EN ISO 4829-1-2018 en Steel and cast iron - Determination of total silicon contents - Reduced molybdosilicate spectrophotometric method - Part 1 Silicon contents between 0 05 % and.pdf

1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Steel and cast iron - Determination of total silicon contents - Reduced molybdosilicate spectrophotometric methodPart 1: Silicon contents between 0,05 % and 1,0 %BS EN ISO 48291:2018National forewordThis British Standar

2、d is the UK implementation of EN ISO 48291:2018. It is identical to ISO 48291:2018. It supersedes BS 62003.26.3:1987, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee ISE/102, Methods of Chemical Analysis for Iron and Steel.A list of organizations repre

3、sented 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. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 58

4、0 89017 8ICS 77.080.01Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDAR

5、DBS EN ISO 48291:2018EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 4829-1May 2018ICS 77.080.01 Supersedes EN 248291:1990EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2018 CEN

6、Ref. No. EN ISO 48291:2018: EAll rights of exploitation in any form and by any means reserved worldwide for CEN national MembersSteel and cast iron Determination of total silicon contents Reduced molybdosilicate spectrophotometric method Part 1: Silicon contents between 0,05 % and 1,0 % (ISO 48291:2

7、018)Aciers et fontes Dtermination du silicium total Mthode spectrophotomtrique au silicomolybdate rduit Partie 1: Teneurs en silicium comprises entre 0,05 % et 1,0 % (ISO 48291:2018)Stahl und Gusseisen Bestimmung des Gesamtsiliciumanteils Spektrophotometrische Methode mit reduziertem Molybdatosilica

8、t Teil 1: Siliciumanteile zwischen 0,05 % und 1,0 % (ISO 48291:2018)This European Standard was approved by CEN on 6 March 2018.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard

9、without any alteration. Uptodate lists and bibliographical references concerning such national standards may be obtained on application to the CENCENELEC Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other

10、language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Den

11、mark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.English Ve

12、rsionEN ISO 4829-1:2018 (E)European forewordThis document (EN ISO 48291:2018) has been prepared by Technical Committee ISO/TC 17 “Steel“ in collaboration with Technical Committee ECISS/TC 102 “Methods of chemical analysis for iron and steel” the secretariat of which is held by SIS.This European Stan

13、dard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2018, and conflicting national standards shall be withdrawn at the latest by November 2018.Attention is drawn to the possibility that some of the elements of

14、 this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights.This document supersedes EN 248291:1990.According to the CENCENELEC Internal Regulations, the national standards organizations of the following countries are bound to i

15、mplement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Roma

16、nia, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.Endorsement noticeThe text of ISO 4829-1:2018 has been approved by CEN as EN ISO 4829-1:2018 without any modification.2BS EN ISO 48291:2018ISO 4829-1:2018Foreword iv1 Scope . 12 Normative references 13 Terms a

17、nd definitions . 14 Principle 15 Reagents 26 Apparatus . 37 Sampling 48 Procedure. 48.1 Test portion 48.2 Blank test . 48.3 Determination . 48.3.1 Dissolution of the test portion . 48.3.2 Treatment of insoluble residue . 58.3.3 Preparation of the test solution 58.3.4 Development of the colour 58.3.5

18、 Spectrophotometric measurements . 68.4 Establishment of the calibration curve 68.4.1 Preparation of the calibration solutions 68.4.2 Spectrophotometric measurements . 68.4.3 Plotting of the calibration curves 69 Expression of results 79.1 Method of calculation 79.2 Precision . 810 Test report . 8An

19、nex A (informative) Additional information on the international interlaboratory test 9Annex B (informative) Graphical representation of precision data .10Bibliography .11 ISO 2018 All rights reserved iiiContents PageBS EN ISO 48291:2018ISO 4829-1:2018ForewordISO (the International Organization for S

20、tandardization) 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 a technical committee has been established has the ri

21、ght to be represented on that committee. International organizations, governmental and nongovernmental, 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. The procedure

22、s used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial ru

23、les of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).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. Details of any patent rights ident

24、ified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement. For an explanation

25、on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/forew

26、ord.html.This document was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of chemical composition.This second edition cancels and replaces the first edition (ISO 4829-1:1986), which has been technically revised.A list of all the parts in the ISO 4829 se

27、ries can be found on the ISO website.iv ISO 2018 All rights reservedBS EN ISO 48291:2018Steel and cast iron - Determination of total silicon contents - Reduced molybdosilicate spectrophotometric method Part 1: Silicon contents between 0,05 % and 1,0 %1 ScopeThis document specifies a spectrophotometr

28、ic method for the determination of total silicon in steel and cast iron using reduced molybdosilicate.The method is applicable to the determination of silicon mass fraction between 0,05 % and 1,0 %.2 Normative referencesThe following documents are referred to in the text in such a way that some or a

29、ll of their content constitutes requirements 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 648, Laboratory glassware Single-volume pipettesISO 1042, Laboratory glass

30、ware One-mark volumetric flasksISO 3696, Water for analytical laboratory use Specification and test methodsISO 14284, Steel and iron Sampling and preparation of samples for the determination of chemical composition3 Terms and definitionsNo terms and definitions are listed in this document.ISO and IE

31、C maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at http:/www.electropedia.org/ ISO Online browsing platform: available at https:/www.iso.org/obp4 PrincipleDissolution of a test portion in an acid mixture appropriate to the alloy

32、composition.Fusion of the acidinsoluble residue with sodium peroxide. Formation of the oxidized molybdosilicate (yellow) complex in weak acid solution.Selective reduction of the molybdosilicate complex to a blue complex with ascorbic acid, after increasing the sulphuric acid concentration and adding

