EN ISO 10058-1-2008 en Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method) - Part 1 Apparatus reagents dissolution and de.pdf

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1、BS EN ISO10058-1:2008ICS 73.080; 81.080NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDChemical analysisof magnesite anddolomite refractoryproducts (alternativeto the X-rayfluorescence method)Part 1: Apparatus, reagents,dissolution and determination ofgravimetri

2、c silica (ISO 10058-1:2008)This British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 January2009 BSI 2009ISBN 978 0 580 57833 5Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 10058-1:2008National forewordThis British Standard is the

3、 UK implementation of EN ISO10058-1:2008. It partially supersedes BS EN ISO 10058:1996.Together with BS EN ISO 10058-2 and BS EN ISO 10058-3, itsupersedes BS EN ISO 10058:1996 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee RPI/1, Refractory products an

4、d materials.A list of organizations represented on this committee 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 immu

5、nityfrom legal obligations.EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 10058-1December 2008ICS 73.080 Supersedes EN ISO 10058:1996 English VersionChemical analysis of magnesite and dolomite refractoryproducts (alternative to the X-ray fluorescence method) - Part 1:Apparatus, reagents, diss

6、olution and determination ofgravimetric silica (ISO 10058-1:2008)Analyse chimique des produits de magnsie et de dolomie(mthode alternative la mthode par fluorescence derayons X) - Partie 1: Appareillage, ractifs, mise en solutionet dtermination de la teneur en silice par gravimtrie (ISO10058-1:2008)

7、Chemische Analyse von feuerfesten Erzeugnissen ausMagnesit und Dolomit (Alternative zurRntgenfluoreszenzanalyse) - Teil 1: Gerte, Reagenzien,Aufschluss und gravimetrische Bestimmung vonSilicium(IV)-oxid (ISO 10058-1:2008)This European Standard was approved by CEN on 1 November 2008.CEN members are b

8、ound 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 application to the C

9、EN 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 the same statu

10、s 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, Portugal,Romania, Slo

11、vakia, 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 reservedworldwide f

12、or CEN national Members.Ref. No. EN ISO 10058-1:2008: EBS EN ISO 10058-1:2008EN ISO 10058-1:2008 (E) 3 Foreword This document (EN ISO 10058-1:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration with Technical Committee CEN/TC 187 “Refractory products and material

13、s” 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 June 2009, and conflicting national standards shall be withdrawn at the latest by June 2009. Attention i

14、s 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. This document supersedes EN ISO 10058:1996. According to the CEN/CENELEC Internal Regulations, th

15、e 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, No

16、rway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 10058-1:2008 has been approved by CEN as a EN ISO 10058-1:2008 without any modification. BS EN ISO 10058-1:2008ISO 10058-1:2008(E) ISO 2008 All rights reserved i

17、iiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Terms and definitions .2 4 Apparatus.2 5 Reagents.2 6 Sample preparation .6 7 Determination of loss on ignition (gravimetric) .6 8 Decomposition of the sample and preparation of solutions used in the analysis.6 8.1 General decomposition

18、techniques 6 8.2 Dissolution methods by fusion6 8.3 Dissolution methods by hydrofluoric acid attack8 9 Calculation and expression of test results.10 10 Examination and adoption of test results.10 11 Test report11 Annex A (informative) References for stock solutions and blank solutions in ISO 10058-1

19、:2008 .12 BS EN ISO 10058-1:2008ISO 10058-1:2008(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 out throu

20、gh 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 collabora

21、tes 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 International Standar

22、ds. 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 elements of th

23、is document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 10058-1 was prepared by Technical Committee ISO/TC 33, Refractories. This first edition of ISO 10058-1, together with ISO 10058-2 and ISO 10058-3, cancels and replace

24、s ISO 10058:1992 which has been technically revised to include the increasing use of flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods as well some improvements in the wet chemical analyses procedures developed in Japan. IS

25、O 10058 consists of the following parts, under the general title Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method): Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica Part 2: Wet chemical analysis Part 3: Flam

26、e atomic absorption spectrophotometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) BS EN ISO 10058-1:2008INTERNATIONAL STANDARD ISO 10058-1:2008(E) ISO 2008 All rights reserved 1Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray

27、fluorescence method) Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica 1 Scope This part of ISO 10058 specifies apparatus, reagents, dissolution and gravimetric silica analysis for the chemical analysis of magnesite and dolomite refractory products and raw materials. T

28、his part of ISO 10058 is applicable to the ranges of determination given in Table 1. ISO 10058 specifies procedures for the chemical analysis of magnesite and dolomite refractory products and raw materials within the ranges of determination given in Table 1. Table 1 Range of determination (percentag

29、e by mass) Component Range Component Range SiO20,1 to 10 MgO 30 to 99,9 Al2O30,05 to 10 Na2O 0,01 to 1 Fe2O30,01 to 10 K2O 0,01 to 1 TiO20,01 to 1 Cr2O30,01 to 3 MnO 0,01 to 1 ZrO20,01 to 1 CaO 0,01 to 60 P2O50,01 to 5 LOI 0,01 to 60 NOTE These values are after the loss on ignition (LOI) has been ta

30、ken into account. 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 6353

31、-1, Reagents for chemical analysis Part 1: General test methods ISO 6353-2, Reagents for chemical analysis Part 2: Specifications First series ISO 6353-3, Reagents for chemical analysis Part 3: Specifications Second series ISO 26845:2008, Chemical analysis of refractories General requirements for we

32、t chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods BS EN ISO 10058-1:2008ISO 10058-1:2008(E) 2 ISO 2008 All rights reserved3 Terms and definitions For the purposes of this document, the terms and definitions given i

33、n ISO 26845 apply. 4 Apparatus Normal laboratory apparatus and other apparatus as defined in ISO 26845. 5 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. Reagents shall conform to the requ

34、irements of ISO 6353-1, ISO 6353-2 and ISO 6353-3 as appropriate. Specific requirements for reagents are given in the appropriate clause. Use reagents that are defined in ISO 26845 and the following. 5.1 Standard volumetric solutions. 5.1.1 Standard volumetric CyDTA solution, c(CyDTA) = 0,01 mol/l.

