DIN EN ISO 20565-3-2009 Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) - Part 3 Flame atomi.pdf

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1、June 2009DEUTSCHE 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 71.040.40; 81.080!$X5v“15

2、31883www.din.deDDIN EN ISO 20565-3Chemical analysis of chrome-bearing refractory products andchrome-bearing raw materials (alternative to the X-ray fluorescencemethod) Part 3: Flame atomic absorption spectrometry (FAAS) and inductivelycoupled plasma atomic emission spectrometry (ICP-AES)(ISO 20565-3

3、:2008)English version of DIN EN ISO 20565-3:2009-06Chemische Analyse von chromhaltigen feuerfesten Erzeugnissen und chromhaltigenRohstoffen (Alternative zum Rntgenfluoreszenzverfahren) Teil 3: Flammenatomabsorptionsspektrometrie (FAAS) und Atomemissionsspektrometriemit induktiv gekoppeltem Plasma (I

4、CP-AES) (ISO 20565-3:2008)Englische Fassung DIN EN ISO 20565-3:2009-06Together with DIN EN ISO 20565-1:2009-06 and DIN EN ISO 20565-2:2009-06 supersedesDIN 51074-1:1971-08, DIN 51074-2:1971-08, DIN 51074-3:1971-08 and DIN 51074-4:1971-08Supersedes: see belowwww.beuth.deDocument comprises pages20DIN

5、EN ISO 20565-3:2009-06 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 20565-3:2008 as a European

6、 Standard. ISO 20565-3 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 062-02-61 AA Chemische Analyse von oxidischen Roh- und W

7、erkstoffen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 12677 DIN EN ISO 12677 ISO 20565-1 DIN EN ISO 20565-1 ISO 26845 DIN EN ISO 26845 Amendments This standard differs from DIN 51074-1:1971-08, DIN 51074-2:1971-08, DIN 51074-3:197

8、1-08 and DIN 51074-4:1971-08 as follows: a) The standard has been completely revised taking into account the current chemical analysis aspects. Previous editions DIN 51074-1: 1971-08 DIN 51074-2: 1971-08 DIN 51074-3: 1971-08 DIN 51074-4: 1971-08 National Annex NA (informative) Bibliography DIN EN IS

9、O 12677, Chemical analysis of refractory products by XRF Fused cast bead method 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 determination of gr

10、avimetric silica DIN EN ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, AAS and ICP methods NORME EUROPENNE EUROPISCHE NORM December 2008 ICS 81.080 English Version Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (

11、alternative to the X-ray fluorescence method) Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) (ISO 20565-3:2008) Analyse chimique des produits rfractaires contenant du chrome et des matires premires contenant du chrome (mthode

12、 alternative la mthode par fluorescence de rayons X) Partie 3: Mthodes par spectromtrie dabsorption atomique dans la flamme (FAAS) et spectromtrie dmission AES) (ISO 20565-3:2008) Chemische Analyse von chromhaltigen feuerfesten Erzeugnissen und chromhaltigen Rohstoffen (Alternative zum Rntgenfluores

13、zenzverfahren) Teil 3: Flammenatomabsorptionsspektrometrie (FAAS) und Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) (ISO 20565-3:2008) This European Standard was approved by CEN on 8 November 2008. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which

14、 stipulate the conditions for giving this EuropeanStandard 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 Management Centre or to any CEN member. This European Stan

15、dard exists in three official 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 stan

16、dards 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, Slovenia, Spain, Sweden, Switzerland and United King

17、dom. 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 for CEN national Members. Ref. No. EN ISO 20565-3:2008:

18、 EEUROPEAN STANDARD EN ISO 20565-3 atomique avec plasma induit par haute frquence(ICP-Contents Page 1 Scope 4 2 Normative references 5 3 Instrumental methods using inductively coupled plasma emission spectrometry (ICP-AES) 5 4 Instrumental methods using flame absorption spectrophotometry (FAAS) .13

19、5 Test report 17 Bibliography 18 DIN EN ISO 20565-3:2009-06EN ISO 20565-3:2008 (E)2Foreword3 3 Foreword This document (EN ISO 20565-3:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration with Technical Committee CEN/TC 187 “Refractory products and materials” the s

