DIN EN ISO 10058-2-2009 Chemical analysis of magnesites and dolomites refractory products (alternative to the X-ray fluorescence method) - Part 2 Wet chemical analysis (ISO 10058-2.pdf

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1、April 2009DEUTSCHE NORM English price group 13No 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!$W,“1520991www.di

2、n.deDDIN EN ISO 10058-2Chemical analysis of magnesite and dolomite refractory products(alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis (ISO 10058-2:2008)English version of DIN EN ISO 10058-2:2009-04Chemische Analyse von feuerfesten Erzeugnissen aus Magnesit und Dolomit (A

3、lternativezur Rntgenfluoreszenzanalyse) Teil 2: Nasschemische Analyse (ISO 10058-2:2008)Englische Fassung DIN EN ISO 10058-2:2009-04Together with DIN EN ISO10058-1:2009-04 andDIN EN ISO 10058-3:2009-04supersedesDIN EN ISO 10058:1996-02www.beuth.deDocument comprises 24 pagesDIN EN ISO 10058-2:2009-04

4、 2 National foreword This standard has been prepared by Technical Committee ISO/TC 33 “Refractories” in collaboration with Technical Committee CEN/TC 187 “Refractory products and materials“ (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was the Normenauss

5、chuss Materialprfung (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 this document are as follows: ISO 10058-1 DIN EN ISO 10058-1 ISO 1005

6、8-3 DIN EN ISO 10058-3 ISO 26845 DIN EN ISO 26845 Amendments This standard differs from DIN EN ISO 10058:1996-02 as follows: a) The scope has been restricted to traditional wet chemical methods for the chemical analysis of magnesite and dolomite refractory products and raw materials. b) The determin

7、ation of lithium oxide has been deleted from the scope. c) The standard has been completely revised taking into account the current chemical analysis methods. Previous editions DIN 51073-1: 1967-10 DIN 51073-2: 1967-10 DIN 51073-3: 1967-10, 1969-05 DIN 51073-4: 1967-10 DIN 51073-7: 1967-10 DIN 51073

8、-8: 1967-10 DIN EN ISO 10058: 1996-02 National Annex NA (informative) Bibliography DIN EN ISO 10058-1, 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 DIN E

9、N ISO 10058-3, Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method) Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) DIN EN ISO 26845, Chemical analysis of refracto

10、ries General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 10058-2December 2008Supersedes EN ISO 10058:1996 English VersionChemical analy

11、sis of magnesite and dolomite refractoryproducts (alternative to the X-ray fluorescence method) - Part 2:Wet chemical analysis (ISO 10058-2:2008)Analyse chimique des produits de magnsie et de dolomie(mthode alternative la mthode par fluorescence derayons X) - Partie 2: Mthodes danalyse chimique par

12、voiehumide (ISO 10058-2:2008)Chemische Analyse von feuerfesten Erzeugnissen ausMagnesit und Dolomit (Alternative zurRntgenfluoreszenzanalyse) - Teil 2: NasschemischeAnalyse (ISO 10058-2:2008)This European Standard was approved by CEN on 1 November 2008.CEN members are bound to comply with the CEN/CE

13、NELEC 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

14、 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 status as theofficial versions.CEN

15、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, Slovakia, Slovenia, Spain, Sweden

16、, 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 for CEN national Members.Ref. N

17、o. EN ISO 10058-2:2008: EICS 81.080Contents Page 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 EN ISO 10058-2:2008 (E) 2DIN EN ISO 10058-2:2009-04 Scope4 Normative references4 Determination of silicon(IV) oxide .5 Determination of aluminium oxide 6 Determination of iron(III) oxide 9 Determination of magnesium

18、 oxide 13 Determination of sodium oxide by flame photometry .14 Determination of potassium oxide by flame spectrophotometry.16 Determination of chromium(III) oxide17 Determination of zirconium oxide by xylenol orange absorption spectroscopy .20 Determination of phosphorus(V) oxide by molybdenum blue

