1、BRITISH STANDARDBS EN ISO 21587-2:2007Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysisThe European Standard EN ISO 21587-2:2007 has the status of a British StandardICS 81.080g49g50g3g38g50g51g60g44g49g42g3g58g44g55g
2、43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 21587-2:2007This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 20
3、07 BSI 2007ISBN 978 0 580 58994 2National forewordThis British Standard is the UK implementation of EN ISO 21587-2:2007. Together with BS EN ISO 21587-1:2007, it supersedes BS EN 955-2:1995 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee RPI/1, Refract
4、ory products and materials.A list 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 c
5、annot confer immunity from legal obligations.Amendments issued since publicationAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 21587-2September 2007ICS 81.080 Supersedes EN 955-2:1995 English VersionChemical analysis of aluminosilicate refractory products(alternative to
6、the X-ray fluorescence method) - Part 2: Wetchemical analysis (ISO 21587-2:2007)Analyse chimique des produits rfractairesdaluminosilicates (mthode alternative la mthode parfluorescence de rayons X) - Partie 2: Mthodes danalysechimique par voie humide (ISO 21587-2:2007)Chemische Analyse feuerfester E
7、rzeugnisse ausAlumosilicat (Alternative zumRntgenfluoreszenzverfahren) - Teil 2: NasschemischeAnalyse (ISO 21587-2:2007)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
8、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 member.This European Standard exists in three official versions
9、(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 members are the national standards bodies of Austria, Belgium, Bulgar
10、ia, 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 FOR STANDARDIZATI
11、ONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES 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 21587-2:2007: EForeword The text of ISO 21587-2:2007 has be
12、en prepared by Technical Committee ISO/TC 33 “Refractories” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 21587-2:2007 by Technical Committee CEN/TC 187 “Refractory products and materials“, the secretariat of which is held by BSI. This European Standar
13、d shall be given the status of a national 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. According to the CEN/CENELEC Inter
14、nal Regulations, the 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, Mal
15、ta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 21587-2:2007 has been approved by CEN as EN ISO 21587-2:2007 without any modifications. EN ISO 21587-2:2007Reference numberISO 21587-2:2007(E)INTE
16、RNATIONAL STANDARD ISO21587-2First edition2007-03-01Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis Analyse chimique des produits rfractaires daluminosilicates (mthode alternative la mthode par fluorescence de rayo
17、ns X) Partie 2: Mthodes danalyse chimique par voie humide EN ISO 21587-2:2007ii iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Determination of residual silicon(IV) oxide in solution 2 4 Determination of aluminium oxide 3 5 Determination of iron(III) oxide 5 6 Determination of
18、 titanium(IV) oxide 7 7 Determination of manganese(II) oxide by permanganate absorption spectrophotometric method . 9 8 Determination of calcium oxide 10 9 Determination of magnesium oxide 11 10 Determination of sodium oxide by flame photometry 12 11 Determination of potassium oxide by flame photome
19、try . 14 12 Determination of chromium(III) oxide using diphenylcarbazide 14 13 Determination of zirconium oxide by Xylenol orange. 16 14 Determination of phosphorus(V) oxide by molybdenum blue. 17 15 Test report . 19 EN ISO 21587-2:2007iv Foreword ISO (the International Organization for Standardizat
20、ion) 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 established has the right to be r
21、epresented 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. International Standards
22、 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. Publication as an Internat
23、ional 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 patent rights. ISO 21587-2 wa
24、s 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 gravimetric silica Part
25、2: Wet chemical analysis Part 3: Inductively coupled plasma and atomic absorption spectrometry methods EN ISO 21587-2:20071Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis 1 Scope This part of ISO 21587 specifies tr
26、aditional (“wet“) methods for the chemical analysis of aluminosilicate refractory products and raw materials. The methods are applicable to the determination of the following: silicon(IV) oxide (SiO2) aluminium oxide (Al2O3) iron(III) oxide (total iron oxide calculated as Fe2O3) titanium(IV) oxide (
27、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) This part of ISO 21587 gives alternatives to the X-ray fluorescence (XRF) method given in ISO 12677:2003,
28、 Chemical analysis of refractory products by XRF Fused cast bead method. 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 reference
29、d document (including any amendments) applies. ISO 21587-1:2007, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and gravimetric silica ISO 26845, Chemical analysis of refractories General requirements f
30、or wet chemical analysis, atomic absorption spectrometry and inductively coupled plasma methods EN ISO 21587-2:20072 3 Determination of residual silicon(IV) oxide in solution 3.1 Principle An aliquot portion of the stock solution (S1) or (S1), after pH adjustment, is treated with ammonium molybdate
31、and the silicomolybdate is reduced to yield molybdenum blue, the absorbance of which is measured. The sum of this residual silicon(IV) oxide in solution plus the mass of silicon(IV) oxide (m1 m2) derived in ISO 21587-1:2007, 4.2.2.3 or 4.2.3.3, gives the total silicon(IV) oxide content. 3.2 Procedur
