1、BS EN ISO21079-2:2008ICS 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 2: Wet ch
2、emical analysis (ISO21079-2:2008)This British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 30 April2009 BSI 2009ISBN 978 0 580 58571 5Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 21079-2:2008National forewordThis British Standard is
3、 the UK implementation of EN ISO21079-2:2008.The UK participation in its preparation was entrusted to TechnicalCommittee RPI/1, Refractory products and materials.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to incl
4、ude 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 EUROPENNEEUROPISCHE NORMEN ISO 21079-2April 2008ICS 81.080; 71.040.40English VersionChemical analysi
5、s of refractories containing alumina, zirconia,and silica - Refractories containing 5 percent to 45 percent ofZrO2 (alternative to the X-ray fluorescence method) - Part 2:Wet chemical analysis (ISO 21079-2:2008)Analyse chimique des matriaux rfractaires contenant delalumine, de la zircone et de la si
6、lice - Matriauxrfractaires contenant de 5 % 45 % de ZrO2 (mthodealternative la mthode par fluorescence de rayons X) -Partie 2: Mthodes danalyse chimique par voie humide(ISO 21079-2:2008)Chemische Analyse von aluminiumoxid-, zirkoniumoxid-und silicium(IV)-oxidhaltigen feuerfesten Erzeugnissen -Feuerf
7、este Erzeugnisse mit einem Massenanteil an ZrO2von 5 % bis 45 % (Alternative zumRntgenfluoreszenzverfahren) - Teil 2: NasschemischeAnalyse (ISO 21079-2:2008)This European Standard was approved by CEN on 12 April 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which sti
8、pulate 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 application to the CEN Management Centre or to any CEN member.This European Standard e
9、xists 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 standards b
10、odies 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.EUR
11、OPEAN 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 reservedworldwide for CEN national Members.Ref. No. EN ISO 21079-2:2008: EBS EN ISO 2
12、1079-2:2008EN ISO 21079-2:2008 (E) 3 Foreword This document (EN ISO 21079-2:2008) 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 by BSI. This European Standard
13、 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 October 2008. Attention is drawn to the possibility that some of the elements of this
14、 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 implement this European Stand
15、ard: 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 the United Kingdom.
16、Endorsement notice The text of ISO 21079-2:2008 has been approved by CEN as a EN ISO 21079-2:2008 without any modification. BS EN ISO 21079-2:2008ISO 21079-2:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Determination of silicon(IV) oxide.
17、 2 4 Determination of aluminium oxide 4 5 Determination of iron(III) oxide 7 6 Determination of titanium(IV) oxide 8 7 Determination of calcium oxide 11 8 Determination of magnesium oxide 12 9 Determination of sodium oxide by flame photometry 13 10 Determination of potassium oxide by flame photometr
18、y . 14 11 Determination of chromium(III) oxide using diphenylcarbazide 15 12 Determination of zirconium oxide (including hafnium oxide) by mandelic acid (-hydroxybenzeneacetic acid) gravimetric method. 16 13 Calculation and expression of test results 17 14 Test report . 17 Bibliography . 18 BS EN IS
19、O 21079-2:2008ISO 21079-2:2008(E) iv ISO 2008 All rights 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 c
20、ommittees. Each member body interested in a subject 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 t
21、he International Electrotechnical Commission (IEC) 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 Internat
22、ional Standards adopted by the technical committees 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
23、 the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 21079-2 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 alu
24、mina, zirconia, and silica Refractories containing 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 spectrometr
25、y (ICP-AES) BS EN ISO 21079-2:2008INTERNATIONAL STANDARD ISO 21079-2:2008(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 2: Wet chemical analysi
26、s 1 Scope This part of ISO 21079 specifies methods for the chemical analysis of AZS (alumina, zirconia, and silica) refractory products (containing 5 % to 45 % of ZrO2) and raw materials, using traditional (“wet”) methods. This part of ISO 21079 is not applicable to MgO-based refractories. This part
27、 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 this document. For dated references, only the edition cited applies. For undated references, the latest editi
28、on of the referenced document (including any amendments) applies. ISO 10058-2:1), Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis ISO 21079-1:2008, Chemical analysis of refractories containing alumina, zirco
29、nia and silica Refractories containing 5 % to 45 % of ZrO2(alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents and dissolution ISO 21079-3:2008, Chemical analysis of refractories containing alumina, zirconia and silica Refractories containing 5 % to 45 % of ZrO2(alternative to
30、the X-ray fluorescence method) Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) ISO 21587-2:2007, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analys
31、is ISO 26845:2008, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods 1) To be published. BS EN ISO 21079-2:2008ISO 21079-2:2008(E) 2 ISO 2008 All rights
