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1、BS EN ISO 21079-1:2008 ICS 81.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Chemical analysis of refractories containing alumina, zirconia and silica Refractories containing 5 percent to 45 percent of ZrO2 (alternative to the X-ray fluorescence method) P
2、art 1: Apparatus, reagents and dissolution (ISO 21079-1:2008) Licensed CopyChinese University of Hong Kong, 13/06/2009 08:03, Uncontrolled Copy, (c) BSI This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2009 BSI 2009 ISBN 978 0 580 585
3、70 8 Amendments/corrigenda issued since publication DateComments BS EN ISO 21079-1:2008 National foreword This British Standard is the UK implementation of EN ISO 21079-1:2008. The UK participation in its preparation was entrusted to Technical Committee RPI/1, Refractory products and materials. A li
4、st of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from le
5、gal obligations. Licensed CopyChinese University of Hong Kong, 13/06/2009 08:03, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21079-1 April 2008 ICS 81.080; 71.040.40 English Version Chemical analysis of refractories containing alumina, zirconia and silica - Re
6、fractories containing 5 percent to 45 percent of ZrO2 (alternative to the X-ray fluorescence method) - Part 1: Apparatus, reagents and dissolution (ISO 21079-1:2008) Analyse chimique des matriaux rfractaires contenant de lalumine, de la zircone et de la silice - Matriaux rfractaires contenant de 5 %
7、 45 % de ZrO2 (mthode alternative la mthode par fluorescence de rayons X) - Partie 1: Appareillage, ractifs et dissolution (ISO 21079- 1:2008) Chemische Analyse von aluminiumoxid-, zirkoniumoxid- und silicium(IV)-oxidhaltigen feuerfesten Erzeugnissen - Feuerfeste Erzeugnisse mit einem Massenanteil a
8、n ZrO2 von 5% bis 45% (Alternative zum Rntgenfluoreszenzverfahren) - Teil 1: Gerte, Reagenzien und Aufschluss (ISO 21079-1:2008) This European Standard was approved by CEN on 12 April 2008. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for g
9、iving 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
10、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, Bel
11、gium, 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 FO
12、R STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2008 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 21079-1:2008: E Licensed CopyChinese Uni
13、versity of Hong Kong, 13/06/2009 08:03, Uncontrolled Copy, (c) BSI BS EN ISO 21079-1:2008 EN ISO 21079-1:2008 (E) 3 Foreword This document (EN ISO 21079-1:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration with Technical Committee CEN/TC 187 “Refractory products
14、 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 Octobe
15、r 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 orga
16、nizations 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, R
17、omania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 21079-1:2008 has been approved by CEN as a EN ISO 21079-1:2008 without any modification. Licensed CopyChinese University of Hong Kong, 13/06/2009 08:03, Uncontrolled Copy, (c) BSI BS EN
18、ISO 21079-1:2008 ISO 21079-1:2008(E) ISO 2008 All rights reserved iii Contents Page Foreword iv 1 Scope . 1 2 Normative references. 1 3 Terms and definitions. 2 4 Apparatus 2 5 Reagents 2 5.1 General. 2 5.2 Standard solutions specific to ISO 21079 2 6 Sampling 4 7 General procedures 5 8 Determinatio
19、n of loss on ignition 5 9 Decomposition of the sample and preparation of solutions used in the analysis 5 9.1 General decomposition techniques 5 9.2 Dissolution methods by fusion. 5 9.3 Dissolution methods by hydrofluoric acid attack . 8 10 Expression of test results 10 11 Examination and adoption o
