DIN EN ISO 21079-3-2008 Chemical analysis of refractories containing alumina zirconia and silica - Refractories containing 5 % to 45 % of ZrO (alternative to the X-ray fluorescence.pdf

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1、August 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!$Q/I“1461238www.

2、din.deDDIN EN ISO 21079-3Chemical analysis of refractories containing alumina, zirconia andsilica X-ray fluorescence method) Part 3: Flame atomic absorption spectrophotometry (FAAS) andinductively coupled plasma emission spectrometry (ICP-AES)(ISO 21079-3:2008)English version of DIN EN ISO 21079-3:2

3、008-08Chemische Analyse von aluminiumoxid-, zirkoniumoxid- und silicium(IV)-oxidhaltigenfeuerfesten Erzeugnissen (Alternative zum Rntgenfluoreszenzverfahren) Teil 3: Flammenatomabsorptionsspektrophotometrie (FAAS) undAtomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES)(ISO 21079-3:20

4、08)Englische Fassung DIN EN ISO 21079-3:2008-08www.beuth.deRefractories containing 5 % to 45 % of ZrO2(alternative to theFeuerfeste Erzeugnisse mit einem Massenanteil an ZrO2von 5 % bis 45 %Document comprises 18 pagesDIN EN ISO 21079-3:2008-08 2 National foreword This standard has been prepared by T

5、echnical Committee ISO/TC 33 “Refractories” in collaboration with Technical Committee CEN/TC 187 “Refractory products and materials” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committ

6、ee), Technical Committee NA 062-02-61 AA Chemische Analyse von oxidischen Roh- und Werkstoffen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 12677 DIN EN ISO 12677 ISO 21079-1 DIN EN ISO 21079-1 ISO 26845 DIN EN ISO 26845 National An

7、nex NA (informative) Bibliography DIN EN ISO 12677, Chemical analysis of refractory products by XRF Fused cast bead method 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 m

8、ethod) Part 1: Apparatus, reagents and dissolution DIN EN ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods EUROPEAN STANDARD NORME EUROPENNE

9、EUROPISCHE NORM EN ISO 21079-3 April 2008 ICS 81.080; 71.040.40 English Version Chemical analysis of refractories containing alumina, zirconia, and silica - Refractories containing 5 percent to 45 percent of ZrO2(alternative to the X-ray fluorescence method) - Part 3: Flame atomic absorption spectro

10、photometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) (ISO 21079-3:2008) Analyse chimique des matriaux rfractaires contenant de lalumine, de la zircone et de la silice - Matriaux rfractaires contenant de 5 % 45 % de ZrO2(mthode alternative la mthode par fluorescence de ray

11、ons X) - Partie 3: Mthodes par spectromtrie dabsorption atomique dans la flamme (FAAS) et spectromtrie dmission atomique avec plasma induit par haute frquence (ICP-AES) (ISO 21079-3:2008) und silicium(IV)-oxidhaltigen feuerfesten Erzeugnissen - Feuerfeste Erzeugnisse mit einem Massenanteil an ZrO2vo

12、n 5 % bis 45 % (Alternative zum Rntgenfluoreszenzverfahren) - Teil 3: Flammenatomabsorptionsspektrophotometrie (FAAS) und Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) (ISO 21079-3:2008) This European Standard was approved by CEN on 12 April 2008. CEN members are bound to comp

13、ly 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 on application to the CEN Managem

14、ent 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 Centre has the same status as the

15、 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, Poland, Portugal, Romania, Slovakia

16、, 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 and by any means reserved worldwide f

17、or CEN national Members. Ref. No. EN ISO 21079-3:2008: EChemische Analyse von aluminiumoxid-, zirkoniumoxid- Contents Page 2 DIN EN ISO 21079-3:2008-08EN ISO 21079-3:2008 (E) Foreword3 1 Scope 4 2 Normative references 4 3 Instrumental methods using ICP-AES.4 3.1 Determination of residual silica in s

18、olution by ICP-AES .4 3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, calcium oxide, magnesium oxide, chromium(III) oxide and hafnium oxide using stock solutions (S1), (S1) or (S1) by ICP-AES6 3.3 Determination of calcium oxide, magnesium oxide, sodium o

19、xide and potassium oxide using stock solutions (S4) by ICP-AES 10 4 Instrumental methods using Flame Atomic Absorption Spectrometry (FAAS). 11 4.1 Determination of calcium oxide, magnesium oxide, sodium oxide and potassium oxide using stock solutions (S3) by FAAS. 11 4.2 Determination of chromium(II

20、I) oxide by FAAS spectrometry. 13 5 Calculation and expression of test results 15 6 Test report . 15 Bibliography. 16 3 EN ISO 21079-3:2008 (E) -DIN EN ISO 21079-3:2008-08Foreword This document (EN ISO 21079-3:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration w