20、ecretariat 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 June 2009, and conflicting national standards shall be withdrawn at the latest by June 2009. Attention is drawn

21、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 organizations of the following

22、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, Slovakia, Slovenia,

23、 Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 20565-3:2008 has been approved by CEN as a EN ISO 20565-3:2008 without any modification. DIN EN ISO 20565-3:2009-06EN ISO 20565-3:2008 (E)1 Scope This part of ISO 20565 specifies flame atomic absorption spectromet

24、ry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods for the chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials. It is applicable in the ranges of determination given in Table 1. ISO 20565 gives alternatives to the X-ray fluore

25、scence (XRF) method given in ISO 12677. Table 1 Range of determination (% by mass) Component Range SiO20,5 to 10 Al2O32 to 30 Fe2O30,5 to 25 TiO20,01 to 1 MnO 0,01 to 1 CaO 0,01 to 3 MgO 15 to 85 Na2O 0,01 to 1 K2O 0,01 to 1 Cr2O32 to 60 ZrO20,01 to 0,5 P2O50,01 to 5 LOI 0,5 to 5 NOTE These values a

26、re after the loss on ignition (LOI) has been taken into account. DIN EN ISO 20565-3:2009-06EN ISO 20565-3:2008 (E)42 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated refer

27、ences, the latest edition of the referenced document (including any amendments) applies. ISO 20565-1:2008, 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 determinatio

28、n of gravimetric silica 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 3 Instrumental methods using inductively coupled plasma emission spe

29、ctrometry (ICP-AES) 3.1 Determination of residual silica in stock solutions (S1) by ICP-AES 3.1.1 Principle The residual silica remaining in solution in solutions (S1) is determined using ICP-AES. 3.1.2 Reagents Prepare the following reagents in addition to any reagents described in ISO 20565-1:2008

30、, Clause 5, that are necessary. 3.1.2.1 Diluted silicon(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. 3.1.2.2 Matrix solution 2. Carry out the procedure given in I

31、SO 20565-1:2008, 9.2.2.3, without the sample, but omit heating the fusion mixture or anhydrous sodium carbonate. The equivalent solution to stock solution (S1) is referred to as matrix solution 2. 3.1.2.3 Series 2 solution for calibration. Transfer appropriate aliquot portions of diluted silicon(IV)

32、 oxide standard 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 2 (3.1.2.2) and dilute to the mark with water. In Table 2, a typical example of the preparation of solutions is shown. In accorda

33、nce with the compositions of the samples, and the type and capabilities of the instrument used, an appropriate series of solutions for calibration is prepared. DIN EN ISO 20565-3:2009-06EN ISO 20565-3:2008 (E)5Table 2 Example of series 2 solution for calibration Solution No. Matrix solution 2 ml Dil

34、uted silicon(IV) oxide standard solution ml Concentration of solution SiO2 mg/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) (see ISO 20565-1) as follows. Transfer 10 ml of stock solution (S1) to a

35、 100 ml volumetric flask and dilute to the mark with water. This solution, for the determination of dissolved silicon(IV) oxide, is referred to as diluted stock solution (S1d). Spray a portion of diluted stock solution (S1d) into the argon plasma flame of the ICP-AE spectrometer, and measure the emi

36、ssion intensity at, for example, the wavelength of 251,611 nm. 3.1.4 Blank test Carry out the procedure in 3.1.3 with blank solution (B1) (see ISO 20565-1). The equivalent diluted blank solution to diluted stock solution (S1d) is referred to as diluted blank solution (B1d). 3.1.5 Plotting of calibra

37、tion graph Calibrate the ICP-AE spectrometer using the series 2 solution (3.1.3.3) and the emission procedure described in 3.1.3. Plot the relation between the emission intensity and mass of oxide. Prepare the calibration graph by adjusting the curve so that it passes through the point of origin. A

38、new calibration should be carried out using the range of calibration and blank solution solutions for each set of determinations. 3.1.6 Calculation Calculate the mass fraction of silicon(IV) oxide, 2SiO,w as a percentage, using Equation (1). Use the mass of silicon(IV) oxide derived from the figures