20、f test results 10 12 Test report . 11 Annex A (informative) References for stock solutions and blank solutions in this part of ISO 21079. 12 Bibliography. 13 Licensed CopyChinese University of Hong Kong, 13/06/2009 08:03, Uncontrolled Copy, (c) BSI BS EN ISO 21079-1:2008 ISO 21079-1:2008(E) iv ISO 2
21、008 All rights reserved Foreword 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
22、 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 the International Electrotechnical Commiss
23、ion (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 International Standards adopted by the technical
24、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 the subject of patent rights. ISO shall
25、not be held responsible for identifying any or all such patent rights. ISO 21079-1 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 co
26、ntaining 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) Licensed CopyChinese Universi
27、ty of Hong Kong, 13/06/2009 08:03, Uncontrolled Copy, (c) BSI BS EN ISO 21079-1:2008 INTERNATIONAL STANDARD ISO 21079-1:2008(E) ISO 2008 All rights reserved 1 Chemical analysis of refractories containing alumina, zirconia and silica Refractories containing 5 % to 45 % of ZrO2 (alternative to the X-r
28、ay fluorescence method) Part 1: Apparatus, reagents and dissolution 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, inductively
29、 coupled plasma atomic emission (ICP-AE) spectrometry and flame atomic absorption (FAA) spectrometry. It covers apparatus, reagents and dissolution methods. The range of determination is given in Table 1. Table 1 Range of determination (% by mass) Component Range Component Range LOI 1 to 40 MgO 0,01
30、 to 2 SiO2 0,1 to 45 Na2O 0,01 to 3 Al2O3 1 to 80 K2O 0,01 to 1 Fe2O3 0,01 to 2 Cr2O3 0,01 to 3 TiO2 0,01 to 5 ZrO2 5 to 45 CaO 0,01 to 2 HfO2 0,01 to 2 NOTE The values other than LOI are on an ignited basis. This part of ISO 21079 is not applicable to MgO-based refractories. NOTE This part of ISO 2
31、1079 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 edition of the
32、 referenced document (including any amendments) applies. ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods Licensed CopyChinese University of
33、Hong Kong, 13/06/2009 08:03, Uncontrolled Copy, (c) BSI BS EN ISO 21079-1:2008 ISO 21079-1:2008(E) 2 ISO 2008 All rights reserved 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 26845 apply. 4 Apparatus Ordinary laboratory apparatus and the apparatus
34、 given in ISO 26845. 5 Reagents 5.1 General Prepare the following reagents, and those given in ISO 26845, as necessary. During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. Reagents should conform to th
35、e requirements of ISO 6353-1, ISO 6353-2 and ISO 6353-3, as appropriate. 5.2 Standard solutions specific to ISO 21079 Traceable standard solutions may be used in place of the following. 5.2.1 Aluminium oxide standard solution, Al2O3 1 mg/ml. Wash the surface of a sufficient amount of aluminium metal
36、 (purity of more than 99,9 % by mass) with hydrochloric acid (1+4) to dissolve the oxidized layer. Then wash with water, ethanol and diethyl ether in succession, and dry in a desiccator. Weigh 0,529 2 g of aluminium and transfer into a 250 ml beaker. Cover with a watch glass, add 20 ml of hydrochlor
37、ic acid (1+1), and heat to dissolve. After cooling, dilute to 1 000 ml in a volumetric flask with water. 5.2.2 Calcium oxide standard solution, CaO 1 mg/ml. Dissolve 1,785 g of pure calcium carbonate, previously dried at 150 C, in a slight excess of dilute hydrochloric acid (1+4) in a 250 ml beaker,
