EN ISO 20565-2-2008 en Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) - Part 2 Wet chemical.pdf

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1、BS EN ISO20565-2:2008ICS 81.080NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDChemical analysisof chrome-bearingrefractory productsand chrome-bearingraw materials(alternative to theX-ray fluorescencemethod)Part 2: Wet chemical analysis (ISO20565-2:2008)Incorpor

2、ating corrigendum September 2010National forewordThis British Standard is the UK implementation of EN ISO 20565-2:2008. Together with BS EN ISO 20565-1:2008 and BS EN ISO 20565-3:2008, it supersedes BS 1902-2.2:1974 which is withdrawn. The UK participation in its preparation was entrusted to Technic

3、al Committee RPI/1, Refractory 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.Complianc

4、e with a British Standard cannot confer immunity from legal obligations.BS EN ISO 20565-2:2008This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2009 BSI 2010Amendments/corrigenda issued since publicationDate Comments 30 September 2010

5、Addition of supersession detailsISBN 978 0 580 72653 8EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 20565-2December 2008ICS 81.080English VersionChemical analysis of chrome-bearing refractory products andchrome-bearing raw materials (alternative to the X-rayfluorescence method) - Part 2: Wet

6、 chemical analysis (ISO20565-2:2008)Analyse chimique des produits rfractaires contenant duchrome et des matires premires contenant du chrome(mthode alternative la mthode par fluorescence derayons X) - Partie 2: Mthodes danalyse chimique par voiehumide (ISO 20565-2:2008)Chemische Analyse von chromhal

7、tigen feuerfestenErzeugnissen und chromhaltigen Rohstoffen (Alternativezum Rntgenfluoreszenzverfahren) - Teil 2:Nasschemische Verfahren (ISO 20565-2:2008)This European Standard was approved by CEN on 8 November 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stip

8、ulate 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 CEN member.This European Standard ex

9、ists 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 members are the national standards bo

10、dies 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, Switzerland and United Kingdom.EURO

11、PEAN 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. No. EN ISO 20565-2:2008: E3 Foreword T

12、his document (EN ISO 20565-2:2008) has been prepared by Technical 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 standa

13、rd, either by publication of an identical text or by endorsement, 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 an

14、d/or CENELEC shall not be held responsible for identifying any or 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 Republ

15、ic, 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 the United Kingdom. Endorsement notice The text of ISO 20565-2:2008 has b

16、een approved by CEN as a EN ISO 20565-2:2008 without any modification. BS EN ISO 20565-2:2008EN ISO 20565-2:2008 (E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope 1 2 Normative references 2 3 Determination of silicon(IV) oxide2 4 Determination of aluminium oxide.5 5 Determination

17、 of total iron as iron(III) oxide .8 6 Determination of titanium(IV) oxide.11 7 Determination of manganese(II) oxide 13 8 Determination of calcium oxide .14 9 Determination of magnesium oxide.15 10 Determination of sodium oxide by flame photometry .18 11 Determination of potassium oxide by flame spe

18、ctrophotometry .20 12 Determination of chromium(III) oxide21 13 Determination of zirconium oxide by xylenol orange absorption spectroscopy24 14 Determination of phosphorus(V) oxide by molybdenum blue method25 15 Test report 27 BS EN ISO 20565-2:2008EN ISO 20565-2:2008 (E)iv ISO 2010 All rights reser

19、vedForeword ISO (the International Organization 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

20、a technical committee has been established 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 matt

21、ers of electrotechnical standardization. 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 circul

22、ated to the member bodies for voting. Publication 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 responsib

23、le for identifying any or all such patent rights. ISO 20565-2 was prepared by Technical Committee ISO/TC 33, Refractories, in collaboration with Technical Committee CEN/TC 187, Refractory products and materials. ISO 20565 consists of the following parts, under the general title Chemical analysis of

24、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 Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupl

25、ed plasma atomic emission spectrometry (ICP-AES) BS EN ISO 20565-2:2008EN ISO 20565-2:2008 (E)INTERNATIONAL STANDARD ISO 2010 All rights reserved 1Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 2: Wet chemi

26、cal analysis 1 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. Table 1 Range of determination (% by mass)

27、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 been taken into account. BS EN ISO 20565-2:

28、2008EN ISO 20565-2:2008 (E)2 ISO 2010 All rights reserved2 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 (incl

29、uding 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, Chemical analysis

30、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 following method

31、s. 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 silicon(IV) oxide. 3.2

32、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 is measured. The s

33、um 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 prepared, as prolonged

34、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 solution. Add 2 ml of

35、 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 mark with water, mix

36、 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. BS EN ISO 20565-2:2008EN ISO 20565-2:2008 (E) ISO 2010 All rights reserved 33.2.3 Plotting calibration graph Transfer 0 ml, 2 ml, 4 ml, 6 ml, 8 ml and 10 ml

37、aliquot portions 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 agains

38、t 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 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 expre

39、ssed as a 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 aliq

40、uot portion 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 portio

41、n 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 is measured. 3.3.2 Procedure Transfer precisely an aliquot portion of stock solution (S1) (to two 100 ml plasti

42、c beakers 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 mi

43、xing 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 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

44、measure the 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.

45、 BS EN ISO 20565-2:2008EN ISO 20565-2:2008 (E)4 ISO 2010 All rights reservedWhen 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 spectrophotom

46、eter to show the differences within 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 absor

47、ption cells. Measure the absorbance 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

48、solution is the same as that for the corresponding stock solution. BS EN ISO 20565-2:2008EN ISO 20565-2:2008 (E)10 ISO 2010 All rights reserved5.3.4 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 i

49、ron(III) oxide to several 250 ml volumetric flasks. Treat these 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 the 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 absorban