39、 obtained from 3.1.3 and 3.1.4 and the calibration prepared in 3.1.5. ()()212 sbSiO25010100mm mmwm+= (1) where m is the mass of the test portion (see ISO 20565-1), in grams (g); m1is the first mass from ISO 20565-1:2008, 9.2.2.3.3, in grams (g);m2is the second mass from ISO 20565-1:2008, 9.2.2.3.3,

40、in grams (g); msis the mass of silicon(IV) oxide in diluted stock solution (S1d) as described in 3.1.3, in grams (g); mbis the mass of silicon(IV) oxide in diluted blank solution (B1d) as described in 3.1.4, in grams (g). DIN EN ISO 20565-3:2009-06EN ISO 20565-3:2008 (E)63.2 Determination of silicon

41、(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, manganese(II) oxide, calcium oxide, magnesium oxide, chromium(III) oxide and zirconium oxide using stock solutions (S1) or (S1) by ICP-AES 3.2.1 Principle The emission intensities of silicon(IV) oxide, aluminium oxide, iron(III) oxide

42、, titanium(IV) oxide, manganese(II) oxide, calcium oxide, magnesium oxide, chromium(III) oxide and zirconium oxide are measured by an ICP-AE spectrometer for stock solutions (S1) (see ISO 20565-1) or (S1) (see ISO 20565-1). This method should be applied to components in (S1) or (S1) in accordance wi

43、th Table 3. Table 3 Application range (% by mass) Component Range SiO20,1 to 10 Al2O30,05 to 10 Fe2O30,01 to 10 TiO20,01 to 1 MnO 0,01 to 1 CaO 0,01 to 10 Cr2O30,01 to 10 ZrO20,01 to 0,5 NOTE 1 When solution (S1) is used, the SiO2is residual silica. When solution (S1) is used, the SiO2is all of the

44、silicon(IV) oxide. NOTE 2 Determination of calcium oxide by this method cannot be applied to calcium oxide contents of more than 10 % by mass. 3.2.2 Reagents Prepare the following reagents in addition to any reagents described in ISO 20565-1:2008, Clause 5, that are necessary. 3.2.2.1 Mixed standard

45、 solution 3, SiO20,04 mg/ml, Al2O30,04 mg/ml, Fe2O30,04 mg/ml, TiO20,005 mg/ml, MnO 0,005 mg/ml, CaO 0,04 mg/ml, Cr2O30,04 mg/ml, ZrO20,005 mg/ml. Transfer aliquot portions of standard silicon(IV) oxide (40 ml), aluminium oxide (40 ml), iron(III) oxide (40 ml), titanium(IV) oxide (5 ml), manganese(I

46、I) oxide (5 ml), calcium oxide (40 ml), chromium(III) oxide (40 ml) and zirconium oxide (5 ml) solutions to a 1 000 ml volumetric flask and dilute to the mark with water. 3.2.2.2 Matrix solution 3 or 3. Carry out the procedure given in ISO 20565-1:2008, 9.2.2.3 or 9.2.3.3, without the sample, but om

47、it heating the fusion mixture or anhydrous sodium carbonate. The equivalent solution to stock solution (S1) or (S1) is referred to as matrix solution 3 or 3 as applicable. DIN EN ISO 20565-3:2009-06EN ISO 20565-3:2008 (E)73.2.2.3 Internal standard solution. Transfer 10 ml of standard scandium oxide

48、solution (1 mg/ml) and standard yttrium oxide solution (1 mg/ml) to a 100 ml volumetric flask and dilute to the mark with water. Prepare when necessary. 3.2.2.4 Series 3 solutions for calibration. Transfer appropriate aliquot portions of mixed standard solution 3 to each of several 100 ml volumetric

49、 flasks. Add 20 ml of matrix solution 3 or matrix solution 3 and 5 ml of internal standard solution, respectively, and dilute to the mark with water. In Table 4, an example of the preparation of solutions is shown. Prepare an appropriate solution series for calibration in accordance with the composition of the sample, the type and capabilities of instrument used. When using this approach to calibration, it is essential to check for line interferences of any of these oxides on each other. If any are present, appropriate corre