33、 oxalic acid to prevent the interference of phosphorus, arsenic and vanadium.Spectrophotometric measurement of the reduced blue complex at a wavelength of about 810 nm.INTERNATIONAL STANDARD ISO 4829-1:2018 ISO 2018 All rights reserved 1BS EN ISO 48291:2018ISO 4829-1:20185 ReagentsDuring the analysi

34、s, unless otherwise specified, use only reagents of recognized analytical grade and only grade 2 water as specified in ISO 3696. Water demineralized by ion-exchange shall not be used as it may contain significant amounts of colloidal silica.Reagents supplied in glass bottles, once opened, can absorb

35、 moisture and become reactive to glassware. Alkaline reagents, e.g. sodium carbonate and sodium peroxide, are particularly susceptible.To avoid the risk of significant contamination arising from this source, it is recommended that only freshly opened bottles of all reagents be used for the preparati

36、on of reagent solutions.To avoid adventitious contamination, the water shall be prepared, as required, for the specific purpose and collected in polypropylene containers for immediate use.All solutions shall be freshly prepared and stored in polypropylene or polytetrafluoroethylene containers.5.1 Pu

37、re iron, silicon content less than 5 g/g.5.2 Sodium peroxide, particle size less than 500 m.5.3 Nitric acid, , approximately 1,40 g/ml, diluted 3 + 17.Slowly add 150 ml of nitric acid, , approximately 1,40 g/ml, to 600 ml of water. Cool, dilute to 1 l with water and mix.5.4 Sulphuric acid, , approxi

38、mately 1,84 g/ml, diluted 1 + 3.Add cautiously, while stirring, 250 ml of sulphuric acid, , approximately 1,84 g/ml to 600 ml of water. Cool, dilute to 1 l with water and mix.5.5 Sulphuric acid, , approximately 1,84 g/ml, diluted 1 + 19.Add cautiously, while stirring, 50 ml of sulphuric acid, approx

39、imately 1,84 g/ml to 800 ml of water. Cool, dilute to 1 l with water and mix.5.6 Hydrochloric/nitric acids mixture.Add 180 ml of hydrochloric acid, , approximately 1,19 g/ml, and 65 ml of nitric acid, , approximately 1,40 g/ml, to 500 ml of water. Cool, dilute to 1 l with water and mix.5.7 Sulphuric

40、/nitric acids mixture.Add cautiously, while stirring, 35 ml of sulphuric acid, approximately 1,84 g/ml, and 45 ml of nitric acid, , about 1,40 g/ml to 500 ml of water. Cool, dilute to 1 l with water and mix.5.8 Ascorbic acid, 20 g/l solution.This solution shall be freshly prepared.5.9 Oxalic acid, 5

41、0 g/l solution.Dissolve 5 g of oxalic acid dihydrate (C2H2O42H2O) in water, dilute to 100 ml with water and mix.5.10 Hydrogen peroxide, 60 g/l solution.Dilute 200 ml of hydrogen peroxide, 300 g/l, to 1 l with water and mix.2 ISO 2018 All rights reservedBS EN ISO 48291:2018ISO 4829-1:20185.11 Potassi

42、um permanganate, 22,5 g/l solution.This solution shall be filtered before use in order to remove the fine particles of MnO2that may be present in the solution, as they will interfere with the measurement.5.12 Sodium molybdate, 25 g/l solution.Dissolve 2,5 g of sodium molybdate dihydrate (Na2MoO42H2O

43、) in 50 ml of water and filter through a medium-texture filter paper.Immediately before use, add 15 ml of sulphuric acid (5.5), dilute to 100 ml with water and mix.5.13 Silicon standard solution, 1 g/l.Prepare a 1 g/l silicon standard solution by using one of the procedures described in a) or b).a)

44、Preparation with silica.Weigh to the nearest 0,1 mg, 2,139 3 g of freshly calcined highpurity silica (SiO2mass fraction 99,9 %) and transfer to a platinum crucible.The highpurity silica shall be calcined for 1 h at 1 100 C and cooled in a desiccator immediately before use.Mix thoroughly with 16 g of

45、 anhydrous sodium carbonate (Na2CO3) and fuse at 1 050 C for 30 min. Extract the fusion product with 100 ml of water in a polypropylene or polytetrafluoroethylene beaker.NOTE Extraction of the fusion product might require gentle heating.Transfer the extract, which should contain no trace of residue,

46、 into a 1 000 ml onemark volumetric flask, dilute to the mark with water and mix. Transfer immediately into a well-stoppered polytetrafluoroethylene bottle for storage.1 ml of this standard solution contains 1 mg of silicon.b) Preparation with ammonium hexafluorosilicate.Dry several grams of ammoniu

47、m hexafluorosilicate (NH4)2SiF6 for about 1 h at 105 C to 110 C in an oven and cool to room temperature in a desiccator.Weigh to the nearest 0,1 mg, 3,171 0 g of the dried product. Transfer into a suitable plastic beaker and dissolve it in hot water (approximately 80 C).Allow to cool and transfer th

48、e solution quantitatively into a 500 ml polyethylene onemark volumetric flask, dilute to the mark with water and mix well.1 ml of this standard solution contains 1 mg of silicon.5.14 Silicon standard solution, 200 mg/l.Transfer 50,0 ml of one of the silicon stock solutions 5.13 a) or b) into a 250 m

49、l onemark volumetric flask. Dilute to the mark with water and mix. Transfer immediately to a well-stoppered polytetrafluoroethylene bottle for immediate use.1 ml of this standard solution contains 200 g of silicon.6 ApparatusOrdinary laboratory apparatus and the following shall be used.6.1 Beakers and lids, of polypropylene or polytetrafluoroethylene. ISO 2018 All rights reserved 3BS EN ISO 48291:2018ISO 4829-1:20186.2 Zirconium crucibles, of 50 ml capacity.NOTE As alternati