DIN EN ISO 21587-3-2007 Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) - Part 3 Inductively coupled plasma and atomic absor.pdf

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1、December 2007DEUTSCHE NORM English price group 13No 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!$JB“1398831www

2、.din.deDDIN EN ISO 21587-3Chemical analysis of aluminosilicate refractory products(alternative to the X-ray fluorescence method) Part 3: Inductively coupled plasma and atomic absorption spectrometrymethods (ISO 21587-3:2007)English version of DIN EN ISO 21587-3:2007-12Chemische Analyse feuerfester E

3、rzeugnisse aus Alumosilicat(Alternative zum Rntgenfluoreszenzverfahren) Teil 3: Verfahren mit induktiv gekoppeltem Plasma und Atomabsorptionsspektrometrie(ISO 21587-3:2007)Englische Fassung DIN EN ISO 21587-3:2007-12supersedesDIN V ENV 955-4:1997-07www.beuth.deTogether with DIN EN ISO 21587-1:2007-1

4、2,Document comprises 26 pagesDIN EN ISO 21587-3:2007-12 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 Standa

5、rd ISO 21587-3:2007 as a European Standard. ISO 21587-3 was prepared by Technical Committee ISO/TC 33 “Refractories”. The responsible German body involved in its preparation was the Normenausschuss Materialprfung oxidischen Roh- und Werkstoffen. The DIN Standards corresponding to the International S

6、tandards referred to in clause 2 of the EN are as follows: ISO 21587-1 DIN EN ISO 21587-1 ISO 21587-2 DIN EN ISO 21587-2 ISO 26845 DIN EN ISO 26845 Amendments This standard differs from DIN V ENV 955-4:1997-07 as follows: a) The standard has been split into three parts. b) The standard has been comp

7、letely revised taking into account the current chemical analysis and environmental aspects. Previous editions DIN V ENV 955-4: 1997-07 National Annex NA (informative) Bibliography DIN EN ISO 21587-1, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence meth

8、od) 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 26845, Chemical analysis of refractories General requirements for w

9、et chemical analysis, AAS and ICP methods (Materials Testing Standards Committee), Technical Committee NA 062-02-61 AA Chemische Analyse von EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 21587-3September 2007ICS 81.080 Supersedes ENV 955-4:1997 English VersionChemical analysis of aluminosili

10、cate refractory products(alternative to the X-ray fluorescence method) - Part 3:Inductively coupled plasma and atomic absorption spectrometrymethods (ISO 21587-3:2007)Analyse chimique des produits rfractairesdaluminosilicates (mthode alternative la mthode parfluorescence de rayons X) - Partie 3: Mth

11、odes parspectromtrie dabsorption atomique (AAS) etspectromtrie dmission atomique avec plasma induit parhaute frquence (ICP-AES) (ISO 21587-3:2007)Chemische Analyse feuerfester Erzeugnisse ausAlumosilicat (Alternative zumRntgenfluoreszenzverfahren) - Teil 3: Verfahren mitinduktiv gekoppeltem Plasma u

12、ndAtomabsorptionspektrometrie (ISO 21587-3:2007)This European Standard was approved by CEN on 13 September 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 alte

13、ration. 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 trans

14、lationunder 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, G

15、reece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement

16、 Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 21587-3:2007: EContents Page 2 EN ISO 21587-3:2007 (E) Foreword 3 1 Scope . 4 2 Normative references 5 3 Determination of residual

17、silica in solution by ICP/AES . 5 4 Determination of iron(III) oxide by ICP/AES 7 5 Determination of titanium(IV) oxide by ICP/AES 9 6 Determination of manganese(II) oxide by ICP/AES 9 7 Determination of calcium oxide by ICP/AES . 10 8 Determination of magnesium oxide by ICP/AES 12 9 Determination o

18、f sodium oxide by ICP/AES . 12 10 Determination of potassium oxide by ICP/AES 13 11 Determination of chromium(III) oxide by ICP/AES . 14 12 Determination of zirconium oxide by ICP/AES . 14 13 Determination of phosphorus(V) oxide by ICP/AES 15 14 Determination of calcium by AAS 17 15 Determination of

19、 magnesium oxide by AAS . 19 16 Determination of sodium oxide by AAS 20 17 Determination of potassium oxide by AAS . 21 18 Determination of manganese oxide by AAS . 21 19 Determination of chromium(III) oxide by AAS 23 20 Test report 24 Foreword The text of ISO 21587-3:2007 has been prepared by Techn

