DIN EN ISO 21587-1-2007 Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) - Part 1 Apparatus reagents dissolution and gravimet.pdf

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1、December 2007DEUTSCHE NORM English price group 10No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 81.080!$JE“1398834www

2、.din.deDDIN EN ISO 21587-1Chemical analysis of aluminosilicate refractory products(alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and gravimetric silica(ISO 21587-1:2007)English version of DIN EN ISO 21587-1:2007-12Chemische Analyse feuerfester Erzeugnisse aus

3、 Alumosilicat(Alternative zum Rntgenfluoreszenzverfahren) Teil 1: Gerte, Reagenzien, Aufschluss und gravimetrische Bestimmung vonSilicium(IV)-oxid (ISO 21587-1:2007)Englische Fassung DIN EN ISO 21587-1:2007-12Together with DIN EN ISO 21587-2:2007-12, supersedes DIN EN 955-2:1995-06;together with DIN

4、 EN ISO 21587-3:2007-12, supersedes DIN V ENV 955-4:1997-07Supersedes: see belowwww.beuth.deDocument comprises 16 pagesDIN EN ISO 21587-1:2007-12 2 National foreword This standard has been published in accordance with a decision taken by Technical Committee CEN/TC 187 “Refractory products and materi

5、als” (Secretariat: BSI, United Kingdom) to adopt, without alteration, International Standard ISO 21587-1:2007 as a European Standard. ISO 21587-1 was prepared by Technical Committee ISO/TC 33 “Refractories”. The responsible German body involved in its preparation was the Normenausschuss Materialprfu

6、ng (Materials Testing Standards Committee), Technical Committee NA 062-02-61 AA Chemische Analyse von oxidischen Roh- und Werkstoffen. The DIN Standards corresponding to the International Standards referred to in clause 2 of the EN are as follows: ISO 21587-2 DIN EN ISO 21587-2 ISO 21587-3 DIN EN IS

7、O 21587-3 ISO 26845 DIN EN ISO 26845 Amendments This standard differs from DIN EN 955-2:1995-06 and DIN V ENV 955-4:1997-07 as follows: a) The standard has been split into three parts. b) The standard has been completely revised taking into account the current chemical analysis and environmental asp

8、ects. Previous editions DIN 51070: 1957-04 DIN 51070-9: 1966-02 DIN 51070-1: 1966-02 DIN 51071: 1957-05 DIN 51070-2: 1966-02 DIN 51077-1: 1972-04 DIN 51070-3: 1966-02 DIN 51077-2: 1972-04 DIN 51070-4: 1966-02 DIN 51077-3: 1972-04 DIN 51070-5: 1966-02 DIN 51081: 1979-07 DIN 51070-6: 1966-02 DIN EN 95

9、5-2: 1995-06 DIN 51070-7: 1966-02 DIN V ENV 955-4: 1997-07 DIN 51070-8: 1966-02 National Annex NA (informative) Bibliography DIN EN ISO 21587-2, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis DIN EN ISO 21587-3, C

10、hemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 3: Inductively coupled plasma and atomic absorption spectrometry methods DIN EN ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, AAS and ICP methods

11、 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21587-1 September 2007 ICS 81.080 Supersedes EN 955-2:1995, ENV 955-4:1997 English Version Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) - Part 1: Apparatus, reagents, dissolution and

12、gravimetric silica (ISO 21587-1:2007) Analyse chimique des produits rfractaires daluminosilicates (mthode alternative la mthode par fluorescence de rayons X) - Partie 1: Appareillage, ractifs, dissolution et teneur en silice par gravimtrie (ISO 21587-1:2007) Chemische Analyse feuerfester Erzeugnisse

13、 aus Alumosilicat (Alternative zum Rntgenfluoreszenz-verfahren) - Teil 1: Gerte, Reagenzien, Aufschluss und gravimetrische Bestimmung von Silicium(IV)-oxid (ISO 21587-1:2007) This European Standard was approved by CEN on 13 September 2007. CEN members are bound to comply with the CEN/CENELEC Interna

14、l Regulations which stipulate the conditions for giving 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

15、. This European Standard exists in three official 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

