1、BS EN ISO21079-3:2008ICS 81.080NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDChemical analysis ofrefractories containingalumina, zirconia, andsilica Refractoriescontaining 5 percentto 45 percent of ZrO2(alternative to theX-ray fluorescencemethod)Part 3: Flame
2、atomic absorptionspectrophotometry (FAAS) andinductively coupled plasma emissionspectrometry (ICP -AES) (ISO21079-3:2008)This British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 30 April2009 BSI 2009ISBN 978 0 580 58572 2Amendments/corrigenda issued since
3、 publicationDate CommentsBS EN ISO 21079-3:2008National forewordThis British Standard is the UK implementation of EN ISO21079-3:2008.The UK participation in its preparation was entrusted to TechnicalCommittee RPI/1, Refractory products and materials.A list of organizations represented on this commit
4、tee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARDNORME EUROPENNEEUR
5、OPISCHE NORMEN ISO 21079-3April 2008ICS 81.080; 71.040.40English VersionChemical analysis of refractories containing alumina, zirconia,and silica - Refractories containing 5 percent to 45 percent ofZrO2 (alternative to the X-ray fluorescence method) - Part 3:Flame atomic absorption spectrophotometry
6、 (FAAS) andinductively coupled plasma emission spectrometry (ICP -AES)(ISO 21079-3:2008)Analyse chimique des matriaux rfractaires contenant delalumine, de la zircone et de la silice - Matriauxrfractaires contenant de 5 % 45 % de ZrO2 (mthodealternative la mthode par fluorescence de rayons X) -Partie
7、 3: Mthodes par spectromtrie dabsorptionatomique dans la flamme (FAAS) et spectromtriedmission atomique avec plasma induit par hautefrquence (ICP-AES) (ISO 21079-3:2008)Chemische Analyse von aluminiumoxid-, zirkomiumoxid-und silicium(IV)-oxidhaltigen feuerfesten Erzeugnissen -Feuerfeste Erzeugnisse
8、mit einem Massenanteil an ZrO2von 5 % bis 45 % (Alternative zumRntgenfluoreszenzverfahren) - Teil 3:Flammenatomabsorptionsspektrophotometrie (FAAS) undAtomemissionsspektrometrie mit induktiv gekoppeltemPlasma (ICP-AES) (ISO 21079-3:2008)This European Standard was approved by CEN on 12 April 2008.CEN
9、 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 without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on applic
10、ation 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
11、the 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, Portuga
12、l,Romania, 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 reser
13、vedworldwide for CEN national Members.Ref. No. EN ISO 21079-3:2008: EBS EN ISO 21079-3:2008EN ISO 21079-3:2008 (E) 3 Foreword This document (EN ISO 21079-3:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration with Technical Committee CEN/TC 187 “Refractory product
14、s 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 national standards shall be withdrawn at the latest by Octob
15、er 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/CENELEC Internal Regulations, the national standards org
16、anizations 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,
17、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. BS EN ISO 21079-3:2008ISO 21079-3:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword
18、 iv 1 Scope . 1 2 Normative references . 1 3 Instrumental methods using ICP-AES 1 3.1 Determination of residual silica in solution by ICP-AES 1 3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, calcium oxide, magnesium oxide, chromium(III) oxide and hafniu
19、m oxide using stock solutions (S1), (S1) or (S1) by ICP-AES. 3 3.3 Determination of calcium oxide, magnesium oxide, sodium oxide and potassium oxide using stock solutions (S4) by ICP-AES 7 4 Instrumental methods using Flame Atomic Absorption Spectrometry (FAAS). 8 4.1 Determination of calcium oxide,
20、 magnesium oxide, sodium oxide and potassium oxide using stock solutions (S3) by FAAS . 8 4.2 Determination of chromium(III) oxide by FAAS spectrometry. 10 5 Calculation and expression of test results 12 6 Test report . 12 Bibliography . 13 BS EN ISO 21079-3:2008ISO 21079-3:2008(E) iv ISO 2008 All r
21、ights reservedForeword ISO (the International Organization 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
22、 for which a technical committee has been established 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)
23、on all matters of electrotechnical standardization. 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
24、 are circulated to the member bodies for voting. Publication 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 hel
25、d responsible for identifying any or all such patent rights. ISO 21079-3 was prepared by Technical Committee ISO/TC 33, Refractories. ISO 21079 consists of the following parts, under the general title Chemical analysis of refractories containing alumina, zirconia, and silica Refractories containing
26、5 % to 45 % of ZrO2(alternative to the X-ray fluorescence method): Part 1: Apparatus, reagents and dissolution Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) BS EN ISO 21079-3:2008INTERNATIONAL STA
27、NDARD ISO 21079-3:2008(E) ISO 2008 All rights reserved 1Chemical analysis of refractories containing alumina, zirconia, and silica Refractories containing 5 % to 45 % of ZrO2(alternative to the X-ray fluorescence method) Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively couple
28、d plasma emission spectrometry (ICP-AES) 1 Scope This part of ISO 21079 specifies flame 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
29、% of ZrO2) and raw materials. This part of ISO 21079 is not applicable to MgO-based 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 th
30、is document. For dated references, only the edition cited applies. For undated references, 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 %
31、 of ZrO2(alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents 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 usi
32、ng ICP-AES 3.1 Determination of residual silica in solution by ICP-AES 3.1.1 Principle 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, a
33、s necessary. BS EN ISO 21079-3:2008ISO 21079-3:2008(E) 2 ISO 2008 All rights reserved3.1.2.2 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. 3.1.2.3
34、 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 without 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 Se
35、ries 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. Add 10 ml each of matrix solution 1 or 1 and dilute to the mark with
36、water. Table 1 shows a typical example of the preparation of solutions. An appropriate series of solutions 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 s
37、olution 1 or 1 Diluted silicon(IV) oxide standard solution Concentration of solution Solution No. ml ml 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 21079-1:200
38、8) as follows. Transfer 10 ml of stock solution (S1) or (S1) to a 100 ml volumetric flask, and dilute to 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)
39、into the argon plasma flame of the inductively coupled plasma atomic emission (ICP-AE) spectrometer, and 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-
40、1:2008). Designate the equivalent diluted blank solution to diluted stock solution (S1d) or (S1d) as diluted blank solution (B1d or B1d). BS EN ISO 21079-3:2008ISO 21079-3:2008(E) ISO 2008 All rights reserved 33.1.5 Plotting the calibration graph Using the series 2 solution for calibration, carry ou
41、t 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 new calibration should be carried out using the range of calibration and blank soluti
42、ons for each set of determinations. 3.1.6 Calculation Calculate the mass fraction of silicon(IV) oxide, w(SiO2), expressed 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
43、. ()()()12 sb250010SiO 100mm mmwm+= (1) where m is the mass of the test portion obtained in accordance with 9.2.2.2 or 9.2.3.2 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
44、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 described 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, alum
45、inium 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-AES 3.2.1 Principle The emission intensity of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, calcium oxide
46、, magnesium oxide, chromium(III) oxide and hafnium oxide are measured by the ICP-AE spectrometer for stock solutions (S1), (S1) or (S1). The ICP-AES method is applicable to the components in (S1), (S1) or (S1) as given in Table 2. BS EN ISO 21079-3:2008ISO 21079-3:2008(E) 4 ISO 2008 All rights reser
47、vedTable 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 Cr2O30,01 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(I
48、V) 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 3.2.2.1 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
49、. 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, gradually 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. Weigh 0,127 0 g of this, transfer to a 10