20、ical Committee ISO/TC 33 “Refractories” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 21587-3:2007 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

21、 status of a national standard, either by publication of an identical text or by endorsement, at the latest by March 2008, and conflicting national standards shall be withdrawn at the latest by March 2008. This document supersedes ENV 955-4:1997. According to the CEN/CENELEC Internal Regulations, th

22、e 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, No

23、rway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 21587-3:2007 has been approved by CEN as EN ISO 21587-3:2007 without any modifications. 3 EN ISO 21587-3:2007 (E) 1 Scope This part of ISO 21587 specifies inductivel

24、y coupled plasma/atomic emission (ICP/AE) spectrometry and flame atomic absorption (FAA) spectrometry methods for the chemical analysis of aluminosilicate refractory products and raw materials. The methods are applicable to the determination of the following: silicon(IV) oxide (SiO2) aluminium oxide

25、 (Al2O3) iron(III) oxide (total ir on oxide calculated as Fe2O3) titanium(IV) oxide (TiO2) manganese(II) oxide (MnO) calcium oxide (CaO) magnesium oxide (MgO) sodium oxide (Na2O) potassium oxide (K2O) chromium(III) oxide (Cr2O3) zirconium oxide (ZrO2) phosphorous(V) oxide (P2O5) This part of ISO 215

26、87 gives alternatives to the X-ray flluorescence (XRF) method given in ISO 12677:2003, Chemical analysis of refractory products by XRF Fused cast bead method. 4 EN ISO 21587-3:2007 (E) 2 Normative references The following referenced documents are indispensable for the application of this document. F

27、or dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 21587-1:2007, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 1: Apparatus,

28、reagents, dissolution and gravimetric silica ISO 21587-2:2007, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic abs

29、orption spectrometry and inductively coupled plasma methods 3 Determination of residual silica in solution by ICP/AES 3.1 Principle The residual silica remaining in stock solutions (S1) or (S1) is determined using ICP/AES. 3.2 Reagents Prepare the reagents specified in ISO 26845 and ISO 21587-1 and

30、the following. 3.2.1 Aluminium oxide solution, Al2O35 mg/ml. Weigh 2,65 g of aluminium (purity, more than 99,5 % by mass, having Si, less than 0,001 % by mass) into a platinum dish (e.g. 100 ml). Cover the dish with a watch glass, add approximately 100 ml of hydrochloric acid (1+1) and heat on a ste

31、am bath in order to dissolve the metal. After cooling, dilute to 1 l in a volumetric flask with water. 3.2.2 Matrix solution 1. Transfer an appropriate aliquot portion of the aluminium oxide solution (5 mg/ml) into a 500 ml volumetric flask and dilute to the mark with water. Prepare this solution fr

32、eshly whenever needed. NOTE The amount of the aluminium oxide solution to be used is determined by the chemical composition of the sample. For example, use 35 ml for the aluminium oxide solution of a sample containing 35 % by mass of aluminium oxide. 3.2.3 Matrix solution 2 or 2. Carry out the proce

33、dure given in 4.2.2.3 or 4.2.3.3 of ISO 21587-1:2007 without the sample, but omit heating the fusion mixture or anhydrous sodium carbonate. The solution equivalent to stock solution (S1) or (S1) is referred to as matrix solution 2 or 2, as applicable. 3.2.4 Series 2 solution for calibration. Transfe

34、r appropriate amounts of aliquot portions of dilute standard silicon(IV) oxide solution (0,2 mg/ml) precisely into several 100 ml volumetric flasks, in accordance with the composition of the samples. Add 10 ml each of matrix solution 1 and either matrix solution 2 or 2, respectively, and dilute to t

35、he mark with water. Table 1 is shown as an example. NOTE In Table 2, a typical example of the preparation of solutions is shown. Prepare an appropriate series of solutions for calibration in accordance with the compositions of the samples, and the type and capabilities of instrument used. 5 EN ISO 2

36、1587-3:2007 (E) Table 1 Example of Series 2 solution for calibration Calibration solution Series 2 Matrix solution 1 Matrix solution2 or 2 Dilute standard silicon(IV) oxide solution Concentration of solution No. ml ml ml SiO2mg/100 ml 1 10 10 0 0 2 10 10 1 0,2 3 10 10 2 0,4 4 10 10 5 1,0 5 10 10 10