16、 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, Swit

17、zerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. N

18、o. EN ISO 21587-1:2007: EContents Page 2 EN ISO 21587-1:2007 (E) Foreword .3 1 Scope 4 2 Normative references .5 3 Reagents 5 4 Dissolution and gravimetric silica 9 Foreword The text of ISO 21587-1:2007 has been prepared by Technical Committee ISO/TC 33 “Refractories” of the International Organizati

19、on for Standardization (ISO) and has been taken over as EN ISO 21587-1:2007 by Technical Committee CEN/TC 187 “Refractory products 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 t

20、ext or by endorsement, at the latest by March 2008, and conflicting national standards shall be withdrawn at the latest by March 2008. This document supersedes EN 955-2:1995 and ENV 955-4:1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following c

21、ountries 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, Romania, Slovakia, Slovenia,

22、Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 21587-1:2007 has been approved by CEN as EN ISO 21587-1:2007 without any modifications. 3 EN ISO 21587-1:2007 (E) 1 Scope This part of ISO 21587 specifies reagents, dissolution and gravimetric silica analysis for the c

23、hemical analysis of aluminosilicate refractory products and raw materials. This part of ISO 21587 gives alternatives to the X-ray fluorescence (XRF) method given in ISO 12677:2003, Chemical analysis of refractory products by XRF Fused cast bead method. This part of ISO 21587 should be used in conjun

24、ction with ISO 21587-2 and ISO 21587-3, which give the analytical procedures for the determination of the following: silicon(IV) oxide (SiO2) aluminium oxide (Al2O3) iron(III) oxide (total ir on oxide calculated as Fe2O3) titanium(IV) oxide (TiO2) manganese(II) oxide (MnO) calcium oxide (CaO) magnes

25、ium oxide (MgO) sodium oxide (Na2O) potassium oxide (K2O) chromium(III) oxide (Cr2O3) zirconium oxide (ZrO2) phosphorous(V) oxide (P2O5) 4 EN ISO 21587-1:2007 (E) 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, o

26、nly the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 21587-2, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis ISO 21587-3, Che

27、mical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 3: Inductively coupled plasma and atomic absorption spectrometry methods ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectromet

28、ry and inductively coupled plasma methods 3 Reagents Standard solutions specified in ISO 26845 and the following reagents. 3.1 Standard volumetric solutions 3.1.1 Standard volumetric CyDTA solution, c(CyDTA) = 0,05 mol/l. Dissolve 18 g of 1,2 cyclohexanediamine-N,N,N,N-tetraacetic acid monohydrate (

29、CyDTA) in 500 ml of water by the progressive addition of the minimum amount of potassium hydroxide solution. NOTE Approximately 25 ml is required. Determine the exact strength of this solution by titration against the standard volumetric zinc solution, c(Zn) = 0,05 mol/l. 3.1.2 Standard volumetric C

30、yDTA solution, c(CyDTA) = 0,02 mol/l. Add 16 ml of sodium hydroxide solution (100 g/l) and approximately 150 ml of water to 7,30 g of 1,2-cyclohexanediamine-N,N,N,N-tetraacetic acid monohydrate (CyDTA), and dissolve by heating. After cooling, dilute to 1 000 ml with water. NOTE Approximately 25 ml i

31、s required. Determine the exact strength of this solution by titration against the standard volumetric zinc solution, c(Zn) = 0,02 mol/l. 3.1.3 Standard volumetric EDTA solution, c(EDTA) = 0,012 5 mol/l. Dissolve 5 g of EDTANa2(ethylenediamine-tetraacetic acid disodium salt, dihydrate) in water and

32、dilute to 1 000 ml in a volumetric flask. Store in a plastic bottle. Standardize against calcium as follows. Pipette 25 ml of standard calcium oxide 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 C

33、alcein indicator, and titrate with the standard volumetric EDTA solution, from a fluorescent green colour to pink. Standardize against magnesium as follows. Pipette 25 ml of standard magnesium oxide solution (1 mg/ml), into a 500 ml conical flask, add 20 drops of hydrochloric acid (concentrated) and