32、reserved3 Determination of silicon(IV) oxide 3.1 General The determination of silicon(IV) oxide is carried out using one of the following methods. a) Combined use of the dehydration or the coagulation and molybdenum blue methods. This method is applied to samples consisting of more than 4 % by mass
33、of silicon(IV) oxide. b) Molybdenum blue method. This method is applied to samples consisting of less than 8 % by mass of silicon(IV) oxide. 3.2 Combined use of dehydration or coagulation and molybdenum blue methods 3.2.1 Principle An aliquot portion of stock solution (S1) or (S1) is treated with am
34、monium molybdate and the silicomolybdate is reduced to yield molybdenum blue, the absorbance of which is measured. The sum of this residual silicon(IV) oxide in solution plus the mass of silicon(IV) oxide (m1 m2) derived in accordance with 9.2.2.3 or 9.2.3.3 of ISO 21079-1:2008 gives the total silic
35、on(IV) oxide content. 3.2.2 Procedure This determination should be commenced with little delay after the stock solution (S1) or (S1) is prepared, as prolonged standing could allow polymerization of silica to occur leading to low results. Transfer a 10,0 ml aliquot portion of stock solution (S1) or (
36、S1) (see Annex A of ISO 21079-1:2008) to a 100 ml plastic beaker, add 2 ml of hydrofluoric acid (1+9), mix with a plastic rod and allow to stand for 10 min. Add 50 ml of boric acid solution, 2 ml of ammonium molybdate solution while swirling at a temperature of about 25 C, and allow to stand for 10
37、min. Add 5 ml of L (+)-tartaric acid solution while swirling and after 1 min add 2 ml of L (+)-ascorbic acid solution while shaking. Transfer a solution to a 100 ml plastics volumetric flask, dilute to the mark with water and allow to stand for 60 min. Measure the absorbance of the solution in a 10
38、mm cell at a wavelength of 650 nm using water as reference. 3.2.3 Plotting the calibration graph Transfer 0 ml, 2 ml, 4 ml, 6 ml, 8 ml and 10 ml aliquot portions of diluted silicon(IV) oxide solution (0 mg to 0,4 mg as silicon(IV) oxide) into six 100 ml plastic beakers and, to each, add 10 ml of bla
39、nk solution (B1) or (B1) (see Annex A of ISO 21079-1:2008). Treat these solutions and measure the absorbance as described in 3.2.2, and plot the absorbances against the amounts of silicon(IV) oxide. Prepare the calibration graph by adjusting the curve so that it passes through the point of origin. 3
40、.2.4 Calculation Calculate the mass fraction of silicon(IV) oxide, w(SiO2), expressed as a percentage, using Equation (1) with the absorbances obtained in 3.2.2 and the calibration graph. ()()()12 sb250010SiO 100mm mmwm+= (1) where m1is the mass from 9.2.2.3 or 9.2.3.3 of ISO 21079-1:2008, in grams;
41、 BS EN ISO 21079-2:2008ISO 21079-2:2008(E) ISO 2008 All rights reserved 3m2is the mass from the blank prepared in accordance with 9.2.2.4 or 9.2.3.4 of ISO 21079-1:2008, in grams; msis the mass of silicon(IV) oxide in the aliquot portion of stock solution (S1) or (S1), in grams; mbis the mass of sil
42、icon(IV) oxide in the aliquot portion of blank solution (B1) or (B1), in grams; m is the mass of the test portion prepared in accordance with ISO 21079-1:2008, in grams. 3.3 Molybdenum blue method 3.3.1 Principle An aliquot portion of the stock solution (S1) is treated with ammonium molybdate and th
43、e silicomolybdate is reduced to yield molybdenum blue, the absorbance of which is measured. 3.3.2 Procedure Transfer the specified volume of stock solution (S1) (see Annex A of ISO 21079-1:2008) to two plastic beakers and add, to each, the specified volume of blank solution (B1) (see Annex A of ISO
44、21079-1:2008). Add 2 ml of hydrofluoric acid (1+9), mix with a plastic rod and allow to stand for 10 min. Then add 50 ml of boric acid solution and dilute to about 80 ml with water. Add 5 ml of ammonium molybdate solution while mixing at a temperature of 20 C to 30 C and allow to stand for 10 min. A
45、dd 20 ml of tartaric acid solution while stirring. After 1 min, add 10 ml of L (+)-ascorbic acid solution while stirring. Transfer each solution to two 200 ml plastics volumetric flasks, dilute to the mark with water and mix. Allow to stand for 60 min and measure the absorbance of the solutions in a
46、 10 mm cell at a wavelength of 650 nm against water. Take the mean value of the two measurements for the calculation of silica content. The volume of the aliquot portions from stock solution (S1) and the blank solution are given in Table 1 depending on the mass fraction of silicon(IV) oxide. Table 1
47、 Aliquot volume of stock solution (S1) and blank solution (B1) Mass fraction of SiO2Volume of stock solution (S1) Volume of blank solution (B1)% ml ml 1 25 5.2.2 Dilute to about 60 ml with water, add 5 ml of L (+)-tartaric acid solution and 2 ml of L (+)-ascorbic acid while mixing. Add 10 ml of 1,10
48、-phenanthroline chloride solution and 10 ml of ammonium acetate solution. Dilute to the mark with water and allow to stand for 30 min. Measure the absorbance of the solution in a 10 mm cell at the wavelength of 510 nm against water. 5.3 Blank test Transfer the same aliquot volume used in 5.2.1 of bl
49、ank solution (B1), (B1), or (B1) (see Annex A of ISO 21079-1:2008) and carry out the procedure in 5.2.2. 5.4 Plotting of calibration graph Transfer 0 ml (as reference), 5 ml, 10 ml and 15 ml aliquot portions of diluted iron(III) oxide standard solution 0,0 mg to 0,75 mg as iron(III) oxide into several 100 ml volumetric flasks. Treat these solutions as described in 5.2.2 and measure the absorbance against the reference solution. Plot the relation between the absorbances and mass of iro