37、2,0 6 10 10 15 3,0 3.3 Procedure Determine the silicon(IV) oxide remaining in solution (S1) or (S1) (4.2.2.3 or 4.2.3.3 in ISO 21587-1:2007) as follows. Transfer 10 ml of stock solution (S1) or (S1) to a 100 ml volumetric flask, and dilute to the mark with water. This solution, for the determination

38、 of dissolved silicon(IV) oxide, is referred to as diluted 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, for example,

39、the wavelength of 251,61 nm. 3.4 Blank test Carry out the procedure in 3.3 with blank solution (B1) or (B1). The diluted blank solution equivalent to diluted stock solution (S1d) or (S1d) is referred to as diluted blank solution (B1d) or (B1d). 3.5 Plotting the calibration graph Using the calibratio

40、n solution Series 2, carry out the emission procedure described in 3.3. Plot the relation between the emission intensity and the mass of oxide, and 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 r

41、ange of calibration and blank solution solutions for each set of determinations. 3.6 Calculation Calculate the mass fraction of silicon(IV) oxide, wSiO2, as a percentage, from the amount of silicon(IV) oxide derived from the figures obtained from 3.3 and 3.4 and the calibration described in 3.5 usin

42、g the equation: ()()212 3 4SiO50010100mm mmwm+= (1) 6 EN ISO 21587-3:2007 (E) where m is the mass, in g, of the test portion (4.2.2.2 or 4.2.3.2 in ISO 21587-1:2007); m1, m2are the mass, in g, differences in 4.2.2.3 or 4.2.3.3 in ISO 21587-1:2007; m3is the mass, in g, of silicon(IV) oxide in diluted

43、 stock solution (S1d or S1d) as described in 3.3. m4is the mass, in g, of silicon(IV) oxide in diluted blank solution (B1d or B1d) as described in 3.4. 4 Determination of iron(III) oxide by ICP/AES 4.1 Principle The emission intensity of iron is measured by an ICP/AE spectrometer on solutions S1 or

44、S1, obtained from 4.2.2.3 or 4.2.3.3 of ISO 21587-1:2007. 4.2 Reagents Any of the reagents described in 4.1, 4.2 and 4.3 of ISO 21587-1:2007 and the following are required. 4.2.1 Aluminium oxide solution, Al2O32 mg/ml. Dilute aluminium oxide solution (10 mg/ml) with water to a concentration of one-f

45、ifth. 4.2.2 Mixed standard solution 2, Fe2O30,04 mg/ml, TiO20,04 mg/ml, MnO 0,01 mg/ml, Cr2O30,01 mg/ml, ZrO20,01 mg/ml. Transfer 40 ml each of the standard iron(III) oxide solution (1 mg/ml) and the standard titanium(IV) oxide solution (1 mg/ml), and 10 ml each of the standard manganese(II) oxide s

46、olution (1 mg/ml), the standard chromium(III) oxide solution (1 mg/ml) and the standard zirconium oxide solution (1 mg/ml), to a 1 000 ml volumetric flask and dilute to the mark with water. 4.2.3 Matrix solution 2 or 2. See 3.2.3. 4.2.4 Series 3 solutions for calibration. Transfer appropriate aliquo

47、t portions of mixed standard solution 2 into each of several 100 ml volumetric flasks. Add 10 ml of matrix solution 2 or matrix solution 2, 5 ml of internal standard solution (Sc 0,1 mg/ml, Y 0,1 mg/ml), and a specified amount of aluminium oxide solution (2 mg/ml), respectively, and dilute to the ma

48、rk with water. NOTE An example of the preparation of solutions is shown in Table 2. Prepare an appropriate series of solutions for calibration in accordance with the composition of the samples, and the type and capabilities of instrument used. 7 EN ISO 21587-3:2007 (E) Table 2 Example of Series 3 so

49、lution for calibration (mass fraction of aluminium oxide is 30 %) Solution for calibration Matrix solution 2 or 2 Internal standard solution Aluminium oxide solution Mixed standard solution 2 Concentration of solution No. ml ml ml ml mg/100 ml Fe2O3TiO2MnO Cr2O3ZrO21 10 5 3 0 0,00 0,00 0,00 0,00 0,00 2 10 5 3 1 0,04 0,04 0,01 0,01 0,01 3 10 5 3 2 0,08 0,08 0,02 0,02 0,02 4 10 5 3 3 0,12 0,12 0,03 0,03 0,03 5 10 5 3 4 0,16 0,16 0,04 0,04 0,04 6 10 5 3 5 0,20 0,20 0,05 0,05 0,05 7 10 5 3 10 0,40 0,4