21、ith 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 October 2008, and conflicting nation

22、al standards shall be withdrawn at the latest by October 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/CE

23、NELEC 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, Luxe

24、mbourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, 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. 1 Scope This part of ISO 21079 specifies f

25、lame 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 ZrO2) and raw materials. This part of ISO 21079 is not applicable to MgO-based

26、 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 document. For dated references, only the edition cited applies. For undated refe

27、rences, 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 ZrO2(alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents

28、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-AES 3.1 Determination of residual silica in solution by ICP-AES 3.1.1 Princi

29、ple 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 necessary. 4 DIN EN ISO 21079-3:2008-08EN ISO 21079-3:2008 (E) 3.1.2.2 Diluted si

30、licon(IV) oxide standard solution, SiO20,08 mg/ml. Transfer 20 ml of the silicon(IV) oxide standard solution (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 withou

31、t the sample, but omit heating the fusion mixture or anhydrous sodium carbonate. Designate the solution 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 sta

32、ndard solution (0,08 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 or 1 and dilute to the mark with water. Table 1 shows a typical example of the preparation of solutions. An appropriate series of soluti

33、ons for calibration should be prepared, depending on the compositions of the samples and the types and capabilities 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

34、 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 Determine 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 t

35、o the mark with water. Designate this solution for the determination of dissolved silicon(IV) oxide 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, an

36、d measure the emission intensity at an appropriate wavelength, for example, 251,611 nm. 3.1.4 Blank test 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 di

37、luted blank solution (B1d or B1d). 5 EN ISO 21079-3:2008 (E) DIN EN ISO 21079-3:2008-083.1.5 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 oxide, prepare th

38、e 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(SiO2), expressed

39、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 9.2.2.2 or 9.2.

40、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 or S1d) as desc

41、ribed 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 hafnium oxide usi

42、ng 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 solutions (S1),

43、(S1) or (S1). The ICP-AES method is applicable to the components in (S1), (S1) or (S1) as given in Table 2. 6 DIN EN ISO 21079-3:2008-08EN ISO 21079-3:2008 (E) Table 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 Cr2O

44、30,01 to 3 HfO20,01 to 2 NOTE 1 When solutions (S1) or (S1) are used, the SiO2is residual silica. When solution (S1) is used, the SiO2is all of the silicon(IV) oxide. NOTE 2 This method cannot be applied to silicon(IV) oxide and aluminium oxide contents of more than 10 % by mass. 3.2.2 Reagents 3.2.

45、2.1 General Prepare the reagents given in 3.2.2.2 to 3.2.2.7 and those specified in ISO 26845, as necessary. 3.2.2.2 Scandium standard solution, Sc 1,0 mg/ml. Dry about 0,2 g of scandium oxide at 110 C 5 C for 60 min, cool in a desiccator. Weigh 0,153 4 g of this, transfer to a 100 ml beaker, gradua

46、lly add 10 ml of hydrochloric acid (1+1) to dissolve, and dilute precisely to 1 l in a volumetric flask with water. A suitable commercial standard solution may be used. 3.2.2.3 Yttrium standard solution, Y 1,0 mg/ml. Dry about 0,2 g of yttrium oxide at 110 C 5 C for 60 min, cool in a desiccator. Wei

47、gh 0,127 0 g of this, transfer to a 100 ml beaker.Dissolve by gradually adding 10 ml of hydrochloric acid (1+1) to dissolve, and dilute precisely to 1 l in a volumetric flask with water. A suitable commercial standard solution may be used. 3.2.2.4 Internal standard solution. Transfer 10 ml of yttriu

48、m or scandium standard solution into a volumetric 100 ml flask, and dilute to the mark with water. Prepare this solution immediately prior to use. 3.2.2.5 Mixed standard solution 2, SiO20,1 mg/ml, Al2O30,10 mg/ml, Fe2O30,02 mg/ml, CaO 0,02 mg/ml, MgO 0,2 mg/ml, HfO20,02 mg/ml, Cr2O30,03 mg/ml and Ti

49、O20,05 mg/ml. Transfer 50 ml each of the silicon(IV) oxide and the aluminium oxide, 10 ml each of the iron(III) oxide, the calcium oxide, the magnesium oxide and the hafnium oxide, 15 ml of the chromium(III) oxide, and 25 ml of the titanium(IV) oxide standard solutions into a 500 ml volumetric flask, and dilute to the mark with water. 7 EN ISO 21079-3:2008 (E) DIN EN ISO 21079-3:2008-083.2.2.6 Matrix solution 1, 1 or 1. Carry out the procedure given in 9.2.2.3, 9.2.3.3 or 9.2.4.3 of ISO 21079-