BS EN ISO 21079-3-2008 Chemical analysis of nrefractories containing nalumina zirconia and nsilica — Refractories ncontaining 5 percent nto 45 percent of ZrO2 n(alternative to the .pdf

1、BS EN ISO21079-3:2008ICS 81.080NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDChemical analysis ofrefractories containingalumina, zirconia, andsilica Refractoriescontaining 5 percentto 45 percent of ZrO2(alternative to theX-ray fluorescencemethod)Part 3: Flame

2、atomic absorptionspectrophotometry (FAAS) andinductively coupled plasma emissionspectrometry (ICP -AES) (ISO21079-3:2008)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/08/2009 02:44, Uncontrolled Copy, (c) BSIThis British Standardwas published under theauthority of the StandardsPolicy and

3、 StrategyCommittee on 30 April2009 BSI 2009ISBN 978 0 580 58572 2Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 21079-3:2008National forewordThis British Standard is the UK implementation of EN ISO21079-3:2008.The UK participation in its preparation was entrusted to TechnicalCo

4、mmittee RPI/1, Refractory products and materials.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with

5、a British Standard cannot confer immunityfrom legal obligations.Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/08/2009 02:44, Uncontrolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 21079-3April 2008ICS 81.080; 71.040.40English VersionChemical analysis of refractor

6、ies containing alumina, zirconia,and silica - Refractories containing 5 percent to 45 percent ofZrO2 (alternative to the X-ray fluorescence method) - Part 3:Flame atomic absorption spectrophotometry (FAAS) andinductively coupled plasma emission spectrometry (ICP -AES)(ISO 21079-3:2008)Analyse chimiq

7、ue des matriaux rfractaires contenant delalumine, de la zircone et de la silice - Matriauxrfractaires contenant de 5 % 45 % de ZrO2 (mthodealternative la mthode par fluorescence de rayons X) -Partie 3: Mthodes par spectromtrie dabsorptionatomique dans la flamme (FAAS) et spectromtriedmission atomiqu

8、e avec plasma induit par hautefrquence (ICP-AES) (ISO 21079-3:2008)Chemische Analyse von aluminiumoxid-, zirkomiumoxid-und silicium(IV)-oxidhaltigen feuerfesten Erzeugnissen -Feuerfeste Erzeugnisse mit einem Massenanteil an ZrO2von 5 % bis 45 % (Alternative zumRntgenfluoreszenzverfahren) - Teil 3:Fl

9、ammenatomabsorptionsspektrophotometrie (FAAS) undAtomemissionsspektrometrie mit induktiv gekoppeltemPlasma (ICP-AES) (ISO 21079-3:2008)This European Standard was approved by CEN on 12 April 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions

10、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 officia

11、l 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, Belg

12、ium, 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 ST

13、ANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 21079-3:2008: ELicensed Copy: Wang Bin, ISO/EXCH

14、ANGE CHINA STANDARDS, 10/08/2009 02:44, Uncontrolled Copy, (c) BSIBS EN ISO 21079-3:2008EN ISO 21079-3:2008 (E) 3 Foreword This document (EN ISO 21079-3:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration with Technical Committee CEN/TC 187 “Refractory products a

15、nd 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 October 2008, and conflicting national standards shall be withdrawn at the latest by October

16、2008. 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 organi

17、zations 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, Rom

18、ania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 21079-3:2008 has been approved by CEN as a EN ISO 21079-3:2008 without any modification. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/08/2009 02:44, Uncontrolled Copy, (c) BSI

19、BS EN ISO 21079-3:2008ISO 21079-3:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Instrumental methods using ICP-AES 1 3.1 Determination of residual silica in solution by ICP-AES 1 3.2 Determination of silicon(IV) oxide, aluminium oxide, iro

20、n(III) oxide, titanium(IV) oxide, calcium oxide, magnesium oxide, chromium(III) oxide and hafnium oxide using stock solutions (S1), (S1) or (S1) by ICP-AES. 3 3.3 Determination of calcium oxide, magnesium oxide, sodium oxide and potassium oxide using stock solutions (S4) by ICP-AES 7 4 Instrumental

21、methods using Flame Atomic Absorption Spectrometry (FAAS). 8 4.1 Determination of calcium oxide, magnesium oxide, sodium oxide and potassium oxide using stock solutions (S3) by FAAS . 8 4.2 Determination of chromium(III) oxide by FAAS spectrometry. 10 5 Calculation and expression of test results 12

22、6 Test report . 12 Bibliography . 13 Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/08/2009 02:44, Uncontrolled Copy, (c) BSIBS EN ISO 21079-3:2008ISO 21079-3:2008(E) iv ISO 2008 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation

23、 of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee.

24、International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance wit

25、h the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approv

26、al by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 21079-3 was prepared by Technical Commit

27、tee ISO/TC 33, Refractories. ISO 21079 consists of the following parts, under the general title 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 dissol

28、ution Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/08/2009 02:44, Uncontrolled Copy, (c) BSIBS EN ISO 21079-3:2008INTERNATIONAL STANDARD

29、ISO 21079-3:2008(E) ISO 2008 All rights reserved 1Chemical analysis of refractories containing alumina, zirconia, and silica Refractories containing 5 % to 45 % of ZrO2(alternative to the X-ray fluorescence method) Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plas

30、ma emission spectrometry (ICP-AES) 1 Scope This part of ISO 21079 specifies flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) methods for the analysis of AZS (alumina, zirconia, and silica) refractory products (containing 5 % to 45 % of Z

31、rO2) and raw materials. This part of ISO 21079 is not applicable to MgO-based refractories. This part of ISO 21079 gives alternatives to the X-ray fluorescence (XRF) method given in ISO 12677. 2 Normative references The following referenced documents are indispensable for the application of this doc

