EN ISO 20565-3-2008 en Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) - Part 3 Flame atomic.pdf

1、BS EN ISO20565-3:2008ICS 81.080NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDChemical analysisof chrome-bearingrefractory productsand chrome-bearingraw materials(alternative to theX-ray fluorescencemethod)Part 3: Flame atomic absorptionspectrometry (FAAS) and

2、inductivelycoupled plasma atomic emissionspectrometry (ICP- AES) (ISO 20565-3:2008) Incorporating corrigendum September 2010National forewordThis British Standard is the UK implementation of EN ISO 20565-3:2008. Together with BS EN ISO 20565-1:2008 and BS EN ISO 20565-2:2008, it supersedes BS 1902-2

3、.2:1974 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee RPI/1, Refractory products and materials.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the nece

4、ssary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.BS EN ISO 20565-3:2008This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March

5、2009 BSI 2010Amendments/corrigenda issued since publicationDate Comments 30 September 2010 Addition of supersession detailsISBN 978 0 580 72654 5EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 20565-3December 2008ICS 81.080English VersionChemical analysis of chrome-bearing refractory products

6、andchrome-bearing raw materials (alternative to the X-rayfluorescence method) - Part 3: Flame atomic absorptionspectrometry (FAAS) and inductively coupled plasma atomicemission spectrometry (ICP-AES) (ISO 20565-3:2008)Analyse chimique des produits rfractaires contenant duchrome et des matires premir

7、es contenant du chrome(mthode alternative la mthode par fluorescence derayons X) - Partie 3: Mthodes par spectromtriedabsorption atomique dans la flamme (FAAS) etspectromtrie dmission atomique avec plasma induit parhaute frquence (ICP-AES) (ISO 20565-3:2008)Chemische Analyse von chromhaltigen feuerf

8、estenErzeugnissen und chromhaltigen Rohstoffen (Alternativezum Rntgenfluoreszenzverfahren) - Teil 3:Flammenatomabsorptionsspektrometrie (FAAS) undAtomemissionsspektrometrie mit induktiv gekoppeltemPlasma (ICP-AES) (ISO 20565-3:2008)This European Standard was approved by CEN on 8 November 2008.CEN me

9、mbers 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 alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on applicati

10、on 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the

11、 same status as theofficial 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,R

12、omania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT 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 reserved

13、worldwide for CEN national Members.Ref. No. EN ISO 20565-3:2008: E3 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 secretariat of which is held

14、 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 to the possibility that som

15、e 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 countries are bound to impl

16、ement 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, Spain, Sweden, Switzerland

17、 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. BS EN ISO 20565-3:2008EN ISO 20565-3:2008 (E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope 1 2 Normative references 2 3 Instrument

18、al methods using inductively coupled plasma emission spectrometry (ICP-AES) 2 4 Instrumental methods using flame absorption spectrophotometry (FAAS) .10 5 Test report 14 Bibliography 15 BS EN ISO 20565-3:2008EN ISO 20565-3:2008 (E)iv ISO 2010 All rights reservedForeword ISO (the International Organi

19、zation for Standardization) is a worldwide federation 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 establishe

20、d has the right to be represented on that committee. 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.

21、International Standards are drafted in accordance with 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. Pub

22、lication as an International Standard requires approval 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

23、 rights. ISO 20565-3 was prepared by Technical Committee ISO/TC 33, Refractories, in collaboration with Technical Committee CEN/TC 187, Refractory products and materials. ISO 20565 consists of the following parts, under the general title Chemical analysis of chrome-bearing refractory products and ch

24、rome-bearing raw materials (alternative to the X-ray fluorescence method): Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (I

25、CP-AES) BS EN ISO 20565-3:2008EN ISO 20565-3:2008 (E)INTERNATIONAL STANDARD ISO 2010 All rights reserved 1Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 3: Flame atomic absorption spectrometry (FAAS) and in

26、ductively coupled plasma atomic emission spectrometry (ICP-AES) 1 Scope This part of ISO 20565 specifies flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods for the chemical analysis of chrome-bearing refractory products and chrom

27、e-bearing raw materials. It is applicable in the ranges of determination given in Table 1. ISO 20565 gives alternatives to the X-ray fluorescence (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,

28、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 are after the loss on ignition (LOI) has been taken into account. BS EN ISO 20565-3:2008EN ISO 20565-3:2008 (E)2 ISO 2010 All rights reserved2 Normative reference

29、s The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 20565-1:2008, Chemical analysis of chrome-b

30、earing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption s

31、pectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods 3 Instrumental methods using inductively coupled plasma emission spectrometry (ICP-AES) 3.1 Determination of residual silica in stock solutions (S1) by ICP-AES 3.1.1 Principle The residual silica remainin

32、g 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, 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) o

33、xide 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 ISO 20565-1:2008, 9.2.2.3, without the sample, but omit heating the fusion mixture or anhydrous sodium carbonate. The equivalent solution

34、 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) oxide standard solution (0,08 mg/ml) precisely into several 100 ml volumetric flasks in accordance with the composition of the samples.

35、 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 accordance with the compositions of the samples, and the type and capabilities of the instrument used, an appropriate series of solutions for c

36、alibration is prepared. BS EN ISO 20565-3:2008EN ISO 20565-3:2008 (E) ISO 2010 All rights reserved 3Table 2 Example of series 2 solution for calibration Solution No. Matrix solution 2 ml Diluted silicon(IV) oxide standard solution ml Concentration of solution SiO2 mg/100 ml 1 10 0 0 2 10 5 0,4 3 10

37、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 100 ml volumetric flask and dilute to the mark with water. This solution, for the determination of dissolved

38、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 emission intensity at, for example, the wavelength of 251,611 nm. 3.1.4 Blank test Carry out the procedure in 3.1

39、.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 calibration graph Calibrate the ICP-AE spectrometer using the series 2 solution (3.1.3.3) and the emission procedure

40、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 new calibration should be carried out using the range of calibration and blank solution solutions for each set

41、 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 obtained from 3.1.3 and 3.1.4 and the calibration prepared in 3.1.5. ()()212 sbSiO25010100mm mmwm+= (1) where

42、 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, in grams (g); msis the mass of silicon(IV) oxide in diluted stock solution (S1d) as described in 3.1.3, in gra

43、ms (g); mbis the mass of silicon(IV) oxide in diluted blank solution (B1d) as described in 3.1.4, in grams (g). BS EN ISO 20565-3:2008EN ISO 20565-3:2008 (E)4 ISO 2010 All rights reserved3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, manganese(II) oxide

44、, 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, titanium(IV) oxide, manganese(II) oxide, calcium oxide, magnesium oxide, chromium(I

45、II) 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 with Table 3. Table 3 Application range (% by mass) Component Range SiO20,1 to 10 Al2O3

46、0,05 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 silicon(IV) oxide. NOTE 2 Determination of calcium oxide by this method cannot be app

47、lied 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 solution 3, SiO20,04 mg/ml, Al2O30,04 mg/ml, Fe2O30,04 mg/ml, TiO20,005 mg/ml, MnO 0

48、,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(II) oxide (5 ml), calcium oxide (40 ml), chromium(III) oxide (40 ml) and zirconium oxi

49、de (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 omit 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. BS EN ISO 20565-3:2008EN ISO 20565-3:2008 (E) ISO 2010 All rights reserved 53.2.2.3 Internal standard solution. Transfer 10 ml of st