DIN EN ISO 20565-2-2009 Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) - Part 2 Wet chemica.pdf

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1、June 2009DEUTSCHE NORM English price group 15No 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 71.040.40; 81.080!$X5r“15

2、31879www.din.deDDIN EN ISO 20565-2Chemical analysis of chrome-bearing refractory products andchrome-bearing raw materials (alternative to the X-ray fluorescencemethod) Part 2: Wet chemical analysis (ISO 20565-2:2008)English version of DIN EN ISO 20565-2:2009-06Chemische Analyse von chromhaltigen feu

3、erfesten Erzeugnissen und chromhaltigenRohstoffen (Alternative zum Rntgenfluoreszenzverfahren) Teil 2: Nasschemische Verfahren (ISO 20565-2:2008)Englische Fassung DIN EN ISO 20565-2:2009-06Together with DIN EN ISO 20565-1:2009-06 and DIN EN ISO 20565-3:2009-06 supersedesDIN 51074-1:1971-08, DIN 5107

4、4-2:1971-08, DIN 51074-3:1971-08 and DIN 51074-4:1971-08Supersedes: see belowwww.beuth.deDocument comprises pages322 National foreword This standard has been published in accordance with a decision taken by Technical Committee CEN/TC 187 International Standard ISO 20565-2:2008 as a European Standard

5、. ISO 20565-2 was prepared by Technical The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Technical Committee NA 062-02-61 AA Chemische Analyse von oxidischen Roh- und Werkstoffen. The DIN Standards corresponding t

6、o the International Standards referred to in this document are as follows: ISO 20565-1 DIN EN ISO 20565-1 ISO 26845 DIN EN ISO 26845 Amendments This standard differs from DIN 51074-1:1971-08, DIN 51074-2:1971-08, DIN 51074-3:1971-08 and DIN 51074-4:1971-08 as follows: a) The standard has been comple

7、tely revised taking into account the current chemical analysis aspects. Previous editions DIN 51074-1: 1971-08 DIN 51074-2: 1971-08 DIN 51074-3: 1971-08 DIN 51074-4: 1971-08 National Annex NA (informative) Bibliography DIN EN ISO 20565-1, Chemical analysis of chrome-bearing refractory products and c

8、hrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica DIN EN ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, AAS and ICP methods DIN EN ISO 20565-2:2009-

9、06Committee ISO/TC 33 “Refractories“. “Refractory products and materials“ (Secretariat: BSI, United Kingdom) to adopt, without alteration, EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 20565-2 December 2008 ICS 81.080 English Version Chemical analysis of chrome-bearing refractory products

10、 and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis (ISO 20565-2:2008) Analyse chimique des produits rfractaires contenant du chrome et des matires premires contenant du chrome (mthode alternative la mthode par fluorescence de rayons X) Part

11、ie 2: Mthodes danalyse chimique par voie humide (ISO 20565-2:2008) Chemische Analyse von chromhaltigen feuerfesten Erzeugnissen und chromhaltigen Rohstoffen (Alternative zum Rntgenfluoreszenzverfahren) Teil 2: Nasschemische Verfahren (ISO 20565-2:2008) This European Standard was approved by CEN on 8

12、 November 2008. CEN members are bound 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 national standards may b

13、e 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 any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN M

14、anagement Centre has the same status 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, N

15、orway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any f

16、orm and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 20565-2:2008: EContents Page 1 Scope 4 2 Normative references 5 3 Determination of silicon(IV) oxide5 4 Determination of aluminium oxide.8 5 6 Determination of titanium(IV) oxide.14 7 Determination of manganese(II) oxi

17、de 16 8 Determination of calcium oxide .17 9 Determination of magnesium oxide.18 10 Determination of sodium oxide by flame photometry .21 11 Determination of potassium oxide by flame spectrophotometry .23 12 Determination of chromium(III) oxide24 13 Determination of zirconium oxide by xylenol orange

