BS EN ISO 10058-3-2008 Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method) - Part 3 Flame atomic absorption spectrophotom.pdf

1、BS EN ISO10058-3:2008ICS 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 3: Flame atomic absorptionspectrophotometry (FAAS) andinductively

2、 coupled plasma atomicemission spectrometry (ICP-AES) (ISO10058-3:2008)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/05/2009 01:57, Uncontrolled Copy, (c) BSIThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 January2009 BSI 2009ISBN

3、978 0 580 57835 9Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 10058-3:2008National forewordThis British Standard is the UK implementation of EN ISO10058-3:2008. It partially supersedes BS EN ISO 10058:1996.Together with BS EN ISO 10058-1 and BS EN ISO 10058-2, itsupersedes BS

4、 EN ISO 10058:1996 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee RPI/1, Refractory products and materials.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all

5、 the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/05/2009 01:57, Uncontrolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENN

6、EEUROPISCHE NORMEN ISO 10058-3December 2008ICS 73.080 Supersedes EN ISO 10058:1996 English VersionChemical analysis of magnesite and dolomite refractoryproducts (alternative to the X-ray fluorescence method) - Part 3:Flame atomic absorption spectrophotometry (FAAS) andinductively coupled plasma atom

7、ic emission spectrometry (ICP-AES) (ISO 10058-3:2008)Analyse chimique des produits de magnsie et de dolomie(mthode alternative la mthode par fluorescence derayons X) - Partie 3: Mthodes par spectromtriedabsorption atomique dans la flamme (FAAS) etspectromtrie dmission atomique avec plasma induit par

8、haute frquence (ICP-AES) (ISO 10058-3:2008)Chemische Analyse von feuerfesten Erzeugnissen ausMagnesit und Dolomit (Alternative zurRntgenfluoreszenzanalyse) - Teil 3:Flammenatomabsorptionsspektroskopie (FAAS) undAtomemissionsspektrometrie mit induktiv gekoppeltemPlasma (ICP-AES) (ISO 10058-3:2008)Thi

9、s 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 bibliographical referenc

10、es 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 member into i

11、ts 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, Latvia, Lith

12、uania, 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 Brussels 2008 CEN

13、 All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 10058-3:2008: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/05/2009 01:57, Uncontrolled Copy, (c) BSIBS EN ISO 10058-3:2008EN ISO 10058-3:2008 (E) 3 Foreword This document

14、 (EN ISO 10058-3:2008) 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 standard, either b

15、y 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 and/or CENELEC

16、 shall not be held responsible for identifying any or all such patent rights. This document 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

17、, 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 the United Kingdom. Endorsement notice Th

18、e text of ISO 10058-3:2008 has been approved by CEN as a EN ISO 10058-3:2008 without any modification. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/05/2009 01:57, Uncontrolled Copy, (c) BSIBS EN ISO 10058-3:2008ISO 10058-3:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword i

19、v 1 Scope1 2 Normative references1 3 Instrumental methods using ICP-AES.2 3.1 Determination of residual silica in stock solutions (S1) by ICP-AES 2 3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, manganese(II) oxide, calcium oxide, chromium(III) oxide an

20、d zirconium oxide using stock solutions (S1) or (S1) by ICP-AES.3 3.3 Determination of sodium oxide and potassium oxide using stock solutions (S4) by ICP-AES.6 3.4 Determination of phosphorus(V) oxide by ICP-AES7 4 Instrumental methods using FAAS .9 4.1 Determination of manganese(II) oxide, calcium

21、oxide and chromium(III) oxide by FAAS 9 4.2 Determination of calcium oxide, sodium oxide and potassium oxide using stock solutions (S3) by FAAS11 5 Test report13 Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/05/2009 01:57, Uncontrolled Copy, (c) BSIBS EN ISO 10058-3:2008ISO 10058-3:2008(

22、E) iv ISO 2008 All rights reservedForeword 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 int

23、erested in a subject for which 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 Electrotechnic

24、al Commission (IEC) on all matters 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

25、technical committees are circulated 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.

26、ISO shall not be held responsible for identifying any or all such patent rights. ISO 10058-3 was prepared by Technical Committee ISO/TC 33, Refractories. This first edition of ISO 10058-3, together with ISO 10058-1 and ISO 10058-2, cancels and replaces ISO 10058:1992 which has been technically revis

27、ed to include the increasing use of flame atomic absorption spectrophotometry (FAAS) and inductively coupled 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 th

28、e general title 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 Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrophotometry (FAAS) and

29、inductively coupled plasma atomic emission spectrometry (ICP-AES) Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/05/2009 01:57, Uncontrolled Copy, (c) BSIBS EN ISO 10058-3:2008INTERNATIONAL STANDARD ISO 10058-3:2008(E) ISO 2008 All rights reserved 1Chemical analysis of magnesite and dolom

30、ite 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) 1 Scope This part of ISO 10058 specifies atomic absorption spectrometry (AAS) and inductively coupled

31、plasma atomic emission spectrometry (ICP-AES) 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 determination (percentage by mass) Component Range Com

32、ponent Range SiO20,1 to 10 Na2O 0,01 to 1 Al2O30,05 to 10 K2O 0,01 to 1 Fe2O30,01 to 10 Cr2O30,01 to 3 TiO20,01 to 1 ZrO20,01 to 1 MnO 0,01 to 1 P2O50,01 to 5 CaO 0,01 to 10 LOI 0,01 to 60 NOTE These values are after the loss on ignition (LOI) has been taken into account. 2 Normative references The