19、 method .21 Test report22 Determination of calcium oxide .12 Determination of titanium(IV) oxide.10 Determination of manganese(II) oxide 11 Foreword .3 Foreword This document (EN ISO 10058-2:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration with Technical Commi

20、ttee 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 text or by endorsement, at the latest by June 2009, and conflicting national standards shall be

21、withdrawn at the latest by June 2009. Attention is 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. Acco

22、rding to the CEN/CENELEC Internal 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, Latv

23、ia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 10058-2:2008 has been approved by CEN as a EN ISO 10058-2:2008 without any modification. EN ISO 10058-2:2008 (E)

24、 3DIN EN ISO 10058-2:2009-04 1 Scope This part of ISO 10058 specifies traditional (“wet process”) methods for the chemical analysis of magnesite and dolomite refractory products and raw materials. It is applicable to components within the ranges of determination given in Table 1. Table 1 Range of de

25、termination (percentage 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 igni

26、tion (LOI) has been taken 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 amendme

27、nts) applies. ISO 10058-1:2008, 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 ISO 10058-3:2008, Chemical analysis of magnesite and dolomite refractory pro

28、ducts (alternative to the X-ray fluorescence method) Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled atomic plasma emission spectrometry (ICP-AES) ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrome

29、try (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods EN ISO 10058-2:2008 (E) 4DIN EN ISO 10058-2:2009-04 3 Determination of silicon(IV) oxide 3.1 General The determination of silicon(IV) oxide is carried out using one of the following methods. a) Combined use of th

30、e dehydration or the coagulation and molybdenum blue methods This method is applied to samples consisting of more than 4 % by mass of silicon(IV) oxide (see 3.2). b) Molybdenum blue method This method is applied to samples consisting of less than 10 % by mass of silicon(IV) oxide (see 3.3). 3.2 Comb

31、ined use of the coagulation and molybdenum blue methods 3.2.1 Principle An aliquot portion of the stock solution (S1) (see ISO 10058-1:2008, Annex A), after pH adjustment, is treated with ammonium molybdate and the silicomolybdate is reduced to yield molybdenum blue, the absorbance of which is measu

32、red. The sum of this residual silicon(IV) oxide in solution plus the mass of silicon (IV) oxide (m1 m2) calculated in accordance with ISO 10058-1:2008, 8.2.2.3.3, gives the total silicon(IV) oxide content. 3.2.2 Procedure This determination should be commenced with little delay after the stock solut

33、ion (S1) is prepared, as prolonged standing may allow polymerization of silica to occur leading to low results. Transfer 10 ml of stock solution (S1) (see ISO 10058-1:2008, Annex A) to a 100 ml plastic beaker, add 2 ml of hydrofluoric acid (1+9) and mix with a plastic rod. Allow to stand for 10 min

34、and 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 solution while stirring and, after 1 min, add 2 ml of L (+)-ascorbic acid solution. Transfer the solution to a 100 ml vol

35、umetric 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 as reference. 3.2.3 Plotting the calibration graph Transfer 0 ml, 2 ml, 4 ml, 6 ml, 8 ml and 10 ml aliquot portions 0 mg to 0,

36、4 mg as silicon(IV) oxide of dilute standard silicon(IV) oxide solution (SiO20,04 mg/ml) to separate 100 ml plastic beakers and add to each 10 ml of blank solution (B1) (see ISO 10058-1:2008, Annex A). Treat these solutions and measure the absorbance as given in 3.2.2, and plot the absorbances again

37、st the amounts of silicon(IV) oxide. Prepare the calibration graph by adjusting the curve so that it passes through the point of origin. 3.2.4 Blank test Using the blank solution (B1) (see ISO 10058-1:2008, Annex A), carry out the procedure given in 3.2.2. EN ISO 10058-2:2008 (E) 5DIN EN ISO 10058-2

38、:2009-04 3.2.5 Calculation Calculate the mass fraction of silicon(IV) oxide, 2SiO,w expressed as a percentage, using Equation (1), with the absorbances obtained by the procedures given in 3.2.2 and 3.2.4 and the calibration graph plotted in 3.2.3. ()()212 sbSiO25010100mm mmwm+= (1) where m1is the ma