18、 absorption spectroscopy27 14 Determination of phosphorus(V) oxide by molybdenum blue method28 15 Test report 30 DIN EN ISO 20565-2:2009-06EN ISO 20565-2:2008 (E)2Determination of total iron as iron(III) oxide .11 Foreword3 Foreword This document (EN ISO 20565-2:2008) has been prepared by Technical

19、Committee ISO/TC 33 “Refractories“ in collaboration with 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 text or by endorsement,

20、at the latest by June 2009, and conflicting national standards shall be 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

21、all such patent rights. According 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, I

22、celand, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 20565-2:2008 has been approved by CEN as a EN ISO 20565-2:2008 without any modificat

23、ion. DIN EN ISO 20565-2:2009-06EN ISO 20565-2:2008 (E)31 Scope This part of ISO 20565 specifies traditional (“wet process”) methods for the chemical analysis of chrome-bearing refractory products and raw materials. It is applicable to components within the ranges of determination given in Table 1. T

24、able 1 Range of determination (% by mass) Component Range SiO20,5 to 10 Al2O32 to 30 Fe2O30,5 to 25 TiO20,01 to 1 MnO 0,01 to 1 CaO 0,01 to 3 MgO 15 to 85 Na2O 0,01 to 1 K2O 0,01 to 1 Cr2O32 to 60 ZrO20,01 to 0,5 P2O50,01 to 5 LOI 0,5 to 5 NOTE These values are after the loss on ignition (LOI) has b

25、een taken into account. DIN EN ISO 20565-2:2009-06EN ISO 20565-2:2008 (E)42 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 referenc

26、ed document (including any amendments) applies. ISO 20565-1:2008, Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica ISO 26845:2008, C

27、hemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively compled plasma atomic emission spectromety (ICP-AES) methods 3 Determination of silicon(IV) oxide 3.1 General Determine the silicon(IV) oxide content using one of the

28、 following methods. a) Combined use of the 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. b) Molybdenum blue method This method is applied to samples consisting of less than 10 % by mass of silico

29、n(IV) oxide. 3.2 Combined use of the coagulation and molybdenum blue methods 3.2.1 Principle An aliquot portion of the stock solution (S1) (see ISO 20565-1), after pH adjustment, is treated with ammonium molybdate and the silicomolybdate is reduced to yield molybdenum blue, the absorbance of which i

30、s measured. The sum of this residual silicon(IV) oxide in solution plus the mass of silicon(IV) oxide determined in ISO 20565-1:2008, 9.2.2.3.3, gives the total silicon(IV) oxide content. 3.2.2 Procedure This determination should be commenced with little delay after the stock solution (S1) is prepar

31、ed, as prolonged standing may allow polymerization of silica to occur leading to low results. Transfer 10 ml of stock solution (S1) (see ISO 20565-1) 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 and add 50 ml of boric acid solu

32、tion. 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 volumetric flask, dilute to the mar

33、k 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 against water as a reference. DIN EN ISO 20565-2:2009-06EN ISO 20565-2:2008 (E)53.2.3 Plotting calibration graph Transfer 0 ml, 2 ml, 4 ml, 6 ml, 8 ml and 10 ml aliquot p

34、ortions of diluted standard silicon(IV) oxide solution (0 mg to 0,4 mg as silicon(IV) oxide) to separate 100 ml plastic beakers and add to each 10 ml of blank solution (B1) (see ISO 20565-1). Treat these solutions and measure the absorbance as given in 3.2.2, and plot the absorbances against the amo

35、unts 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 blank solution (B1), carry out the procedure given in 3.2.2. 3.2.5 Calculation Calculate the mass fraction of silicon(IV) oxide, 2SiO,w expressed as a

36、 percentage, using Equation (1) with the absorbances obtained in 3.2.2 and 3.2.4 and the calibration in 3.2.3. ()()212 sbSiO50010100mm mmwm+= (1) where m1is the mass from ISO 20565-1, in grams (g); m2is the mass from ISO 20565-1, in grams (g); ms is the mass of silicon(IV) oxide in the aliquot porti