32、e This determination should be commenced with little delay after the stock solution (S1) or (S1) is prepared, as prolonged standing can allow polymerization of silica to occur, leading to low results. Transfer 10 ml of stock solution (S1) or (S1) obtained in 4.2.2.3 or 4.2.3.3 of ISO 21587-1:2007 to
33、 a 100 ml plastic beaker, and add 2 ml of hydrofluoric acid (1+9), mix with a plastic rod and allow to stand for 10 min. Then add 50 ml of boric acid solution. Add 2 ml of ammonium molybdate solution while mixing at a temperature of 25 C, and allow to stand for 10 min. Add 5 ml of L(+)-tartaric acid
34、 solution while stirring, and after 1 min add to it 2 ml of L(+)-ascorbic acid solution. Transfer the solution to a 100 ml volumetric flask, dilute to the mark with water, mix, and allow to stand for 60 min. Measure the absorbance of the solution in a 10 mm cell at a wavelength of 650 nm using water
35、 as the reference. 3.3 Plotting the calibration graph Transfer 0, 2, 4, 6, 8 and 10 ml aliquot portions (0 mg to 0,4 mg as silicon(IV) oxide) of dilute standard silicon(IV) oxide solution (SiO20,04 mg/ml) into several 100 ml plastic beakers, and to each add 10 ml of blank solution (B1) or (B1) obtai
36、ned in 4.2.2.4 or 4.2.3.4 of ISO 21587-1:2007. Treat these solutions and measure the absorbance as given in 3.2, and plot the absorbances against the amounts of silicon(IV) oxide. Prepare the calibration graph by adjusting the curve so that it passes through the point of origin. 3.4 Calculation Calc
37、ulate the mass fraction of silicon(IV) oxide, wSiO2, as a percentage, using the following equation, with the absorbances obtained by the procedure in 3.2 and the plotting of the calibration graph by the procedure in 3.3. ()()212 3 4SiO50010100mm mmwm+= (1) where m1is the mass, in g, from 4.2.2.3 or
38、4.2.3.3 of ISO 21587-1:2007; m2is the mass, in g, from 4.2.2.3 or 4.2.3.3 of ISO 21587-1:2007; m3is the mass, in g, of silicon(IV) oxide in the aliquot portion of stock solution (S1) or (S1) as applicable; m4is the mass, in g, of silicon(IV) oxide in the aliquot portion of blank solution (B1) or (B1
39、) as applicable; m is the mass, in g, of the test portion from 4.2.2.2 or 4.2.3.2 of ISO 21587-1:2007. EN ISO 21587-2:200734 Determination of aluminium oxide 4.1 General The determination of titanium(IV) oxide is carried out using one of the following methods: a) separation by cupferron-CyDTA-zinc b
40、ack titration method; b) CyDTA-zinc back titration method (without separation method). 4.2 Separation by cupferron-CyDTA-zinc back titration method 4.2.1 Principle Hydrochloric acid is added to an aliquot portion of stock solution (S1) or (S1), obtained in 4.2.2.3 or 4.2.3.3 of ISO 21587-1:2007, to
41、adjust the acidity. Iron, titanium, manganese and zirconium are separated from the solution by solvent extraction with cupferron solution and the precipitate removed by dissolution in chloroform. The organic phase is discarded. Excess standard volumetric CyDTA solution is added to the aqueous soluti
42、on after adjusting the pH with ammonia solution, and a chelate compound of aluminium CyDTA is formed. The pH is further adjusted by the addition of ammonium acetate buffer solution and an equivalent volume of ethanol is added to the solution. The amount of excess CyDTA is determined by back-titratio
43、n with standard volumetric zinc solution using dithizone as an indicator and the content of aluminium oxide calculated. 4.2.2 Procedure Transfer a 100 ml aliquot portion of the stock solution (S1) or (S1), obtained in 4.2.2.3 or 4.2.3.3 of ISO 21587-1:2007, to a 500 ml separating funnel and add 20 m
44、l of hydrochloric acid (concentrated) To the solution, add 20 ml of chloroform and 10 ml of cupferron solution. Stopper the funnel and shake vigorously. Release the pressure in the funnel by carefully removing the stopper and rinse the stopper and neck of the funnel with a little water. Allow the la
45、yers to separate and withdraw the chloroform layer. Confirm that extraction is complete by checking that the addition of a few drops of the cupferron solution to the aqueous solution does not produce a permanent coloured precipitate. Add further 10 ml portions of the chloroform and repeat the extrac
46、tion until the chloroform layer is colourless. Wash the stem of the funnel, inside and out, with chloroform, using a polyethylene wash bottle. Discard the chloroform extracts; do not allow them to dry as there can be an explosion risk. Transfer the aqueous solution and washings from the funnel into
47、a 1 l conical flask. Add a few drops of bromophenol blue indicator and ammonia solution (concentrated) until the solution is just alkaline. Re-acidify quickly with hydrochloric acid (concentrated) and add 5 to 6 drops in excess. Cool to room temperature. Add sufficient standard volumetric CyDTA solu
48、tion c(CyDTA) = 0,05 mol/l to combine with the aluminium oxide present, and a few millilitres in excess. NOTE 1 1 ml of standard volumetric CyDTA solution c(CyDTA) = 0,05 mol/l is equivalent to 1,275 % Al203for a 100 ml aliquot portion. Add ammonium acetate buffer solution until the indicator turns
49、blue, followed by 10 ml in excess. Add a volume of the ethanol equal to the total volume of the solution. If sulfates are precipitated by the alcohol, add just enough water to re-dissolve them. Add 20 ml of hydroxyammonium chloride and 1 ml to 2 ml of dithizone indicator, and titrate with standard volumetric zinc solution c(Zn) = 0,05 mol/l from green to the first appearance of a permanent pink colour. NOTE 2 The end point is often improved by the addition of a little naphthol green B solution (1 g/l) t
