1、BS EN ISO21079-1:2008ICS 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 1: Apparat
2、us, reagents anddissolution (ISO 21079-1:2008)This British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 30 April2009 BSI 2009ISBN 978 0 580 58570 8Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 21079-1:2008National forewordThis Britis
3、h Standard is the UK implementation of EN ISO21079-1:2008.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 pu
4、rport 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 EUROPENNEEUROPISCHE NORMEN ISO 21079-1April 2008ICS 81.080; 71.040.40English VersionChe
5、mical analysis of refractories containing alumina, zirconiaand silica - Refractories containing 5 percent to 45 percent ofZrO2 (alternative to the X-ray fluorescence method) - Part 1:Apparatus, reagents and dissolution (ISO 21079-1:2008)Analyse chimique des matriaux rfractaires contenant delalumine,
6、 de la zircone et de la silice - Matriauxrfractaires contenant de 5 % 45 % de ZrO2 (mthodealternative 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 feuerfeste
7、n Erzeugnissen -Feuerfeste Erzeugnisse mit einem Massenanteil an ZrO2von 5% bis 45% (Alternative zumRntgenfluoreszenzverfahren) - Teil 1: Gerte, Reagenzienund 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
8、 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 application to the CEN Management Centre or to any CEN
9、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 the same status as theofficial versions.CEN membe
10、rs 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, Swi
11、tzerland 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 reservedworldwide for CEN national Members.Ref. No. EN
12、 ISO 21079-1:2008: EBS EN ISO 21079-1:2008EN 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 and materials” the secretariat of which is held
13、 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 October 2008. Attention is drawn to the possibility th
14、at 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 organizations of the following countries are bound t
15、o 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, Switz
16、erland 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. BS EN ISO 21079-1:2008ISO 21079-1:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Term
17、s 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 Determination of loss on ignition 5 9 Decomposition of the sample and preparation of solutions used in the analysis 5 9.1 General decomposition techniqu
18、es 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 of test results 10 12 Test report . 11 Annex A (informative) References for stock solutions and blank solutions in this part of ISO 21079. 1
19、2 Bibliography . 13 BS EN ISO 21079-1:2008ISO 21079-1:2008(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
20、 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 committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO
21、 collaborates closely with the 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 Internation
22、al Standards. Draft International 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 elem
23、ents 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 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
24、 refractories containing alumina, 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
25、plasma emission spectrometry (ICP-AES) BS EN ISO 21079-1:2008INTERNATIONAL STANDARD ISO 21079-1:2008(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) Pa
26、rt 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 coupled plasma atomic emi
27、ssion (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 to 2 SiO20,1 to 45 Na2O 0
28、,01 to 3 Al2O31 to 80 K2O 0,01 to 1 Fe2O30,01 to 2 Cr2O30,01 to 3 TiO20,01 to 5 ZrO25 to 45 CaO 0,01 to 2 HfO20,01 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 21079 gives alternatives to the X-
29、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 referenced document (including a
30、ny 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 BS EN ISO 21079-1:2008ISO 21079-1:2008(E) 2 ISO 2008 All rights rese
31、rved3 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 given in ISO 26845. 5 Reagents 5.1 General Prepare the following reagents, and those given in ISO 26845, as necessary. During
32、 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 the requirements of ISO 6353-1, ISO 6353-2 and ISO 6353-3, as appropriate. 5.2 Standard solutions specific to ISO 21079 Traceabl
33、e standard solutions may be used in place of the following. 5.2.1 Aluminium oxide standard solution, Al2O31 mg/ml. Wash the surface of a sufficient amount of aluminium metal (purity of more than 99,9 % by mass) with hydrochloric acid (1+4) to dissolve the oxidized layer. Then wash with water, ethano
34、l 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 hydrochloric 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 st
35、andard 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, 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(II
36、I) oxide standard solution, Cr2O31 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, diluting to 1 000 ml in a volumetric flask. 5.2.4 Diluted chromium(III) oxide standard solution, Cr2O30,025 mg/ml. Dilute 25 ml of
37、 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-cyclohexanediamine-N,N,N,N-tetraacetic acid monohydrate) standard solution, 0,02 mol/l. Add 16 ml of sodium hydroxide solution (100 g/l) and 15
38、0 ml of water to 7,30 g of CyDTA, and dissolve by heating. After cooling, dilute to 1 000 ml with water. BS EN ISO 21079-1:2008ISO 21079-1:2008(E) ISO 2008 All rights reserved 35.2.6 EDTA standard solution, 5 g/l. Dissolve 5 g of EDTANa2(ethylenediamine-tetraacetic acid disodium salt, dihydrate) in
39、water and dilute to 1 000 ml in a volumetric flask. Store in a plastics bottle. 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 screen
40、ed calcein indicator and titrate with the EDTA solution (5 g/l), from a fluorescent 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 ammon
41、ia solution (concentrated), and dilute to about 200 ml. Add about 0,04 g of methylthymol blue complexone indicator and titrate with the EDTA solution (5 g/l). 5.2.7 Hafnium oxide standard solution, HfO21 mg/ml. Transfer 1,5 g of hafnium oxide (of a purity more than 99,9 % by mass) into a 20 ml plati
42、num crucible, ignite at 1 050 C 25 C for 1 h and cool in a desiccator. Weigh 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 co
43、oling, add 55 ml of sulfuric acid (1+9) and heat until dissolved on a steam bath. After cooling, dilute to 500 ml in a flask with water. 5.2.8 Iron(III) oxide standard solution, Fe2O31mg/ml. Wash the surface of a sufficient amount of iron metal (purity greater than 99,9 %) with hydrochloric acid (1+
44、4). Then dissolve the oxidized layer, and wash with water, ethanol and diethyl 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 co
45、oling, dilute to 1 000 ml in a volumetric flask with water. 5.2.9 Diluted iron(III) oxide standard solution, Fe2O30,04 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.
46、 5.2.10 Magnesium oxide standard solution, MgO 1 mg/ml. Wash the surface of 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. W
47、eigh 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 standard s
48、olution, K2O 1 mg/ml. Transfer 1 g to 1,5 g of potassium chloride into a platinum crucible (e.g. 30 ml) and ignite at 600 C 25 C for approximately 60 min. Allow the crucible and contents to cool in a desiccator. Weigh 0,791 4 g of this and transfer to a 200 ml beaker. Dissolve in 100 ml of water, tr
49、ansfer to a 500 ml volumetric flask, and dilute to the mark with water. BS EN ISO 21079-1:2008ISO 21079-1:2008(E) 4 ISO 2008 All rights reserved5.2.12 Silicon(IV) oxide standard solution, SiO21 mg/ml. Weigh 0,7 g to 1,0 g of silicon(IV) oxide (purity, greater that 99,9 % by mass) in a platinum crucible (e.g. 30 ml) and heat for 30 min at 1 150 C 50 C. Cool in a desiccator and then weigh 0,500 0 g of this silicon(IV) oxide into a platinum crucible (e.g. 30 ml). Fuse the silicon(IV) oxide with 3,0 g of anhydrou