37、on of stock solution (S1) as applicable, in grams (g); mbis the mass of silicon(IV) oxide in the aliquot portion of blank solution (B1) as applicable, in grams (g); m is the mass of the test portion from ISO 20565-1, in grams (g). 3.3 Molybdenum blue method 3.3.1 Principle An aliquot portion of the

38、stock solution (S1) (see ISO 20565-1), after pH adjustment, is treated with ammonium 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) (to two 100 ml plastic beakers

39、 and add to each an aliquot portion of blank solution obtained from 3.3.3. Add to each beaker 2 ml of hydrofluoric acid (1+9), mix with a plastic 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

40、 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 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 t

41、he absorbance of the solutions in a 10 mm cell at a wavelength of 650 nm against water as a reference. Take the mean of the two measurements. NOTE Aliquot volumes of stock solution and blank solution (B1) are shown in Table 2, corresponding to the content of silicon(IV) oxide in the sample. DIN EN I

42、SO 20565-2:2009-06EN ISO 20565-2:2008 (E)6When the difference of the two absorbance measurements is greater than 0,005, repeat the procedure in 3.3.2. When measurements of the same sample with around 1,0 absorbance are repeated, it is necessary for the spectrophotometer to show the differences withi

43、n 0,002. Table 2 Aliquot volumes of stock and blank solutions Mass fraction of silicon(IV) oxide % Aliquot portion of stock solution (S1) ml Aliquot portion of blank solution (B1) ml 8 10 20 5.3.2.2 Transfer a portion of the solution obtained in 5.3.2.1 to two absorption cells. Measure the absorbanc

44、e of each solution at the wavelength of 510 nm against water, and calculate the mean of the measured values. 5.3.3 Blank test Using blank solution (BE-b) (see ISO 20565-1), carry out the procedure in accordance with 5.3.2. The volume of the aliquot portion of blank solution is the same as that for t

45、he corresponding stock solution. DIN EN ISO 20565-2:2009-06EN ISO 20565-2:2008 (E)125.3.4 Plotting of calibration graph Transfer a range of 0 ml to 40,0 ml aliquot portions of the diluted iron(III) oxide standard solution 0 mg to 1,6 mg as iron(III) oxide to several 250 ml volumetric flasks. Treat t

46、hese solutions in accordance with 5.3.2.1 and measure the absorbance against the reference solution. Plot the relation between the absorbance and mass of iron(III) oxide. Prepare the calibration graph by adjusting the curve so that it passes through the point of origin. 5.3.5 Calculation Calculate t

47、he mass fraction of iron(III) oxide, 23Fe Ow , expressed as a percentage, using Equation (6), using the amount of iron(III) oxide which is derived from the absorbance obtained in 5.3.2.2 and 5.3.3 and the calibration in 5.3.4. 23sbFe O12250 100100mmwmVV= (6) where msis the mass of iron(III) oxide in

48、 the aliquot portion of stock solution (SE-b), in grams (g); mbis the mass of iron(III) oxide in the aliquot portion of blank solution (BE-b), in grams (g); V1is the volume of the aliquot portion taken for stock solution (SE-b), in millilitres (ml); V2is the volume of aliquot portion taken for stock

49、 solution (SE-b), in grams (g); m is the mass of the test portion described in ISO 20565-1, in grams (g). 5.4 (1,2-Cyclohexylenenitrilo)tetraacetic acid-zinc CyDTA*-zinc back-titrimetric method 5.4.1 Principle An appropriate amount of CyDTA solution is added to an aliquot portion of stock solution (SE-b). A chelate compound of iron CyDTA is formed by adjusting the pH with ammonia water. The pH is further adjusted by addition of hexamethylenetetramine. The amount of remaining CyDTA is determined by back-titration with zinc stand