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

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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)This British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 January2009 BSI 2009ISBN 978 0 580 57835 9Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 10058-3:2008N

3、ational 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BS EN ISO 10058:1996.Together with BS EN ISO 10058-1 and BS EN ISO 10058-2, itsupersedes BS EN ISO 10058:1996 which is withdrawn.The UK participation in its preparation was entrusted to Tech

4、nicalCommittee 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 the necessary provisionsof a contract. Users are responsible for its correct application.Complianc

5、e with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE 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 fluorescenc

6、e method) - Part 3:Flame atomic absorption spectrophotometry (FAAS) andinductively coupled plasma atomic 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 spectrom

7、triedabsorption atomique dans la flamme (FAAS) etspectromtrie dmission atomique avec plasma induit parhaute frquence (ICP-AES) (ISO 10058-3:2008)Chemische Analyse von feuerfesten Erzeugnissen ausMagnesit und Dolomit (Alternative zurRntgenfluoreszenzanalyse) - Teil 3:Flammenatomabsorptionsspektroskop

8、ie (FAAS) undAtomemissionsspektrometrie mit induktiv gekoppeltemPlasma (ICP-AES) (ISO 10058-3:2008)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 t

9、he 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 exists in three official versions (English, French, Germa

10、n). 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 bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Repub

11、lic, 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.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORM

12、ALISATIONEUROPISCHES 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 10058-3:2008: EBS EN ISO 10058-3:2008EN ISO 10058-3:2008 (E) 3 Foreword This docum

13、ent (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, eithe

14、r 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 and/or CENE

15、LEC 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, Belg

16、ium, 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

17、 The text of ISO 10058-3:2008 has been approved by CEN as a EN ISO 10058-3:2008 without any modification. BS EN ISO 10058-3:2008ISO 10058-3:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Instrumental methods using ICP-AES.2 3.1 Determination of r

18、esidual 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 and zirconium oxide using stock solutions (S1) or (S1) by ICP-AES.3 3.3 Determination of sodium ox

19、ide 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 oxide and chromium(III) oxide by FAAS 9 4.2 Determination of calcium oxide, sodium oxide and pot

20、assium oxide using stock solutions (S3) by FAAS11 5 Test report13 BS EN ISO 10058-3:2008ISO 10058-3:2008(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 prepari

21、ng 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 on that committee. International organizations, governmental and non-governmental, in lia

22、ison 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 in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of

23、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 Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is

24、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 10058-3 was prepared by Technical Committee ISO/TC 33, Refractories. This first edition of ISO 10058-3, togeth

25、er with ISO 10058-1 and ISO 10058-2, cancels and replaces ISO 10058:1992 which has been technically revised 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

26、 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 fluorescence method): Part 1: Apparatus, reagents, dissolution and determination of gravi

27、metric 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 10058-3:2008INTERNATIONAL STANDARD ISO 10058-3:2008(E) ISO 2008 All rights reserved 1Chemical analysis of magnesite and

28、 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) 1 Scope This part of ISO 10058 specifies atomic absorption spectrometry (AAS) and inductively co

29、upled 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 Ran

30、ge Component 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 reference

31、s 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 amendments) applies. ISO 10058-1:2008, Chemical analysis of magnesit

32、e and 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

33、plasma atomic emission spectrometry (ICP-AES) methods BS 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 stock solutions (S1) by ICP-AES 3.1.1 Principle The residual silica remaining in solutions (S1) (

34、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 solution (0,08 mg/ml) precisely to several 100 ml volumetric flasks in accordance with the compo

35、sition 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 accordance with the compositions of the samples, and the types and capabilities of the instr

36、ument 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 solution 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,

37、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 water. This solution, which is used for the determination of dissolved silicon(IV) oxide, is

38、 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 251,611 nm. 3.1.4 Blank test Carry out the procedure in 3.1.3 with blank solution (B1) (see ISO 1

39、0058-1:2008, Annex A). The equivalent diluted blank solution to diluted stock solution (S1d) is designated as diluted blank solution (B1d). BS 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

40、out the emission procedure described in 3.1.3. Plot the relation between the emission intensity and mass of 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 ea

41、ch set of determinations. 3.1.6 Calculation Calculate the mass fraction of silicon(IV) oxide, 2SiO,w expressed 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 sbSiO25010100

42、mm mmwm+= (1) where m is the mass of the test portion calculated in accordance with ISO 10058-1:2008, 8.2.2.3.1, 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

43、 solution (S1d) as described in 3.1.3, in grams (g); mbis the mass of silicon(IV) oxide in diluted blank solution (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)

44、 oxide and zirconium oxide using stock solutions (S1) or (S1) by ICP-AES 3.2.1 Principle The emission intensity 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 f

45、or stock solutions (S1) or (S1) (see ISO 10058-1:2008, Annex A). This method should be applied to components 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 Fe2O

46、30,01 to 10 Cr2O30,01 to 3 TiO20,01 to 1 ZrO20,01 to 1 NOTE 1 When solution (S1) is used, the SiO2is residual 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

47、 mass. BS 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/ml, Fe2O30,04 mg/ml, TiO20,005 mg/ml, MnO 0,005 mg/ml, CaO 0,04 mg/ml, Cr2O30

48、,02 mg/ml, ZrO20,005 mg/ml. Transfer an aliquot portion (1 mg/ml) of standard silicon(IV) oxide (40 ml), aluminium oxide (40 ml), iron(III) oxide (40 ml), titanium(IV) oxide (5 ml), manganese(II) oxide (5 ml), calcium oxide (40 ml), chromium(III) oxide (20 ml) and zirconium oxide (5 ml) solutions in

49、to a 1 000 ml volumetric flask and dilute to the mark with water. 3.2.2.2 Matrix solution 2 or 2. Carry out the procedure given in ISO 10058-1:2008, 8.2.2.3 or 8.2.3.3 without the sample, but omit heating the fusion mixture or anhydrous sodium carbonate. The equivalent solution to stock solution (S1) or (S1) is designated as matrix solution 2 or 2 as applicable. 3.2.2.3 Internal standard solution. Transfer 10 ml of standard scandium solution (1 mg/ml) and standard yttrium solution (1 mg/ml) into a volumetri