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1 psbkph=pq^ka^oa== ppjbk=fpl=onrutjpwommt== Fastställd/Approved: Publicerad/Published: Utgåva/Edition: 1 Språk/Language: engelska/english ICS: = `ÜÉãáÅ~ä=~å~äóëáë=çÑ=~äìãáåçëáäáÅ~íÉ=êÉÑê~Åíçêó=éêçÇìÅíë== E~äíÉêå~íáîÉ=íç=íÜÉ=uJê~ó=ÑäìçêÉëÅÉåÅÉ=ãÉíÜçÇF=Ó== m~êí=pw=fåçìåíáîéäó=åçìéäéç=éä~ëã~=~åç=~íçãáå=~äëçêéíáçå= ëééåíêçãéíêó=ãéíüççë=efpl=onrutjpwommtf

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3 Europastandarden EN ISO :2007 gäller som svensk standard. Detta dokument innehåller den officiella engelska versionen av EN ISO :2007. Denna standard ersätter SS-EN 955-2, utgåva 1. The European Standard EN ISO :2007 has the status of a Swedish Standard. This document contains the official English version of EN ISO :2007. This standard supersedes the Swedish Standard SS-EN 955-2, edition 1. >«=`çéóêáöüílrééüçîëê ííéå=íáää=çéåå~=éêççìâí=íáääü ê=pfpi=pïéçáëü=pí~åç~êçë=fåëíáíìíéi=píçåâüçäãi=pîéêáöék=^åî åçåáåöéå== ~î=çéåå~=éêççìâí=êéöäéê~ë=~î=ëäìí~åî åç~êäáåéåëéå=ëçã= íéêñáååë=á=çéåå~=éêççìâíi=ëé=ëí~åç~êçéåë=ëáëí~=ëáççêk= «=`çéóêáöüí=pfpi=pïéçáëü=pí~åç~êçë=fåëíáíìíéi=píçåâüçäãi=pïéçéåk=^ää=êáöüíë=êéëéêîéçk=qüé=ìëé=çñ=íüáë=éêççìåí=áë=öçîéêåéç== Äó=íÜÉ=ÉåÇJìëÉê=äáÅÉåÅÉ=Ñçê=íÜáë=éêçÇìÅíK=vçì=ïáää=ÑáåÇ=íÜÉ=äáÅÉåÅÉ=áå=íÜÉ=ÉåÇ=çÑ=íÜáë=ÇçÅìãÉåíK= rééäóëåáåö~ê=çã=ë~âáååéü ääéí=á=ëí~åç~êçéå=ä ãå~ë=~î=pfpi=pïéçáëü=pí~åç~êçë=fåëíáíìíéi=íéäéñçå=mujrrr=rom=mmk== pí~åç~êçéê=â~å=äéëí ää~ë=üçë=pfp=c êä~ö=^_=ëçã= îéå=ä ãå~ê=~ääã åå~=ìééäóëåáåö~ê=çã=ëîéåëâ=çåü=ìíä åçëâ=ëí~åç~êçk= fåñçêã~íáçå=~äçìí=íüé=åçåíéåí=çñ=íüé=ëí~åç~êç=áë=~î~áä~ääé=ñêçã=íüé=pïéçáëü=pí~åç~êçë=fåëíáíìíé=epfpfi=íéä=hqs=u=rrr=rom=mmk== pí~åç~êçë=ã~ó=äé=çêçéêéç=ñêçã=pfp=c êä~ö=^_i=ïüç=å~å=~äëç=éêçîáçé=öéåéê~ä=áåñçêã~íáçå=~äçìí=pïéçáëü=~åç=ñçêéáöå=ëí~åç~êçëk== = pfp=c êä~ö=^_i=pb=nnu=um=píçåâüçäãi=pïéçéåk=qéäw=hqs=u=rrr=rop=nmk=c~ñw=hqs=u=rrr=rop=nnk== bjã~áäw=ëáëkë~äéë]ëáëkëé=fåíéêåéíw=ïïïkëáëkëé=

4 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO September 2007 ICS Supersedes ENV 955-4:1997 English Version Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) - Part 3: Inductively coupled plasma and atomic absorption spectrometry methods (ISO :2007) Analyse chimique des produits réfractaires d'aluminosilicates (méthode alternative à la méthode par fluorescence de rayons X) - Partie 3: Méthodes par spectrométrie d'absorption atomique (AAS) et spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) (ISO :2007) Chemische Analyse feuerfester Erzeugnisse aus Alumosilicat (Alternative zum Röntgenfluoreszenzverfahren) - Teil 3: Verfahren mit induktiv gekoppeltem Plasma und Atomabsorptionspektrometrie (ISO :2007) This European Standard was approved by CEN on 13 September CEN members are bound to comply 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 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 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 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, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO :2007: E

5 Contents Page Foreword... vi 1 Scope Normative references Determination of residual silica in solution by ICP/AES Determination of iron(iii) oxide by ICP/AES Determination of titanium(iv) oxide by ICP/AES Determination of manganese(ii) oxide by ICP/AES Determination of calcium oxide by ICP/AES Determination of magnesium oxide by ICP/AES Determination of sodium oxide by ICP/AES Determination of potassium oxide by ICP/AES Determination of chromium(iii) oxide by ICP/AES Determination of zirconium oxide by ICP/AES Determination of phosphorus(v) oxide by ICP/AES Determination of calcium by AAS Determination of magnesium oxide by AAS Determination of sodium oxide by AAS Determination of potassium oxide by AAS Determination of manganese oxide by AAS Determination of chromium(iii) oxide by AAS Test report v

6 Foreword The text of ISO :2007 has been prepared by Technical Committee ISO/TC 33 "Refractories of the International Organization for Standardization (ISO) and has been taken over as EN ISO :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 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 This document supersedes ENV 955-4:1997. According to the CEN/CENELEC 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, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO :2007 has been approved by CEN as EN ISO :2007 without any modifications. vi

