluminum (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

44、 SiO2, total Si, oxygen and nitrogen and other oxidic-bound metals which typically occur in the materials. This part of ISO 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 applica

45、bility of the method, depending on the material and analytical requirements. 5 EN ISO 21068-2:2008 (E)DIN EN ISO 21068-2:2008-12 1 Scope This part of ISO 21068 specifies analytical techniques for the determination of change in mass by thermal treatment at specified temperatures, and methods for the

46、determination of the total carbon content, free carbon, silicon carbide, silicon, total silica and free silica content of silicon-carbide-containing raw materials and refractory products. 2 Normative references The following referenced documents are indispensable for the application of this document

47、. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatabili

48、ty and reproducibility of a standard measurement method ISO 9286:1997, Abrasive grains and crude Chemical analysis of silicon carbide ISO 10060, Dense, shaped refractory products Test methods for products containing carbon ISO 21068-1:2008, Chemical analysis of silicon-carbide-containing raw materia

49、ls and refractory products Part 1: General information and sample preparation EN 12698-1:2007, Chemical analysis of nitride bonded silicon carbide refractories Part 1: Chemical methods 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 21068-1 apply. 6 DIN EN ISO 21068-2:2008-12 EN ISO 21068-2:2008 (E)4 Determination of change in mass 4.1 General The determination of change in mass is defined as a loss or increase in mass caused by heat treatment. Several methods are disting