38、 covered with a watch glass. Boil to expel carbon dioxide, cool and dilute to 1 000 ml in a volumetric flask. 5.2.3 Chromium(III) oxide standard solution, Cr2O3 1 mg/ml. Dry about 2 g to 3 g of potassium dichromate, K2Cr2O7, at 110 C. for at least 2 h. Weigh 1,935 g of this and dissolve in water, di
39、luting to 1 000 ml in a volumetric flask. 5.2.4 Diluted chromium(III) oxide standard solution, Cr2O3 0,025 mg/ml. Dilute 25 ml of the chromium(III) oxide standard solution (1 mg/ml), to 1 000 ml in a volumetric flask. Prepare this solution freshly when required. 5.2.5 CyDTA (trans-1,2-cyclohexanedia
40、mine-N,N,N,N-tetraacetic acid monohydrate) standard solution, 0,02 mol/l. Add 16 ml of sodium hydroxide solution (100 g/l) and 150 ml of water to 7,30 g of CyDTA, and dissolve by heating. After cooling, dilute to 1 000 ml with water. Licensed CopyChinese University of Hong Kong, 13/06/2009 08:03, Un
41、controlled Copy, (c) BSI BS EN ISO 21079-1:2008 ISO 21079-1:2008(E) ISO 2008 All rights reserved 3 5.2.6 EDTA standard solution, 5 g/l. Dissolve 5 g of EDTANa2 (ethylenediamine-tetraacetic acid disodium salt, dihydrate) in water and dilute to 1 000 ml in a volumetric flask. Store in a plastics bottl
42、e. Standardize against calcium as follows. Pipette 25 ml of standard calcium solution (1 mg/ml) into a 500 ml conical flask, add 10 ml of potassium hydroxide solution, and dilute to about 200 ml. Add about 0,015 g of screened calcein indicator and titrate with the EDTA solution (5 g/l), from a fluor
43、escent green colour to pink. Standardize against magnesium as follows. Pipette 25 ml of standard magnesium solution (1 mg/ml), into a 500 ml conical flask. Add 20 drops of hydrochloric acid (concentrated) and 20 ml of ammonia solution (concentrated), and dilute to about 200 ml. Add about 0,04 g of m
44、ethylthymol blue complexone indicator and titrate with the EDTA solution (5 g/l). 5.2.7 Hafnium oxide standard solution, HfO2 1 mg/ml. Transfer 1,5 g of hafnium oxide (of a purity more than 99,9 % by mass) into a 20 ml platinum crucible, ignite at 1 050 C 25 C for 1 h and cool in a desiccator. Weigh
45、 0,500 0 g of the ignited residue into a 75 ml platinum crucible. After adding 3,0 g of anhydrous sodium carbonate, add 2,0 g of boric acid and mix.Then carry out melting at 1 050 25 C in an electric muffle furnace. After cooling, add 55 ml of sulfuric acid (1+9) and heat until dissolved on a steam
46、bath. After cooling, dilute to 500 ml in a flask with water. 5.2.8 Iron(III) oxide standard solution, Fe2O3 1mg/ml. Wash the surface of a sufficient amount of iron metal (purity greater than 99,9 %) with hydrochloric acid (1+4). Then dissolve the oxidized layer, and wash with water, ethanol and diet
47、hyl ether in succession. Then dry in a desiccator. Weigh 0,699 4 g of this, transfer to a beaker (200 ml), and cover with a watch glass. Add 30 ml of hydrochloric acid (1+1), and heat on a steam bath until dissolved. After cooling, dilute to 1 000 ml in a volumetric flask with water. 5.2.9 Diluted i
48、ron(III) oxide standard solution, Fe2O3 0,04 mg/ml. Transfer 40 ml of the iron(III) oxide (1 mg/ml) standard solution to a 1 000 ml volumetric flask and dilute to the mark with water. Prepare this solution freshly as required. 5.2.10 Magnesium oxide standard solution, MgO 1 mg/ml. Wash the surface o
49、f a sufficient amount of magnesium metal (purity, more than 99,9 % by mass) with hydrochloric acid (1+1) to dissolve the oxidized layer. Then wash with water, ethanol, and diethyl ether in succession and dry in a desiccator. Weigh 0,301 5 g of the washed magnesium, transfer to a 200 ml beaker and cover with a watch glass. Add 10 ml of hydrochloric acid (1+1), and heat on a steam bath until dissolved. After cooling, transfer to a 500 ml volumetric flask, and dilute to the mark with water. 5.2.11 Potassium oxide