7 Chemical 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 ISO 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) oxide (SiO 2 ) aluminium oxide (Al 2 O 3 ) iron(iii) oxide (total iron oxide calculated as Fe 2 O 3 ) titanium(iv) oxide (TiO 2 ) manganese(ii) oxide (MnO) calcium oxide (CaO) magnesium oxide (MgO) sodium oxide (Na 2 O) potassium oxide (K 2 O) chromium(iii) oxide (Cr 2 O 3 ) zirconium oxide (ZrO 2 ) phosphorous(v) oxide (P 2 O 5 ) This part of ISO 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. 1

8 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 references, the latest edition of the referenced document (including any amendments) applies. ISO :2007, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and gravimetric silica ISO :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 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 (S 1) is determined using ICP/AES. 3.2 Reagents Prepare the reagents specified in ISO and ISO and the following Aluminium oxide solution, Al 2 O 3 5 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 steam bath in order to dissolve the metal. After cooling, dilute to 1 l in a volumetric flask with water 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 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 Matrix solution 2 or 2. Carry out the procedure given in or of ISO :2007 without the sample, but omit heating the fusion mixture or anhydrous sodium carbonate. The solution equivalent to stock solution (S1) or (S 1) is referred to as matrix solution 2 or 2, as applicable Series 2 solution 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, respectively, 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 instrument used. 2

9 Calibration solution Series 2 Table 1 Example of Series 2 solution for calibration Matrix solution 1 Matrix solution 2 or 2 Dilute standard silicon(iv) oxide solution Concentration of solution No. ml ml ml SiO 2 mg/100 ml , , , , ,0 3.3 Procedure Determine the silicon(iv) oxide remaining in solution (S1) or (S 1) ( or in ISO :2007) as follows. Transfer 10 ml of stock solution (S1) or (S 1) to a 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) or (S1 d). Spray a portion of diluted stock solution (S1d) or (S1 d) into the argon plasma flame of the inductively coupled plasma/atomic emission (ICP/AE) spectrometer, and measure the emission intensity 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 (B 1). The diluted blank solution equivalent to diluted stock solution (S1d) or (S1 d) is referred to as diluted blank solution (B1d) or (B1 d). 3.5 Plotting the calibration graph Using 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 carried 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, w SiO2, 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 using the equation: w SiO2 500 m1 m2 m3 m (1) m 3

10 where m is the mass, in g, of the test portion ( or in ISO :2007); m 1, m 2 are the mass, in g, differences in or in ISO :2007; m 3 is the mass, in g, of silicon(iv) oxide in diluted stock solution (S1d or S 1d) as described in 3.3. m 4 is the mass, in g, of silicon(iv) oxide in diluted blank solution (B1d or B 1d) as described in 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 S 1, obtained from or of ISO : Reagents Any of the reagents described in 4.1, 4.2 and 4.3 of ISO :2007 and the following are required Aluminium oxide solution, Al 2 O 3 2 mg/ml. Dilute aluminium oxide solution (10 mg/ml) with water to a concentration of one-fifth Mixed standard solution 2, Fe 2 O 3 0,04 mg/ml, TiO 2 0,04 mg/ml, MnO 0,01 mg/ml, Cr 2 O 3 0,01 mg/ml, ZrO 2 0,01 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 ml volumetric flask and dilute to the mark with water Matrix solution 2 or 2. See Series 3 solutions for calibration. Transfer appropriate aliquot 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 mark 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. 4

11 Solution for calibration Matrix solution 2 or 2 Table 2 Example of Series 3 solution for calibration (mass fraction of aluminium oxide is 30 %) Internal standard solution Aluminium oxide solution Mixed standard solution 2 Concentration of solution No. ml ml ml ml mg/100 ml Fe 2 O 3 TiO 2 MnO Cr 2 O 3 ZrO ,00 0,00 0,00 0,00 0, ,04 0,04 0,01 0,01 0, ,08 0,08 0,02 0,02 0, ,12 0,12 0,03 0,03 0, ,16 0,16 0,04 0,04 0, ,20 0,20 0,05 0,05 0, ,40 0,40 0,10 0,10 0, ,60 0,60 0,20 0,20 0, ,80 0,80 0,30 0,30 0, Procedure Transfer a 10 ml aliquot portion of stock solution (S1) or (S 1), as prepared in or of ISO :2007, into a 100 ml volumetric flask. Add 5 ml of internal standard solution (Sc 0,1 mg/ml, Y 0,1 mg/ml), and dilute to the mark with water. This solution is designated as stock solution (S1 dscy) or (S1 dscy). Spray a portion of stock solution (S1dScY) or (S1 dscy) into the argon plasma flame of an ICP/AE spectrometer, and measure the iron emission intensity at the appropriate wavelength, for example, 259,94 nm. 4.4 Blank test Transfer a 10 ml aliquot portion of blank solution (B1) or (B 1), ( or in ISO :2007) and carry out the procedure given in 4.3. The solution corresponding to stock solution (B1) or (B 1) is designated as blank solution (B1dScY) or (B 1dScY). 4.5 Plotting the calibration graph Use Series 3 solutions for calibration. Carry out the procedure described in 4.3 and plot the relation between the emission intensity and the mass of iron(iii) oxide. Prepare the calibration graph by adjusting the curve so that it passes through the point of origin. 4.6 Calculation Calculate the mass fraction of iron(iii) oxide, w Fe2 O 3, as a percentage, using the following equation, with iron(iii) oxide that is derived from the emission intensity in 4.3 and 4.4, and the calibration in 4.5. w Fe2O3 m1 m2 m (2) 10 5