34、 20 ml of ammonia solution (concentrated), and dilute to about 200 ml. Add about 0,04 g of methylthymol blue complexone indicator, and titrate with the standard volumetric EDTA solution. 5 EN ISO 21587-1:2007 (E) 3.1.4 Standard volumetric zinc solution, c(Zn) = 0,05 mol/l. Wash the surface of about

35、5 g of pellets of metallic zinc in about 50 ml of hydrochloric acid (1+1) to remove oxide, then wash successively with water, ethanol and diethyl ether. Weigh 3,269 g of the dried pellets, dissolve in 10 ml of hydrochloric acid (concentrated) and 50 ml of water, cool and dilute to the mark in a 1 00

36、0 ml volumetric flask. 1 ml of this zinc solution (0,05 mol/l) is equivalent to 2,55 mg of Al2O3. 3.1.5 Standard volumetric zinc solution, c(Zn) = 0,02 mol/l. Wash the surface of the zinc (purity, more than 99,9 % by mass) with hydrochloric acid (1+3) and dissolve the oxidized layer. Subsequently, w

37、ash with water, ethanol and diethyl ether in succession, then dry in a desiccator. Weigh 0,66 g (recorded to 0,1 mg) of zinc, transfer it to a 300 ml beaker, and cover with a watch glass. Add 20 ml of water and 10 ml of nitric acid carefully, and heat to dissolve on a steam bath. After cooling, dilu

38、te to 1 000 ml in a volumetric flask with water. Calculate the factor of this zinc solution using the following equation: 0,653 9 100mAF = (1) where F is the factor of this zinc solution; m is the mass, in grams, of the weighed zinc; A is the purity, in percentage by mass, of the zinc. 3.2 Standard

39、solutions 3.2.1 Standard aluminium oxide solution, Al2O31 mg/ml. Wash the surface of a sufficient amount of aluminum metal (purity 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 desicc

40、ator. Weigh 0,529 2 g of aluminium and transfer to a 250 ml beaker. Cover with a watch glass, add 20 ml hydrochloric acid (1+1), and heat to dissolve. After cooling, dilute to 1 000 ml in a volumetric flask with water. 3.2.2 Standard calcium oxide solution, CaO 1 mg/ml. Dissolve 1,785 g of pure calc

41、ium 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. 3.2.3 Standard chromium(III) oxide solution, Cr2O31 mg/ml. Dry about 2 g t

42、o 3 g of potassium dichromate 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. 3.2.4 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 volumet

43、ric flask and dilute to the mark with water. Prepare this solution freshly when required. 3.2.5 Standard iron(III) oxide solution, Fe2O31 mg/ml. Wash the surface of a sufficient amount of iron metal (purity greater than 99,9 %) with hydrochloric acid (1+4). Then dissolve the oxidized layer, and wash

44、 with water, ethanol and diethyl ether in succession. Then dry in a 6 EN ISO 21587-1:2007 (E) 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 it is dissolved. After cooling, dilute

45、to 1 000 ml in a volumetric flask with water. 3.2.6 Diluted standard iron(III) oxide solution, Fe2O30,2 mg/ml. Pipette 20 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. 3.2.7

46、Dilute standard iron (III) oxide solution, Fe2O30,04 mg/ml. Pipette 4 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. 3.2.8 Standard magnesium oxide solution, MgO, 1 mg/ml. Was

47、h 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. Weigh 0,301 5 g of the washed magnesium, transfer to a 200 ml

48、 beaker and cover with a watch glass. Add 20 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. 3.2.9 Standard manganese(II) oxide solution, MnO 1 mg/ml. Wash the surface of a sufficient ma

49、ss of manganese metal (purity more than 99,9 % by mass) with hydrochloric acid (1+3) to dissolve the oxidized layer. Then wash with water, ethanol and diethyl ether in succession and dry in a desiccator. Weigh 0,774 5 g of this metal, transfer to a 200 ml beaker and cover with a watch glass. Add 40 ml of nitric acid (1+1) and heat to dissolve. After cooling, transfer to a 1 000 ml volumetric flask. 3.2.10 Dilute standard manganese(II) oxide solution, MnO 0,04 mg/ml. Transfer 40 ml of the standard manganese(II) oxide solut