39、ss from ISO 10058-1:2008, 8.2.2.3.3, in grams (g); m2is the mass from ISO 10058-12008, 8.2.2.3.3, in grams (g); msis the mass of silicon(IV) oxide in the aliquot portion of stock solution (S1) as applicable, in grams (g); mbis the mass of silicon(IV) oxide in the aliquot portion of blank solution (B

40、1) as applicable, in grams (g); m is the mass of the test portion calculated in accordance with ISO 10058-1:2008, 8.2.2.3.1, in grams (g). 3.3 Molybdenum blue method 3.3.1 Principle An aliquot portion of the stock solution (S1) (see ISO 10058-1:2008, Annex A), after pH adjustment, is treated with am

41、monium molybdate and the silicomolybdate is reduced to yield molybdenum blue, the absorbance of which is measured. 3.3.2 Procedure Transfer precisely an aliquot portion of stock solution (S1) (see ISO 10058-1:2008, Annex A) to two 100 ml plastic beakers and add to each an aliquot portion of blank so

42、lution (B1) (see ISO 10058-1:2008, Annex A). Add to each 2 ml of hydrofluoric acid (1+9), mix with a plastics rod and allow to stand for 10 min. Add 50 ml of boric acid solution, dilute to 80 ml with water. Add 5 ml of ammonium molybdate solution while mixing at a temperature of 25 C and allow to st

43、and for 10 min. Add 5 ml of L (+)-tartaric acid solution while stirring and, after 1 min, add to 10 ml of L (+)-ascorbic acid solution. Transfer each solution to a 200 ml volumetric flask, dilute to the mark with water and mix. Allow to stand for 60 min and measure the absorbance of the solutions in

44、 a 10 mm cell at a wavelength of 650 nm against water as a reference. Average the two measurements. NOTE Aliquot volumes of stock solution (S1) and blank solution (B1) corresponding to the mass fraction of silicon(IV) oxide in the sample are shown in Table 2. If the difference of the two absorbance

45、measurements is greater than 0,005, repeat the procedure given in 3.3.2 and ISO 10058-1:2008, 8.2.3.3. When measurements of the same sample with around 1,0 absorbance are repeated, it is necessary for the spectrophotometer to show the differences within 0,002. Table 2 Aliquot volumes of stock soluti

46、on (S1) and blank solution (B1) Mass fraction of silicon(IV) oxide % Aliquot volume of stock solution (S1) ml Aliquot volume of blank solution (B1) ml 2 20 0 W 2, 4 10 10 W 4, u 10 5 15 EN ISO 10058-2:2008 (E) 6DIN EN ISO 10058-2:2009-04 3.3.3 Blank test Carry out a blank determination by treating t

47、he blank solution (B1) (see ISO 10058-1:2008, Annex A) and following the procedure described into 3.3.2. The volume of the aliquot portion of blank solution is the same as those for the corresponding “S” solution. 3.3.4 Plotting of calibration graph Transfer 0 ml, 5 ml, 10 ml, 15 ml, 20 ml and 25 ml

48、 aliquot portions 0 mg to 1 mg as silicon(IV) oxide of dilute standard silicon(IV) oxide solution (SiO20,04 mg/ml) to separate 100 ml plastic beakers and add to each 20 ml of blank solution (B1) (see ISO 10058-1:2008, Annex A). Treat these solutions and measure the absorbance in accordance with the

49、procedure from the addition of hydrofluoric acid (1+9) in 3.3.2. Plot the absorbance against the amounts of silicon(IV) oxide and prepare the calibration graph by adjusting the curve so that it passes through the point of origin. 3.3.5 Calculation Calculate the mass fraction of silicon(IV) oxide, 2SiO,w expressed as a percentage, using Equation (2), with the amount of silicon(IV) oxide derived from the absorbance measurements obtained in 3.3.2 and 3.3.3 and the calibration in 3.3.4. 2sbSiO250100mmwmV= (2) where msis the m