32、ument. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 21079-1:2008, Chemical analysis of refractories containing alumina, zirconia and silica Refractories containing 5 % to 45 % of Zr

33、O2(alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents and dissolution ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma (ICP) methods 3 Instrumental methods using ICP

34、-AES 3.1 Determination of residual silica in solution by ICP-AES 3.1.1 Principle The residual silica remaining in solution in solutions (S1) or (S1) is determined using ICP-AES. 3.1.2 Reagents 3.1.2.1 General Prepare the reagents given in 3.1.2.2 to 3.1.2.4. and those specified in ISO 26845, as nece

35、ssary. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/08/2009 02:44, Uncontrolled Copy, (c) BSIBS EN ISO 21079-3:2008ISO 21079-3:2008(E) 2 ISO 2008 All rights reserved3.1.2.2 Diluted silicon(IV) oxide standard solution, SiO20,08 mg/ml. Transfer 20 ml of the silicon(IV) oxide standard solu

36、tion (SiO21 mg/ml) into a 250 ml volumetric flask, and dilute to the mark with water. 3.1.2.3 Matrix solution 1 or 1. Carry out the procedure given in 9.2.2.3 or 9.2.3.3 of ISO 21079-1:2008 without the sample, but omit heating the fusion mixture or anhydrous sodium carbonate. Designate the solution

37、equivalent to stock solution (S1) or (S1) as matrix solution 1 or 1 as applicable. 3.1.2.4 Series 2 solution for calibration. Transfer appropriate aliquot portions of diluted silicon(IV) oxide standard solution (0,08 mg/ml) precisely into several 100 ml volumetric flasks, in accordance with the comp

38、osition of the samples. Add 10 ml each of matrix solution 1 or 1 and dilute to the mark with water. Table 1 shows a typical example of the preparation of solutions. An appropriate series of solutions for calibration should be prepared, depending on the compositions of the samples and the types and c

39、apabilities of instrument used. Table 1 Example of series 2 solution for calibration Matrix solution 1 or 1 Diluted silicon(IV) oxide standard solution Concentration of solution Solution No. ml ml SiO2mg/100 ml 1 10 0 0 2 10 5 0,4 3 10 10 0,8 4 10 15 1,2 5 10 20 1,6 6 10 25 2,0 3.1.3 Procedure Deter

40、mine the silicon(IV) oxide remaining in solution (S1) or (S1) (see Annex A of ISO 21079-1:2008) as follows. Transfer 10 ml of stock solution (S1) or (S1) to a 100 ml volumetric flask, and dilute to the mark with water. Designate this solution for the determination of dissolved silicon(IV) oxide as d

41、iluted stock solution (S1d) or (S1d). Spray a portion of diluted stock solution (S1d or S1d) into the argon plasma flame of the inductively coupled plasma atomic emission (ICP-AE) spectrometer, and measure the emission intensity at an appropriate wavelength, for example, 251,611 nm. 3.1.4 Blank test

42、 Carry out the procedure in 3.1.3 with blank solution (B1) or (B1) (see Annex A of ISO 21079-1:2008). Designate the equivalent diluted blank solution to diluted stock solution (S1d) or (S1d) as diluted blank solution (B1d or B1d). Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/08/2009 02:

43、44, Uncontrolled Copy, (c) BSIBS EN ISO 21079-3:2008ISO 21079-3:2008(E) ISO 2008 All rights reserved 33.1.5 Plotting the calibration graph Using the series 2 solution for calibration, carry out the emission procedure described in 3.1.3. Plot the relation between the emission intensity and mass of ox

44、ide, prepare the calibration graph by adjusting the curve so that it passes through the point of origin. A new calibration should be carried out using the range of calibration and blank solutions for each set of determinations. 3.1.6 Calculation Calculate the mass fraction of silicon(IV) oxide, w(Si

45、O2), expressed as a percentage, using Equation (1) with the amount of silicon(IV) oxide derived from the values obtained from 3.1.3 and 3.1.4 and the calibration prepared as described in 3.1.5. ()()()12 sb250010SiO 100mm mmwm+= (1) where m is the mass of the test portion obtained in accordance with

46、9.2.2.2 or 9.2.3.2 of ISO 21079-1:2008, in grams; m1is the mass obtained in accordance with 9.2.2.3 or 9.2.3.3 of ISO 21079-1:2008, in grams; m2is the mass obtained in accordance with 9.2.2.4 or 9.2.3.4 of ISO 21079-1:2008, in grams; msis the mass of silicon(IV) oxide in diluted stock solution (S1d

47、or S1d) as described in 3.1.3, in grams; mbis the mass of silicon(IV) oxide in diluted blank solution (B1d or B1d) as described in 3.1.4, in grams. 3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, calcium oxide, magnesium oxide, chromium(III) oxide and ha

48、fnium oxide using stock solutions (S1), (S1) or (S1) by ICP-AES 3.2.1 Principle The emission intensity of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, calcium oxide, magnesium oxide, chromium(III) oxide and hafnium oxide are measured by the ICP-AE spectrometer for stock s

49、olutions (S1), (S1) or (S1). The ICP-AES method is applicable to the components in (S1), (S1) or (S1) as given in Table 2. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/08/2009 02:44, Uncontrolled Copy, (c) BSIBS EN ISO 21079-3:2008ISO 21079-3:2008(E) 4 ISO 2008 All rights reservedTable 2 Application range Range Component % by mass SiO20,1 to 10 Al2O31 to 10 Fe2O30,01 to 2 TiO20,01 to 5 CaO 0,01 to 2 MgO 0,01 to 2 Cr2O30,01 to 3 HfO20,01 to 2 NOTE 1 When solutions (S1) or (S