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

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1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58(alternative to the X-ray fluorescence method) Part 3: Inductively coupled plasma and atomic absorp

2、tion spectrometry methodsThe European Standard EN ISO 21587-3:2007 has the status of a British StandardICS 81.080Chemical analysis of aluminosilicate refractory products BRITISH STANDARDBS EN ISO 21587-3:2007BS EN ISO 21587-3:2007This British Standard was published under the authority of the Standar

3、ds Policy and Strategy Committee on 31 October 2007 BSI 2007ISBN 978 0 580 57921 9Amendments issued since publicationAmd. No. Date CommentsThis publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a Brit

4、ish Standard cannot confer immunity from legal obligations.National forewordThis British Standard is the UK implementation of EN ISO 21587-3:2007. Together with BS EN ISO 21587-1:2007, it supersedes DD ENV 955-4:1997 which is withdrawn.The UK participation in its preparation was entrusted to Technic

5、al Committee RPI/1, Refractory products and materials.A list of organizations represented on this committee can be obtained on request to its secretary.EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 21587-3September 2007ICS 81.080 Supersedes ENV 955-4:1997 English VersionChemical analysis of

6、aluminosilicate 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) - Pa

7、rtie 3: Mthodes 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 gekoppelt

8、em Plasma undAtomabsorptionspektrometrie (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 witho

9、ut 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 official versions (English, French, German). A version in any other language ma

10、de 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, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France,

11、 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 STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUN

12、GManagement 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: EForeword The text of ISO 21587-3:2007 has been prepared by Technical Committee ISO/TC 33 “Refractories” o

13、f 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 status of a national standard, either by

14、 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, the national standards organizations of the

15、 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, Romania, Slovakia

16、, 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. EN ISO 21587-3:2007Reference numberISO 21587-3:2007(E)INTERNATIONAL STANDARD ISO21587-3First edition2007-03-01Chemical

17、 analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 3: Inductively coupled plasma and atomic absorption spectrometry methods Analyse chimique des produits rfractaires daluminosilicates (mthode alternative la mthode par fluorescence de rayons X) Partie

18、 3: Mthodes par spectromtrie dabsorption atomique (AAS) et spectromtrie dmission atomique avec plasma induit par haute frquence (ICP-AES) EN ISO 21587-3:2007ii iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 2 3 Determination of residual silica in solution by ICP/AES 2 4 Determinat

19、ion of iron(III) oxide by ICP/AES. 4 5 Determination of titanium(IV) oxide by ICP/AES . 6 6 Determination of manganese(II) oxide by ICP/AES. 6 7 Determination of calcium oxide by ICP/AES 7 8 Determination of magnesium oxide by ICP/AES . 9 9 Determination of sodium oxide by ICP/AES 9 10 Determination

20、 of potassium oxide by ICP/AES . 10 11 Determination of chromium(III) oxide by ICP/AES 11 12 Determination of zirconium oxide by ICP/AES 11 13 Determination of phosphorus(V) oxide by ICP/AES . 12 14 Determination of calcium by AAS . 14 15 Determination of magnesium oxide by AAS 16 16 Determination o

21、f sodium oxide by AAS . 17 17 Determination of potassium oxide by AAS 18 18 Determination of manganese oxide by AAS 18 19 Determination of chromium(III) oxide by AAS . 20 20 Test report . 21 EN ISO 21587-3:2007iv Foreword ISO (the International Organization for Standardization) is a worldwide federa

22、tion 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 committ

23、ee. 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

24、 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. Publication as an International Standard requires ap

25、proval 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 21587-3 was prepared by Technical Co

26、mmittee ISO/TC 33, Refractories. ISO 21587 consists of the following parts, under the general title Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method): Part 1: Apparatus, reagents, dissolution and gravimetric silica Part 2: Wet chemical analysis P

27、art 3: Inductively coupled plasma and atomic absorption spectrometry methods EN ISO 21587-3:20071Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 3: Inductively coupled plasma and atomic absorption spectrometry methods 1 Scope This part of

28、ISO 21587 specifies inductively 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

29、) oxide (SiO2) aluminium oxide (Al2O3) iron(III) oxide (total iron 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) oxid

30、e (P2O5) This part of ISO 21587 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. EN ISO 21587-3:20072 2 Normative references The following referenced documents are indispensable for the applica

31、tion 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 21587-1:2007, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence met

32、hod) Part 1: Apparatus, 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 chemi

33、cal analysis, atomic absorption 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 26

34、845 and ISO 21587-1 and 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

35、 (1+1) and heat on a steam 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.

36、Prepare this solution freshly 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 o

37、r 2. Carry out the procedure 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

38、for calibration. Transfer 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, respe

39、ctively, and dilute to the 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 ins

40、trument used. EN ISO 21587-3:20073Table 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

41、 5 1,0 5 10 10 10 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

42、 the determination 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

43、 at, for example, 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 Us

44、ing the calibration 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 carrie

45、d out, using the range 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 des

46、cribed in 3.5 using the equation: ()()212 3 4SiO50010100mm mmwm+= (1) EN ISO 21587-3:20074 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) oxi

47、de in diluted 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 sol

48、utions S1 or 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 concentra

49、tion of one-fifth. 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 solution (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 volu