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

1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58(alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and gravime

2、tric silicaThe European Standard EN ISO 21587-1:2007 has the status of a British StandardICS 81.080Chemical analysis of aluminosilicate refractory products BRITISH STANDARDBS EN ISO 21587-1:2007BS EN ISO 21587-1:2007This British Standard was published under the authority of the Standards Policy and

3、Strategy Committee on 31 October 2007 BSI 2007ISBN 978 0 580 53701 1Amendments issued since publicationAmd. No. Date Commentsrequest 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

4、with a British Standard cannot confer immunity from legal obligations.National forewordThis British Standard is the UK implementation of EN ISO 21587-1:2007. Together with BS EN ISO 21587-2:2007, it supersedes BS EN 955-2:1995 which is withdrawn. Together with BS EN ISO 21587-3:2007, it supersedes D

5、D ENV 955-4:1997 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee RPI/1, Refractory products and materials.A list of organizations represented on this committee can be obtained on EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 21587-1September 20

6、07ICS 81.080 Supersedes EN 955-2:1995, ENV 955-4:1997 English VersionChemical analysis of aluminosilicate refractory products(alternative to the X-ray fluorescence method) - Part 1:Apparatus, reagents, dissolution and gravimetric silica (ISO21587-1:2007)Analyse chimique des produits rfractairesdalum

7、inosilicates (mthode alternative la mthode parfluorescence de rayons X) - Partie 1: Appareillage, ractifs,dissolution et teneur en silice par gravimtrie (ISO 21587-1:2007)Chemische Analyse feuerfester Erzeugnisse ausAlumosilicat (Alternative zur Rntgenfluoreszenzanalyse) -Teil 1: Gerte, Reagenzien,

8、Aufschluss und gravimetrischeBestimmung 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 Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a na

9、tional 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 exists in three official versions (English, French, German). A version in

10、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 bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Est

11、onia, 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 FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISC

12、HES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 21587-1:2007: EForeword The text of ISO 21587-1:2007 has been prepared by Technical Committee ISO/T

13、C 33 “Refractories” of the International Organization 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 nationa

14、l standard, either by publication of an identical text 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

15、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, Norw

16、ay, Poland, Portugal, Romania, Slovakia, Slovenia, 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. EN ISO 21587-1:2007Reference numberISO 21587-1:2007(E)INTERNATIONAL STANDARD IS

17、O21587-1First edition2007-03-01Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and gravimetric silica Analyse chimique des produits rfractaires daluminosilicates (mthode alternative la mthode par fluores

18、cence de rayons X) Partie 1: Appareillage, ractifs, dissolution et teneur en silice par gravimtrie EN ISO 21587-1:2007ii iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 2 3 Reagents 2 4 Dissolution and gravimetric silica 6 EN ISO 21587-1:2007iv Foreword ISO (the International Organ

19、ization 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 a subject for which a technical committee has been establish

20、ed 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 Commission (IEC) on all matters of electrotechnical standardization.

21、 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 committees are circulated to the member bodies for voting. Pu

22、blication 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 not be held responsible for identifying any or all such paten

23、t rights. ISO 21587-1 was prepared by Technical Committee ISO/TC 33, Refractories. ISO 21587 consists of the following parts, under the general title Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method): Part 1: Apparatus, reagents, dissolution and

24、gravimetric silica Part 2: Wet chemical analysis Part 3: Inductively coupled plasma and atomic absorption spectrometry methods EN ISO 21587-1:20071Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and grav

25、imetric silica 1 Scope This part of ISO 21587 specifies reagents, dissolution and gravimetric silica analysis for the chemical 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,

26、Chemical analysis of refractory products by XRF Fused cast bead method. This part of ISO 21587 should be used in conjunction 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

27、 (total iron oxide calculated as Fe2O3) titanium(IV) oxide (TiO2) manganese(II) oxide (MnO) calcium oxide (CaO) magnesium oxide (MgO) sodium oxide (Na2O) potassium oxide (K2O) chromium(III) oxide (Cr2O3) zirconium oxide (ZrO2) phosphorous(V) oxide (P2O5) EN ISO 21587-1:20072 2 Normative references T

28、he 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 21587-2, Chemical analysis of aluminosilicate

29、refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis ISO 21587-3, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 3: Inductively coupled plasma and atomic absorption spectrometry methods ISO 2684

30、5, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrometry 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 CyDT

31、A solution, c(CyDTA) = 0,05 mol/l. Dissolve 18 g of 1,2 cyclohexanediamine-N,N,N,N-tetraacetic acid monohydrate (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 sol

32、ution by titration against the standard volumetric zinc solution, c(Zn) = 0,05 mol/l. 3.1.2 Standard volumetric CyDTA 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 monoh

33、ydrate (CyDTA), and dissolve by heating. After cooling, dilute to 1 000 ml with water. NOTE Approximately 25 ml is 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)

34、= 0,012 5 mol/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 plastic bottle. Standardize against calcium as follows. Pipette 25 ml of standard calcium oxide solution (1 mg/ml), into a 500 ml coni

35、cal 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 standard volumetric EDTA solution, from a fluorescent green colour to pink. Standardize against magnesium as follows. Pipette 25 ml of standard magn

36、esium oxide 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 methylthymol blue complexone indicator, and titrate with the standard volumetric EDTA solution.

37、EN ISO 21587-1:200733.1.4 Standard volumetric zinc solution, c(Zn) = 0,05 mol/l. Wash the surface of about 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, diss

38、olve in 10 ml of hydrochloric acid (concentrated) and 50 ml of water, cool and dilute to the mark in a 1 000 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 (puri

39、ty, more than 99,9 % by mass) with hydrochloric acid (1+3) and dissolve the oxidized layer. Subsequently, wash 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 2

40、0 ml of water and 10 ml of nitric acid carefully, and heat to dissolve on a steam bath. After cooling, dilute 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

41、the mass, in grams, of the weighed zinc; A is the purity, in percentage by mass, of the zinc. 3.2 Standard 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 diss

42、olve 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 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 vol

43、umetric flask with water. 3.2.2 Standard calcium oxide 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

44、 1 000 ml in a volumetric flask. 3.2.3 Standard chromium(III) oxide solution, Cr2O31 mg/ml. Dry about 2 g to 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 solut

45、ion, 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 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

46、metal (purity greater than 99,9 %) with hydrochloric acid (1+4). Then dissolve the oxidized layer, and wash with water, ethanol and diethyl ether in succession. Then dry in a EN ISO 21587-1:20074 desiccator. Weigh 0,699 4 g of this, transfer to a beaker (200 ml), and cover with a watch glass. Add 40

47、 ml of hydrochloric acid (1+1), and heat on a steam bath until it is dissolved. After cooling, dilute 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 v

48、olumetric flask and dilute to the mark with water. Prepare this solution freshly when required. 3.2.7 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. P

49、repare this solution freshly when required. 3.2.8 Standard magnesium oxide 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. Weigh 0,301 5 g of the washed magnesium, transfer to a 200 ml beaker and cover with a watch glass. Add 20 ml of hydrochloric acid (1+1), an