35、Add 8 ml of sodium hydroxide solution (100 g/l) and approximately 150 ml of water to 3,65 g of trans-1,2-cyclohexanediamine -N,N,N,N -tetraacetic acid monohydrate (CyDTA), and dissolve by heating. After cooling, dilute to 1 000 ml with water; approximately 25 ml of water are required. Determine the

36、exact strength of this solution by titration against the standard volumetric zinc solution, c(Zn) = 0,01 mol/l. 5.1.2 Standard volumetric zinc solution, c(Zn) = 0,01 mol/l. Wash the surface of the zinc (purity greater than 99,9 % by mass) with hydrochloric acid (1+3) and dissolve the oxidized layer;

37、 subsequently, wash with water, ethanol and diethyl ether in succession, then dry in a desiccator. Weigh 0,65 g (recorded to the nearest 0,000 1 g) of zinc and transfer it to a 300 ml beaker. Cover with a watch glass. Add 20 ml of water and 5 ml of nitric acid carefully, and heat to dissolve on a st

38、eam bath. After cooling, dilute to 1 000 ml in a volumetric flask with water. Calculate the factor, F, of this zinc solution using Equation (1). 0,653 8 100mAF = (1) where m is the mass of the weighed zinc, in grams (g); A is the purity of the zinc, as a percentage by mass (%). 5.1.3 Standard volume

39、tric EDTA solution, c(EDTA) = 0,02 mol/l. Dissolve 7,5 g of EDTA2Na (ethylenediamine-tetraacetic acid disodium salt dihydrate) in 1 l of water. Store in a plastic bottle. BS EN ISO 10058-1:2008ISO 10058-1:2008(E) ISO 2008 All rights reserved 3Determine the factor, F, of the 0,02 mol/l standard volum

40、etric EDTA solution as follows. Transfer 50 ml of 0,01 mol/l zinc solution, obtained in 5.1.2, to a 300 ml beaker and add 50 ml of water. Drop in sodium hydroxide solution (100 g/l) of up to pH 6 to pH 8 and add 2 ml of buffer solution (pH 10) and, while stirring, add 3 to 4 drops of Eriochrome Blac

41、k T solution as an indicator and titrate with 0,02 mol/l standard volumetric EDTA solution. Observe and record the end point, which is when the reddish purple colour of the solution is altered to blue. Calculate the factor, F, of the 0,02 mol/l standard volumetric EDTA solution using Equation (2). 5

42、02fFV=(2) where f is the factor of 0,01 mol/l standard volumetric zinc solution; V is the volume of 0,02 mol/l standard volumetric EDTA solution, in millilitres (ml). 5.2 Standard solutions. 5.2.1 Standard aluminium oxide solution, Al2O31 mg/ml. Wash the surface of a sufficient amount of aluminium m

43、etal (approximately 0,6 g to 0,7 g), 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 it to a 250 ml beaker. Cover the bea

44、ker with a watch glass, add 20 ml hydrochloric acid (1+1), and heat to dissolve. After cooling, dilute to 1 000 ml with water in a volumetric flask. 5.2.2 Standard calcium oxide solution, CaO 1 mg/ml. Dissolve 1,785 g of pure calcium carbonate that has been previously dried at 150 C for 2 h, in a sl

45、ight excess of diluted 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 with water in a volumetric flask. 5.2.3 Standard chromium(III) oxide solution, Cr2O3 1 mg/ml. Dry between 2 g to 3 g of potassium dichromate at 110

46、 C for at least 2 h. Weigh 1,935 5 g of this and dissolve in water. Dilute to 1 000 ml with water in a volumetric flask. 5.2.4 Dilute standard chromium(III) oxide solution, Cr2O30,025 mg/ml. Pipette 25 ml of the standard chromic oxide solution (1 mg/ml) to a 1 000 ml volumetric flask and dilute to t

47、he mark with water. Prepare this solution freshly when required. 5.2.5 Standard iron(III) oxide solution, Fe2O31 mg/ml. Wash the surface of a sufficient amount of iron metal (purity greater than 99,9 % by mass) with hydrochloric acid (1+4). Then dissolve the oxidized layer, wash with water, ethanol,

48、 and diethyl ether in succession. Dry in a desiccator. Weigh 0,699 4 g of this, transfer to a beaker (200 ml) and cover with a watch glass. Add 40 ml of hydrochloric acid (1+1) and heat on a steam bath until dissolved. After cooling, dilute to 1 000 ml with water in a volumetric flask. 5.2.6 Dilute

49、standard iron(III) oxide solution, Fe2O3 0,2 mg/ml. Pipette 200 ml of the standard iron(III) oxide solution (Fe2O31 mg/ml) into a 1 000 ml volumetric flask and dilute to the mark with water. Prepare this solution freshly when required. BS EN ISO 10058-1:2008ISO 10058-1:2008(E) 4 ISO 2008 All rights reserved5.2.7 Dilute standard iron(III) oxide solution, Fe2O3 0,04 mg/ml. Pipette 40 ml of the standard iron(III) oxide solution (Fe2O31 mg/ml) into a 1 000 ml volumetric flask and dilute to the mark with water. Prepare