33、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 amendments) applies. ISO 10058-1:2008, Chemical analysis of magnesite and

34、dolomite 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 for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma

35、 atomic emission spectrometry (ICP-AES) methods Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/05/2009 01:57, Uncontrolled Copy, (c) BSIBS EN ISO 10058-3:2008ISO 10058-3:2008(E) 2 ISO 2008 All rights reserved3 Instrumental methods using ICP-AES 3.1 Determination of residual silica in stoc

36、k solutions (S1) by ICP-AES 3.1.1 Principle The residual silica remaining in solutions (S1) (see ISO 10058-1:2008, Annex A) is determined using ICP-AES. 3.1.2 Reagents 3.1.2.1 Series 1 solution for calibration. Transfer appropriate amounts of aliquot portions of dilute silicon(IV) oxide standard sol

37、ution (0,08 mg/ml) precisely to several 100 ml volumetric flasks in accordance with the composition of the samples. To each, add 10 ml of matrix solution 1 and dilute to the mark with water. An example is shown in Table 2. In this table, a typical example of the preparation of solutions is shown. In

38、 accordance with the compositions of the samples, and the types and capabilities of the instrument used, an appropriate series of solutions for calibration is prepared. Table 2 Example of series 1 solution for calibration Series 1 solution No. Matrix solution 1 ml Dilute silicon(IV) oxide standard s

39、olution ml Concentration of solution SiO2mg/100 ml 1 10 0 0 2 10 5 0,4 3 10 10 0,8 4 10 15 1,2 5 10 20 1,6 6 10 25 2,0 3.1.3 Procedure Determine the silicon(IV) oxide remaining in solution (S1) as follows. Transfer 10 ml of stock solution (S1) to a 100 ml volumetric flask and dilute to the mark with

40、 water. This solution, which is used for the determination of dissolved silicon(IV) oxide, is designated as diluted stock solution (S1d). Spray a portion of diluted stock solution (S1d) into the argon plasma flame of the ICP-AE spectrometer, and measure the emission intensity at a wavelength of 251,

41、611 nm. 3.1.4 Blank test Carry out the procedure in 3.1.3 with blank solution (B1) (see ISO 10058-1:2008, Annex A). The equivalent diluted blank solution to diluted stock solution (S1d) is designated as diluted blank solution (B1d). Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/05/2009 0

42、1:57, Uncontrolled Copy, (c) BSIBS EN ISO 10058-3:2008ISO 10058-3:2008(E) ISO 2008 All rights reserved 33.1.5 Plotting the calibration graph Using the series 1 solution for calibration, carry out the emission procedure described in 3.1.3. Plot the relation between the emission intensity and mass of

43、oxide, prepare the calibration graph by adjusting the curve so that it passes through the point of origin. Carry out a new calibration using the range of calibration and blank solutions for each set of determinations. 3.1.6 Calculation Calculate the mass fraction of silicon(IV) oxide, 2SiO,w express

44、ed as a percentage, using Equation (1), from the amount of silicon(IV) oxide derived from the figures obtained from 3.1.3 and 3.1.4 and the calibration prepared in 3.1.5: ()()212 sbSiO25010100mm mmwm+= (1) where m is the mass of the test portion calculated in accordance with ISO 10058-1:2008, 8.2.2.

45、3.1, in grams (g); m1is the mass from ISO 10058-1:2008, 8.2.2.3.3, in grams (g); m2is the mass from ISO 10058-1:2008, 8.2.2.4, in grams (g); msis the mass of silicon(IV) oxide in diluted stock solution (S1d) as described in 3.1.3, in grams (g); mbis the mass of silicon(IV) oxide in diluted blank sol

46、ution (B1d) as described in 3.1.4, in grams (g). 3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, manganese(II) oxide, calcium oxide, chromium(III) oxide and zirconium oxide using stock solutions (S1) or (S1) by ICP-AES 3.2.1 Principle The emission intens

47、ity of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, manganese(II) oxide, calcium oxide, chromium(III) oxide and zirconium oxide is measured by ICP-AE spectrometer for stock solutions (S1) or (S1) (see ISO 10058-1:2008, Annex A). This method should be applied to components

48、 in (S1) or (S1) in accordance with Table 3. Table 3 Range of determination (percentage by mass) Component Range Component Range SiO20,1 to 10 MnO 0,01 to 1 Al2O30,05 to 10 CaO 0,01 to 10 Fe2O30,01 to 10 Cr2O30,01 to 3 TiO20,01 to 1 ZrO20,01 to 1 NOTE 1 When solution (S1) is used, the SiO2is residua

49、l silica. When solution (S1) is used, the SiO2is all of silicon(IV) oxide. NOTE 2 Determination of calcium oxide by this method cannot be applied to calcium oxide contents of more than 10 % by mass. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/05/2009 01:57, Uncontrolled Copy, (c) BSIBS EN ISO 10058-3:2008ISO 10058-3:2008(E) 4 ISO 2008 All rights reserved3.2.2 Reagents Reagents given in ISO 10058-1:2008, Clause 5, and the following. 3.2.2.1 Mixed standard solution 1, SiO20,04 mg/ml, Al2O30,04 mg/m