EN ISO 10058-2-2008 en Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method) - Part 2 Wet chemical analysis《菱镁矿和白云石耐火制品的化学分.pdf

1、BS EN ISO10058-2:2008ICS 73.080; 81.080NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDChemical analysisof magnesite anddolomite refractoryproducts (alternativeto the X-rayfluorescence method)Part 2: Wet chemical analysis (ISO10058-2:2008)This British Standardwa

2、s published under theauthority of the StandardsPolicy and StrategyCommittee on 31 January2009 BSI 2009ISBN 978 0 580 57834 2Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 10058-2:2008National forewordThis British Standard is the UK implementation of EN ISO10058-2:2008. It parti

3、ally supersedes BS EN ISO 10058:1996.Together with BS EN ISO 10058-1 and BS EN ISO 10058-3, itsupersedes BS EN ISO 10058:1996 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee RPI/1, Refractory products and materials.A list of organizations represented on

4、 this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARDNORME

5、EUROPENNEEUROPISCHE NORMEN ISO 10058-2December 2008ICS 73.080 Supersedes EN ISO 10058:1996 English VersionChemical analysis 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 ma

6、gnsie et de dolomie(mthode alternative la mthode par fluorescence derayons X) - Partie 2: Mthodes danalyse chimique par voiehumide (ISO 10058-2:2008)Chemische Analyse von feuerfesten Erzeugnissen ausMagnesit und Dolomit (Alternative zurRntgenfluoreszenzanalyse) - Teil 2: NasschemischeAnalyse (ISO 10

7、058-2:2008)This European Standard was approved by CEN on 1 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 bibliograp

8、hical 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 any other language made by translationunder the responsibility of a CEN

9、 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, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy

10、, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Bru

11、ssels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 10058-2:2008: EBS EN ISO 10058-2:2008EN ISO 10058-2:2008 (E) 3 Foreword This document (EN ISO 10058-2:2008) has been prepared by Technical Committee ISO/TC 33 “Refractori

12、es“ 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, at the latest by June 2009, and

13、 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 all such patent rights. This do

14、cument supersedes EN ISO 10058:1996. 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, Greec

15、e, 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 10058-2:2008 has been approved by CEN as a EN ISO 10058-2:2008 without

16、any modification. BS EN ISO 10058-2:2008ISO 10058-2:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Determination of silicon(IV) oxide .2 4 Determination of aluminium oxide 4 5 Determination of iron(III) oxide 6 6 Determination of titanium(IV) oxi

17、de.7 7 Determination of manganese(II) oxide 8 8 Determination of calcium oxide .9 9 Determination of magnesium oxide 10 10 Determination of sodium oxide by flame photometry .11 11 Determination of potassium oxide by flame spectrophotometry.13 12 Determination of chromium(III) oxide14 13 Determinatio

18、n of zirconium oxide by xylenol orange absorption spectroscopy .17 14 Determination of phosphorus(V) oxide by molybdenum blue method .18 15 Test report19 BS EN ISO 10058-2:2008ISO 10058-2:2008(E) iv ISO 2008 All rights reservedForeword ISO (the International Organization for Standardization) is a wo

19、rldwide 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 represented o

20、n 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 are drafted

21、 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 International Standa

22、rd 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 10058-2 was prepared b

23、y Technical Committee ISO/TC 33, Refractories. This first edition of ISO 10058-2, together with ISO 10058-1 and ISO 10058-3, cancels and replaces ISO 10058:1992 which has been technically revised to include the increasing use of flame atomic absorption spectrophotometry (FAAS) and inductively couple

24、d plasma atomic emission spectrometry (ICP-AES) methods as well some improvements in the wet chemical analyses procedures developed in Japan. ISO 10058 consists of the following parts, under the general title Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray f

25、luorescence method): Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) BS EN ISO 10058-2:2008INTERNATIONAL STAND

26、ARD ISO 10058-2:2008(E) ISO 2008 All rights reserved 1Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method) Part 2: Wet chemical analysis 1 Scope This part of ISO 10058 specifies traditional (“wet process”) methods for the chemical analysis of

27、 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 determination (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

28、 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 ignition (LOI) has been taken into account. 2 Normative references The following referenced documents are indispensable for the applicatio

29、n 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 10058-1:2008, Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence

30、 method) Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica ISO 10058-3:2008, 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

31、atomic plasma emission spectrometry (ICP-AES) ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods BS EN ISO 10058-2:2008ISO 10058-2:2008(E) 2 IS

32、O 2008 All rights reserved3 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 the dehydration or the coagulation and molybdenum blue methods This method is applied to samples consisting of more

33、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 Combined use of the coagulation and molybdenum blue methods 3.2.1 Principle An aliquot portion of the stock solution (

34、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 measured. The sum of this residual silicon(IV) oxide in solution plus the mass of silicon (IV) oxide (m1 m2) calculated

35、 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 solution (S1) is prepared, as prolonged standing may allow polymerization of silica to occur leading to low results. Tr

36、ansfer 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 and add 50 ml of boric acid solution. Add 2 ml of ammonium molybdate solution while mixing at a temperature of 25

37、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 and allow to stand for 60 min. Measure the absorbance of the sol

38、ution 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 0,4 mg as silicon(IV) oxide of dilute standard silicon(IV) oxide solution (SiO20,04 mg/ml) to separate 100 ml plasti

39、c 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 against the amounts of silicon(IV) oxide. Prepare the calibration graph by adjusting the curve so that it passes throug

40、h 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. BS EN ISO 10058-2:2008ISO 10058-2:2008(E) ISO 2008 All rights reserved 33.2.5 Calculation Calculate the mass fraction of silicon(IV) oxide, 2SiO,w expressed

41、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 mass from ISO 10058-1:2008, 8.2.2.3.3, in grams (g); m2is the mass from ISO 10058-12008, 8.2.2.3

42、.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 (B1) as applicable, in grams (g); m is the mass of the test portion calculated in accordance wit

43、h 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 ammonium molybdate and the silicomolybdate is reduced to yield molybdenum blue, the absorbance o

44、f 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 solution (B1) (see ISO 10058-1:2008, Annex A). Add to each 2 ml of hydrofluoric acid (1+9), mix

45、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 stand for 10 min. Add 5 ml of L (+)-tartaric acid solution while stirring and, after 1 min, add

46、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 a 10 mm cell at a wavelength of 650 nm against water as a reference. Average the two measurem

47、ents. 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 measurements is greater than 0,005, repeat the procedure given in 3.3.2 and ISO 10058-1:2008,

48、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 solution (S1) and blank solution (B1) Mass fraction of silicon(IV) oxide % Aliquot volume of stock s

49、olution (S1) ml Aliquot volume of blank solution (B1) ml 2 20 0 W 2, 4 10 10 W 4, u 10 5 15 BS EN ISO 10058-2:2008ISO 10058-2:2008(E) 4 ISO 2008 All rights reserved3.3.3 Blank test Carry out a blank determination by treating the 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,